CN104515697B - The detection preparation method of sample and vacuum degasser of normal temperature cure Silicone Rubber Based Coatings - Google Patents
The detection preparation method of sample and vacuum degasser of normal temperature cure Silicone Rubber Based Coatings Download PDFInfo
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Abstract
本发明公开了常温固化硅橡胶涂料的检测试样制备方法和真空脱气装置,包括如下步骤:1)取常温固化硅橡胶涂料成品震荡摇匀;2)将震荡摇匀后的常温固化硅橡胶涂料成品倒入涂料杯,于进行真空脱气处理,处理时间为2‑3min,真空度<10‑1pa,得脱气后的涂料;3)将脱气后的涂料的表面凝结膜去除,再将其倒入模具中,静置至涂料表面凝结后,将模具于温度:20℃‑25℃,湿度:30%‑35%的条件下,再静置96‑102h,取出,即得常温固化硅橡胶涂料试样。本方案有效排除环境因素,如涂料中溶解气体、空气中粉尘等对检测结果的影响,提高抽检试验的准确性。
The invention discloses a test sample preparation method and a vacuum degassing device for a normal temperature curing silicone rubber coating, comprising the following steps: 1) taking the finished product of the normal temperature curing silicone rubber coating and shaking and shaking; 2) shaking and shaking the normal temperature curing silicone rubber The finished paint is poured into the paint cup, and vacuum degassing treatment is carried out. The processing time is 2-3min, and the vacuum degree is < 10-1 Pa to obtain the degassed paint; 3) Remove the condensation film on the surface of the degassed paint, Then pour it into the mold, let it stand until the surface of the paint condenses, put the mold under the conditions of temperature: 20-25°C, humidity: 30%-35%, and then let it stand for 96-102h, take it out, and it will be at room temperature Cured silicone rubber coating samples. This scheme effectively eliminates the influence of environmental factors, such as dissolved gas in the paint and dust in the air, on the test results, and improves the accuracy of the random test.
Description
技术领域technical field
本发明属于涂料试验领域,特别涉及常温固化硅橡胶涂料的检测试样制备方法和真空脱气装置。The invention belongs to the field of paint testing, in particular to a test sample preparation method and a vacuum degassing device for normal temperature curing silicone rubber paint.
背景技术Background technique
随着国民经济的发展,各地污染源不断增多,绝缘子表面积污日趋严重,在恶劣气象条件下,极易发生污闪事故,威胁着电力系统的安全稳定运行,常温固化硅橡胶涂料具有优良的憎水性和憎水迁移性,能显著提高绝缘子的污闪电压,实践证明,在绝缘子表面喷涂常温固化硅橡胶涂料,能有效地降低污闪发生概率,对保障电力系统的安全稳定运行具有重要意义。然而,国内现有的常温固化硅橡胶涂料生产厂家众多,产品质量参差不齐,因此,常温固化硅橡胶涂料的入网检测非常必要。在抽检试验项目中,常温固化硅橡胶涂料的体积电阻率、相对介电常数、介质损耗角、介电强度等参数决定了涂料的绝缘性能,这些参数的测定需事先制备常温固化硅橡胶涂料试样,试样的好坏直接决定了最终的检测结果,但是目前尚无统一的方法或标准去规范常温固化硅橡胶涂料试样的制备过程,极易造成检测结果不准确等问题。With the development of the national economy, pollution sources in various places are increasing, and the pollution on the surface of insulators is becoming more and more serious. Under severe weather conditions, pollution flashover accidents are prone to occur, threatening the safe and stable operation of the power system. The room temperature curing silicone rubber coating has excellent hydrophobicity And hydrophobic migration, can significantly improve the pollution flashover voltage of insulators, practice has proved that spraying room temperature curing silicone rubber coating on the surface of insulators can effectively reduce the probability of pollution flashover, which is of great significance to ensure the safe and stable operation of the power system. However, there are many manufacturers of room temperature curing silicone rubber coatings in China, and the product quality is uneven. Therefore, the network inspection of room temperature curing silicone rubber coatings is very necessary. In the sampling test project, the volume resistivity, relative permittivity, dielectric loss angle, dielectric strength and other parameters of the normal temperature curing silicone rubber coating determine the insulation performance of the coating. The determination of these parameters needs to be prepared in advance. Like this, the quality of the sample directly determines the final test result, but there is no unified method or standard to standardize the preparation process of the room temperature curing silicone rubber coating sample, which can easily cause problems such as inaccurate test results.
发明内容Contents of the invention
针对上述问题,本发明提出了一种常温固化硅橡胶涂料检测试样的制备方法,能有效排除环境因素,如涂料中溶解气体、空气中粉尘等对检测结果的影响,提高抽检试验的准确性。In view of the above problems, the present invention proposes a method for preparing test samples of normal temperature curing silicone rubber coatings, which can effectively eliminate the influence of environmental factors, such as dissolved gas in the coating, dust in the air, etc. on the detection results, and improve the accuracy of the sampling test .
为了实现上述目的,本发明采用如下技术方案:In order to achieve the above object, the present invention adopts the following technical solutions:
一种常温固化硅橡胶涂料的检测试样制备方法,包括如下步骤:A method for preparing a detection sample of a normal temperature curing silicone rubber coating, comprising the steps of:
1)取常温固化硅橡胶涂料成品震荡摇匀;1) Take the finished product of normal temperature curing silicone rubber coating and shake it well;
2)将震荡摇匀后的常温固化硅橡胶涂料成品倒入涂料杯,进行真空脱气处理,处理时间为2-3min,真空度<10-1pa,得脱气后的涂料;2) Pour the finished room-temperature-cured silicone rubber coating into the coating cup after shaking and shaking, and carry out vacuum degassing treatment. The treatment time is 2-3 minutes, and the vacuum degree is <10 -1 Pa to obtain the degassed coating;
3)将脱气后的涂料的表面凝结膜去除,再将其倒入模具中,于真空条件下静置至涂料表面凝结后,将模具于温度:20℃-25℃,湿度:30%-35%的条件下,再静置96-102h,取出,即得常温固化硅橡胶涂料的检测试样。3) Remove the condensation film on the surface of the degassed paint, then pour it into the mold, let it stand under vacuum until the surface of the paint condenses, and put the mold at a temperature: 20°C-25°C, humidity: 30%- Under the condition of 35%, let it stand still for 96-102h, take it out, and obtain the test sample of the silicone rubber coating cured at room temperature.
优选的是,步骤1)中,所述的震荡时间为2-3min。Preferably, in step 1), the shaking time is 2-3min.
进一步地,步骤2)中,所述涂料杯为敞口杯。Further, in step 2), the paint cup is an open cup.
进一步地,步骤3)中,所述模具为敞开式槽状平板模具。Further, in step 3), the mold is an open grooved flat mold.
进一步地,步骤3)中,倒入模具的具体步骤为:将模具置于水平桌面上,调节槽面水平后,将脱气除膜后的涂料从模具中心位置倒入,至模具中涂料体积为模具总体积的2/3以上时停止。Further, in step 3), the specific steps of pouring into the mold are: placing the mold on a horizontal table, and after adjusting the level of the groove surface, pour the degassed and film-removed coating from the center of the mold to the volume of the coating in the mold. Stop when it is more than 2/3 of the total mold volume.
进一步地,步骤3)中,所述模具始终处于水平状态。Further, in step 3), the mold is always in a horizontal state.
本发明还提供了一种常温固化硅橡胶涂料的检测试样的真空脱气装置,其特征在于,真空罐通过连接管与真空泵相连,真空罐顶端设置有可开启的密封盖,真空罐侧壁的上部设置有压力计,真空罐侧壁的下部设置有放气阀,真空罐的底部设置有震动台。The present invention also provides a vacuum degassing device for testing samples of silicone rubber coatings cured at room temperature. The upper part of the vacuum tank is equipped with a pressure gauge, the lower part of the side wall of the vacuum tank is equipped with a vent valve, and the bottom of the vacuum tank is equipped with a vibration table.
优选的是,所述连接管通过排气孔与真空罐相连。可通过调整排气孔开口的大小,精确条件真空罐内的压力。Preferably, the connecting pipe is connected with the vacuum tank through an exhaust hole. The pressure in the vacuum tank can be precisely conditioned by adjusting the size of the vent hole opening.
优选的是,所述的震动台上设置有加热丝。Preferably, a heating wire is arranged on the vibrating table.
优选的是,所述的真空罐的侧壁由透明材料制成,设置有向内凸起的胶皮手套。Preferably, the side wall of the vacuum tank is made of transparent material and provided with inwardly protruding rubber gloves.
优选的是,所述的胶皮手套腕口的外侧面与真空罐的侧壁密封连接。Preferably, the outer surface of the cuff of the rubber glove is in sealing connection with the side wall of the vacuum tank.
本发明的有益效果:Beneficial effects of the present invention:
1.本发明提供了一种简单有效的常温固化硅橡胶涂料的检测试样制备方法,通过真空脱气装置和表面凝结膜的去除有效排除环境因素,如涂料中溶解气体、空气中粉尘等对检测结果的影响,提高抽检试验的准确性。1. The present invention provides a simple and effective test sample preparation method for room temperature curing silicone rubber coatings, effectively eliminating environmental factors such as dissolved gas in the coating, dust in the air, etc. The impact of the test results and improve the accuracy of the random test.
2.本发明制备过程简单、成本低,制备的涂料试样稳定性高,重现性和检测精度高。2. The preparation process of the present invention is simple, the cost is low, and the prepared coating sample has high stability, high reproducibility and detection precision.
附图说明Description of drawings
图1为本发明的操作流程图Fig. 1 is the operation flowchart of the present invention
图2为真空脱气装置的结构图,其中,1-真空罐2-压力计3-排气孔4-震动台5-连接管6-放气阀7-真空泵8-密封盖9-涂料杯10-真空罐侧壁11-胶皮手套。Figure 2 is a structural diagram of the vacuum degassing device, wherein, 1-vacuum tank 2-pressure gauge 3-vent hole 4-vibration table 5-connecting pipe 6-deflation valve 7-vacuum pump 8-sealing cover 9-paint cup 10-vacuum tank side wall 11-rubber gloves.
图3为真空脱气装置侧视图Figure 3 is a side view of the vacuum degassing device
具体实施方式Detailed ways
以下通过实施例的方式进一步说明本发明,但并不因此将本发明限制在所述的实施例范围之中。下列实施例中未注明具体条件的实验方法,按照常规的方法和条件进行选择。The present invention is further illustrated by way of examples below, but the present invention is not limited to the scope of the examples. For the experimental methods not indicating specific conditions in the following examples, select according to conventional methods and conditions.
实施例1Example 1
在未开桶前,将常温固化硅橡胶涂料成品震荡摇匀,对于长时间静置的涂料,摇动的时间为2分钟,摇匀后即开桶,迅速将试样倒入涂料杯内的3/4处,尽量避免空气溶入涂料,抽真空装置进行抽真空处理,抽真空时间为3min,真空度<10-1pa。抽真空过程中,为检验抽真空效果,涂料表面可见明显的气泡析出。待试样中气体析出后,用镊子去除表面凝结膜,快速将涂料倒入敞开式槽状平板模具,模具应放置于水平桌面上,处于真空条件下,且保证槽面水平。待涂料表面凝结后,将模具放置于恒温恒湿箱内,移动模具时应保持水平,同时在恒温恒湿箱内保证模具处于水平状态。温度设定为20℃,湿度为30%,96h后取出。Before opening the barrel, shake and shake the finished silicone rubber coating at room temperature. For the paint that has been left standing for a long time, shake it for 2 minutes. After shaking well, open the barrel and quickly pour the sample into the paint cup for 3 /4 place, try to avoid the air from dissolving into the paint, vacuumize the vacuum device, the vacuum time is 3min, and the vacuum degree is <10 -1 pa. During the vacuuming process, in order to test the vacuuming effect, obvious air bubbles can be seen on the surface of the coating. After the gas in the sample is precipitated, use tweezers to remove the surface condensation film, and quickly pour the paint into an open groove-shaped flat mold. The mold should be placed on a horizontal table under vacuum conditions, and the groove surface must be kept level. After the surface of the paint is condensed, place the mold in a constant temperature and humidity box, keep the level when moving the mold, and at the same time ensure that the mold is in a horizontal state in the constant temperature and humidity box. The temperature was set at 20°C, the humidity was 30%, and it was taken out after 96 hours.
结果表明:与原有检测方法相比,采用本发明所提供的方法,体积电阻率、相对介电常数、介电强度、介质损耗角正切值等指标的检测精确度提高5%-7%,同时该发明方法排除了环境因素、人为因素对检测结果的干扰,检测结果的可重复性高。The results show that: compared with the original detection method, the method provided by the invention can improve the detection accuracy of volume resistivity, relative permittivity, dielectric strength, dielectric loss tangent and other indicators by 5%-7%, At the same time, the inventive method eliminates the interference of environmental factors and human factors on the detection results, and the detection results have high repeatability.
一种常温固化硅橡胶涂料检测试样的真空脱气装置,真空罐1通过连接管5与真空泵7相连,真空罐1顶端设置有可开启的密封盖8,真空罐1侧壁的上部设置有压力计2,真空罐侧壁的下部设置有放气阀6,真空罐1的底部设置有震动台4。A vacuum degassing device for testing samples of silicone rubber coatings cured at room temperature, the vacuum tank 1 is connected to the vacuum pump 7 through the connecting pipe 5, the top of the vacuum tank 1 is provided with an openable sealing cover 8, and the upper part of the side wall of the vacuum tank 1 is provided with The pressure gauge 2 is provided with a vent valve 6 at the bottom of the side wall of the vacuum tank, and the vibration table 4 is provided at the bottom of the vacuum tank 1 .
优选的是,所述连接管5通过排气孔3与真空罐1相连。Preferably, the connecting pipe 5 is connected with the vacuum tank 1 through the exhaust hole 3 .
打开真空罐1的密封盖8,将装有涂料的涂料杯9置于真空罐内的震动台4上,闭合密封盖8,关闭放气阀6的阀门开关,开启震动台4,震动强度以涂料杯9不发生移动为宜,打开真空泵7,随着真空室内气体的减少,密封盖8被紧密的吸附在真空罐1上,观察压力计2,当真空度达到10-1pa后,维持3min,此时涂料内的气体完全被排出,关闭真空泵7和震动台4,打开放气阀6开关,待气压平衡后,打开密封盖8,取出涂料杯9即可。(具体装置参见图2)Open the sealing cover 8 of the vacuum tank 1, place the coating cup 9 with the coating on the vibrating table 4 in the vacuum tank, close the sealing cover 8, close the valve switch of the air release valve 6, open the vibrating table 4, and the vibration intensity is as high as It is advisable that the paint cup 9 does not move. Turn on the vacuum pump 7. With the reduction of the gas in the vacuum chamber, the sealing cover 8 is tightly adsorbed on the vacuum tank 1. Observe the pressure gauge 2. When the vacuum degree reaches 10 -1 Pa, maintain 3min, at this time, the gas in the paint is completely discharged, turn off the vacuum pump 7 and the vibration table 4, open the switch of the air release valve 6, after the air pressure is balanced, open the sealing cover 8, and take out the paint cup 9. (Refer to Figure 2 for the specific device)
优选的是,所述的震动台上设置有加热丝。可通过加热控制真空罐内的温度,满足不同材料的测试要求。Preferably, a heating wire is arranged on the vibrating table. The temperature in the vacuum tank can be controlled by heating to meet the testing requirements of different materials.
优选的是,所述的真空罐的侧壁10由透明材料制成,设置有向内凸起的胶皮手套11。使用者可通过手套对处于真空罐内的试样进行操作,实现了绝度真空条件下的试样测试,避免了外部环境的干扰。Preferably, the side wall 10 of the vacuum tank is made of transparent material and provided with a rubber glove 11 protruding inward. The user can operate the sample in the vacuum tank through gloves, realizing the test of the sample under absolute vacuum conditions and avoiding the interference of the external environment.
优选的,所述的胶皮手套腕口的外侧面与真空罐的侧壁密封连接。当真空罐内处于真空条件是,在大气压的作用下,胶皮手套向内膨胀,方便使用者的将手伸入手套中。Preferably, the outer surface of the cuff of the rubber glove is in sealing connection with the side wall of the vacuum tank. When the vacuum tank is in a vacuum condition, under the action of atmospheric pressure, the rubber glove expands inward, which is convenient for the user to put his hand into the glove.
实施例2Example 2
在未开桶前,将常温固化硅橡胶涂料成品震荡摇匀,对于长时间静置的涂料,摇动的时间为3分钟,摇匀后即开桶,迅速将试样倒入涂料杯内的3/4处,尽量避免空气溶入涂料,抽真空装置进行抽真空处理,抽真空时间为3min,真空度<10-1pa。抽真空过程中,为检验抽真空效果,涂料表面可见明显的气泡析出。待试样中气体析出后,用镊子去除表面凝结膜,快速将涂料倒入敞开式槽状平板模具,模具应放置于水平桌面上,处于真空条件下,且保证槽面水平。待涂料表面凝结后,将模具放置于恒温恒湿箱内,移动模具时应保持水平,同时在恒温恒湿箱内保证模具处于水平状态。温度设定为25℃,湿度为60%,102h后取出。所述模具始终处于真空条件下,真空度<10-1pa。Before opening the barrel, shake and shake the finished silicone rubber coating at room temperature. For the paint that has been left standing for a long time, shake it for 3 minutes. After shaking well, open the barrel and quickly pour the sample into the paint cup for 3 minutes. /4 place, try to avoid the air from dissolving into the paint, vacuumize the vacuum device, the vacuum time is 3min, and the vacuum degree is <10 -1 pa. During the vacuuming process, in order to test the vacuuming effect, obvious air bubbles can be seen on the surface of the coating. After the gas in the sample is precipitated, use tweezers to remove the surface condensation film, and quickly pour the paint into an open groove-shaped flat mold. The mold should be placed on a horizontal table under vacuum conditions, and the groove surface must be kept level. After the surface of the paint is condensed, place the mold in a constant temperature and humidity box, keep the level when moving the mold, and at the same time ensure that the mold is in a horizontal state in the constant temperature and humidity box. The temperature was set at 25°C, the humidity was 60%, and it was taken out after 102 hours. The mold is always under vacuum condition, the degree of vacuum is less than 10 -1 Pa.
实施例3Example 3
在未开桶前,将常温固化硅橡胶涂料成品震荡摇匀,对于长时间静置的涂料,摇动的时间为2.5分钟,摇匀后即开桶,迅速将试样倒入涂料杯内的3/4处,尽量避免空气溶入涂料,抽真空装置进行抽真空处理,抽真空时间为3min,真空度<10-1pa。抽真空过程中,为检验抽真空效果,涂料表面可见明显的气泡析出。待试样中气体析出后,用镊子去除表面凝结膜,快速将涂料倒入敞开式槽状平板模具,模具应放置于水平桌面上,处于真空条件下,且保证槽面水平。待涂料表面凝结后,将模具放置于恒温恒湿箱内,移动模具时应保持水平,同时在恒温恒湿箱内保证模具处于水平状态。温度设定为22.5℃,湿度为45%,98h后取出。Before opening the barrel, shake and shake the finished silicone rubber coating at room temperature. For the paint that has been left standing for a long time, the shaking time is 2.5 minutes. After shaking well, open the barrel and quickly pour the sample into the paint cup for 3 /4 place, try to avoid the air from dissolving into the paint, vacuumize the vacuum device, the vacuum time is 3min, and the vacuum degree is <10 -1 pa. During the vacuuming process, in order to test the vacuuming effect, obvious air bubbles can be seen on the surface of the coating. After the gas in the sample is precipitated, use tweezers to remove the surface condensation film, and quickly pour the paint into an open groove-shaped flat mold. The mold should be placed on a horizontal table under vacuum conditions, and the groove surface must be kept level. After the surface of the paint is condensed, place the mold in a constant temperature and humidity box, keep the level when moving the mold, and at the same time ensure that the mold is in a horizontal state in the constant temperature and humidity box. The temperature was set at 22.5°C, the humidity was 45%, and it was taken out after 98 hours.
上述虽然结合附图对本发明的具体实施方式进行了描述,但并非对本发明保护范围的限制,所属领域技术人员应该明白,在本发明的技术方案的基础上,本领域技术人员不需要付出创造性劳动即可做出的各种修改或变形仍在本发明的保护范围以内。Although the specific implementation of the present invention has been described above in conjunction with the accompanying drawings, it does not limit the protection scope of the present invention. Those skilled in the art should understand that on the basis of the technical solution of the present invention, those skilled in the art do not need to pay creative work Various modifications or variations that can be made are still within the protection scope of the present invention.
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