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CN110511600A - Preparation method of modified fumed silica coating material for protecting silicate cultural relics - Google Patents

Preparation method of modified fumed silica coating material for protecting silicate cultural relics Download PDF

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CN110511600A
CN110511600A CN201910976885.1A CN201910976885A CN110511600A CN 110511600 A CN110511600 A CN 110511600A CN 201910976885 A CN201910976885 A CN 201910976885A CN 110511600 A CN110511600 A CN 110511600A
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fumed silica
coating material
silica coating
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silicate cultural
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杨进
李佳钰
宋浩杰
贾晓华
李永
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Shaanxi University of Science and Technology
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    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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    • C09D1/00Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40Additives
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    • C09D7/63Additives non-macromolecular organic

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Abstract

本发明公开一种用于保护硅酸盐质文物的改性气相二氧化硅涂层材料的制备方法,包括如下步骤:1)量取气相二氧化硅分散在乙醇和异丙醇混合溶液中,得到气相二氧化硅分散液;2)量取全氟辛基三氯硅烷及正硅酸四乙酯加入步骤1)得到的分散液中,形成均匀的白色溶液;3)在白色溶液中滴加氨水形成均匀悬浮液;4)溶液超声分散并搅拌均匀的改性气相二氧化硅涂层材料;通过用正硅酸四乙酯和全氟辛基三氯硅烷改性气相二氧化硅,并将改性气相二氧化硅分散于乙醇中喷涂,即可形成透明超疏水超疏油涂层,制备方法简单快速,制备成本低,制备的产品具有优异的超疏水超疏油性能,透光性能,自清洁性能和耐久性的特点。The invention discloses a method for preparing a modified fumed silica coating material for protecting silicate cultural relics, which comprises the following steps: 1) measuring fumed silica and dispersing it in a mixed solution of ethanol and isopropanol, Obtain a fumed silica dispersion; 2) measure perfluorooctyltrichlorosilane and tetraethylorthosilicate and add it to the dispersion obtained in step 1) to form a uniform white solution; 3) dropwise add Ammonia forms a homogeneous suspension; 4) the solution ultrasonically disperses and stirs the uniform modified fumed silica coating material; by modifying the fumed silica with tetraethyl orthosilicate and perfluorooctyltrichlorosilane, and The modified fumed silica is dispersed in ethanol and sprayed to form a transparent superhydrophobic and superoleophobic coating. The preparation method is simple and fast, and the preparation cost is low. The prepared product has excellent superhydrophobic and superoleophobic properties, light transmission properties, Characterized by self-cleaning performance and durability.

Description

用于保护硅酸盐质文物的改性气相二氧化硅涂层材料的制备 方法Preparation of modified fumed silica coating material for protection of silicate cultural relics method

技术领域technical field

本发明属于文物保护领域,具体涉及一种用于保护硅酸盐质文物的改性气相二氧化硅涂层材料的制备方法。The invention belongs to the field of cultural relics protection, and in particular relates to a preparation method of a modified fumed silica coating material for protecting silicate cultural relics.

背景技术Background technique

有机/无机材料新材料领域有着广阔的应用前景,在涂料、薄膜、纳米复合材料方面都有着广泛的应用。但在文物保护领域,特别是硅酸盐质文物的保护领域少有报道和公布的专利。目前的保护材料往往容易受到水的侵蚀,机械强度低,而且抗老化和湿热能力差。气相二氧化硅具有良好的耐高温、化学稳定性、耐酸碱腐蚀等特点,而氟化物有着良好的热稳定性、机械性能以及疏水疏油特性,将二者结合起来可以充分发挥有机/无机材料的优势。Organic/inorganic materials have broad application prospects in the field of new materials, and have a wide range of applications in coatings, thin films, and nanocomposites. However, in the field of cultural relics protection, especially the protection of silicate cultural relics, there are few reports and published patents. Current protective materials are often vulnerable to water erosion, have low mechanical strength, and have poor resistance to aging and heat and humidity. Fumed silica has good high temperature resistance, chemical stability, acid and alkali corrosion resistance, etc., while fluoride has good thermal stability, mechanical properties and hydrophobic and oleophobic properties. Combining the two can give full play to the organic/inorganic The advantage of the material.

研究指出要使得涂层具有优异的透光性能,需要严格控制表面凸起尺寸,使得其粗糙度不超过可见光波长的1/4。因此,需要制备过程中严格控制好表面凸起结构的尺寸。一方面,超疏水超疏油性能的形成需要在表面形成较大的粗糙度,另一方面较大的粗糙度又会降低透光率,因此,在制备过程中有效控制表面凸起结构的尺寸,调控表面粗糙度至关重要。Studies have pointed out that in order to make the coating have excellent light transmission properties, the size of the surface protrusions needs to be strictly controlled so that the roughness does not exceed 1/4 of the wavelength of visible light. Therefore, it is necessary to strictly control the size of the surface protrusion structures during the preparation process. On the one hand, the formation of superhydrophobic and superoleophobic properties requires the formation of large roughness on the surface, on the other hand, large roughness will reduce the light transmittance. Therefore, the size of the surface protrusion structure can be effectively controlled during the preparation process. , it is very important to control the surface roughness.

喷涂法具有操作简单、易于实现、对涂覆的基体没有特殊要求、适用于室温下大面积涂层制备、现场应用性强等特点,是最适用于用于保护硅酸盐质文物的改性气相二氧化硅涂层材料的制备方法。因此,改性气相二氧化硅涂层可以在不改变硅酸盐基体本身原始形态及信息的前提下实现对其进行科学合理的保护,成为目前硅酸盐类文化遗产保护的杂化纳米材料亟需解决的问题。The spraying method has the characteristics of simple operation, easy implementation, no special requirements on the coated substrate, suitable for large-area coating preparation at room temperature, and strong field applicability. It is the most suitable modification for protecting silicate cultural relics. Preparation method of fumed silica coating material. Therefore, the modified fumed silica coating can achieve scientific and reasonable protection without changing the original form and information of the silicate matrix itself, and has become an urgent hybrid nanomaterial for the protection of silicate cultural heritage. problem to be solved.

发明内容Contents of the invention

本发明目的在于提出一种的用于保护硅酸盐质文物的改性气相二氧化硅涂层材料的制备方法,制备方法简单、快速,成本低,制备的产品喷涂在硅酸盐物质上形成的涂层具有优异的超疏水超疏油性能,透光性能,自清洁性能和耐久性的特点。The purpose of the present invention is to propose a method for preparing a modified fumed silica coating material used to protect silicate cultural relics. The preparation method is simple, fast, and low in cost. The prepared product is sprayed on the silicate material to form a The coating has the characteristics of excellent superhydrophobic and superoleophobic performance, light transmission performance, self-cleaning performance and durability.

为了实现上述目的,本发明采用以下技术方案。In order to achieve the above object, the present invention adopts the following technical solutions.

用于保护硅酸盐质文物的改性气相二氧化硅涂层材料的制备方法,包括如下步骤:A method for preparing a modified fumed silica coating material for protecting silicate cultural relics, comprising the following steps:

1)一次量取气相二氧化硅分散在混合溶剂中,得到浓度为1~10mg/mL的气相二氧化硅分散液;1) Measure the fumed silica at one time and disperse it in a mixed solvent to obtain a fumed silica dispersion with a concentration of 1-10 mg/mL;

2)按全氟辛基三氯硅烷与气相二氧化硅分散液的体积比为1:20,全氟辛基三氯硅烷与正硅酸四乙酯体积比为5:1,量取全氟辛基三氯硅烷及正硅酸四乙酯加入步骤1)得到的分散液中,磁力搅拌后形成均匀的白色溶液;2) According to the volume ratio of perfluorooctyl trichlorosilane to fumed silica dispersion liquid of 1:20, and the volume ratio of perfluorooctyl trichlorosilane to tetraethyl orthosilicate as 5:1, measure perfluorooctyl trichlorosilane Add octyltrichlorosilane and tetraethyl orthosilicate to the dispersion liquid obtained in step 1), and form a uniform white solution after magnetic stirring;

3)在步骤2)的白色溶液中滴加质量分数为25%~28%的氨水,边滴加边搅拌,滴加完毕之后再继续搅拌10~15min,边超声边搅拌至形成均匀悬浮液;3) Add dropwise ammonia water with a mass fraction of 25% to 28% in the white solution in step 2), and stir while dropping, and continue stirring for 10 to 15 minutes after the dropwise addition, and stir while ultrasonically until a uniform suspension is formed;

4)将步骤3)中的溶液超声分散并搅拌10~15min获得均匀的改性气相二氧化硅涂层材料。4) Ultrasonic dispersion of the solution in step 3) and stirring for 10-15 minutes to obtain a uniform modified fumed silica coating material.

进一步,所述步骤3)中滴加的氨水与步骤2)加入的全氟辛基三氯硅烷体积比为4:1。Further, the volume ratio of the ammonia water added dropwise in step 3) to the perfluorooctyltrichlorosilane added in step 2) is 4:1.

进一步,所述步骤1)中混合溶剂为乙醇和异丙醇,且体积比为1:1。Further, the mixed solvent in step 1) is ethanol and isopropanol, and the volume ratio is 1:1.

进一步,所述步骤2)中磁力搅拌时间为20-30min。Further, the magnetic stirring time in the step 2) is 20-30min.

进一步,所述步骤3)中搅拌时间为6h。Further, the stirring time in the step 3) is 6h.

进一步,所述步骤1)中气相二氧化硅分散在混合溶剂中,超声震荡15-20min充分分散,得到气相二氧化硅分散液。Further, in the step 1), the fumed silica is dispersed in the mixed solvent, and ultrasonically oscillated for 15-20 minutes to fully disperse to obtain a fumed silica dispersion.

进一步,所述步骤2)及步骤3)搅拌处理过程在室温25~30℃条件下进行。Further, the stirring process of step 2) and step 3) is carried out at a room temperature of 25-30°C.

本发明用于保护硅酸盐质文物的改性气相二氧化硅涂层材料的制备方法,选用气相二氧化硅提供粗糙结构,选用全氟辛基三氯硅烷提供低表面能,正硅酸四乙酯作为耦合剂,氨水作为水解促进剂,乙醇作为溶剂,在锥形瓶中形成凝胶,将分散均匀的凝胶通过喷涂法直接在玻璃基片上即可形成透明超疏水超疏油涂层。通过用正硅酸四乙酯和全氟辛基三氯硅烷改性气相二氧化硅,并将改性气相二氧化硅分散于乙醇中喷涂,即可形成透明超疏水超疏油涂层,制备方法简单快速,制备成本低,制备的产品具有优异的超疏水超疏油性能,透光性能,自清洁性能和耐久性的特点。The preparation method of the modified gas-phase silica coating material used for protecting silicate cultural relics in the present invention uses gas-phase silica to provide a rough structure, selects perfluorooctyltrichlorosilane to provide low surface energy, and tetra-orthosilicate Ethyl ester is used as a coupling agent, ammonia water is used as a hydrolysis accelerator, and ethanol is used as a solvent to form a gel in a conical flask, and the uniformly dispersed gel can be directly sprayed on a glass substrate to form a transparent super-hydrophobic and super-oleophobic coating. . By modifying fumed silica with tetraethylorthosilicate and perfluorooctyltrichlorosilane, and spraying the modified fumed silica in ethanol, a transparent superhydrophobic and superoleophobic coating can be formed, prepared The method is simple and quick, the preparation cost is low, and the prepared product has the characteristics of excellent superhydrophobic and superoleophobic performance, light transmission performance, self-cleaning performance and durability.

附图说明Description of drawings

图1为本发明实施例2中涂层的水的接触角Fig. 1 is the contact angle of the water of coating in the embodiment of the present invention 2

图2为本发明实施例2中涂层的十六烷的接触角Fig. 2 is the contact angle of the hexadecane of coating in embodiment 2 of the present invention

图3a为本发明实施例2中涂层的断面图Fig. 3 a is the sectional view of coating in embodiment 2 of the present invention

图3b为本发明实施例2中涂层的粗糙度三维图Figure 3b is a three-dimensional map of the roughness of the coating in Example 2 of the present invention

具体实施方式Detailed ways

下面结合具体实施例对本发明作进一步详细描述,但不作为对本发明的限定。The present invention will be described in further detail below in conjunction with specific examples, but not as a limitation of the present invention.

实施例1Example 1

1)一次量取200mg气相二氧化硅分散在10mL乙醇和10mL异丙醇中,置于超声机中超声15min,得到10mg/mL的均匀分散液;1) Measure 200mg of fumed silica at one time and disperse in 10mL of ethanol and 10mL of isopropanol, place it in an ultrasonic machine and sonicate for 15min to obtain a uniform dispersion of 10mg/mL;

2)量取1mL全氟辛基三氯硅烷及200μL正硅酸四乙酯加入步骤1)中的溶液,置于磁力搅拌器上搅拌20min,形成均匀的白色溶液;2) Measure 1 mL of perfluorooctyltrichlorosilane and 200 μL of tetraethyl orthosilicate to the solution in step 1), place on a magnetic stirrer and stir for 20 minutes to form a uniform white solution;

3)在步骤2)的溶液中滴加4mL质量分数为25%~28%的氨水,边滴加边搅拌,滴加完毕之后再继续搅拌10min,边超声边搅拌,至形成均匀悬浮液,搅拌6h;3) Add 4 mL of ammonia water with a mass fraction of 25% to 28% dropwise into the solution in step 2), and stir while adding dropwise, and continue stirring for 10 minutes after the dropwise addition is completed, stirring while ultrasonically until a uniform suspension is formed, and stir 6h;

4)将步骤3)中的溶液,超声分散10min,并搅拌获得均匀的改性气相二氧化硅涂层材料;4) Ultrasonic disperse the solution in step 3) for 10 minutes, and stir to obtain a uniform modified fumed silica coating material;

5)将3ml步骤4)中的涂层材料喷涂5层在玻璃基片上,即可形成薄的透明超疏水超疏油涂层。5) Spray 5 layers of 3ml of the coating material in step 4) on the glass substrate to form a thin transparent super-hydrophobic and super-oleophobic coating.

实施例2Example 2

1)一次量取100mg气相二氧化硅分散在10mL乙醇和10mL异丙醇中,置于超声机中超声20min,得到5mg/mL的均匀分散液;1) Disperse 100mg of fumed silica at one time in 10mL of ethanol and 10mL of isopropanol, and place it in an ultrasonic machine for 20min to obtain a uniform dispersion of 5mg/mL;

2)量取1mL全氟辛基三氯硅烷及200μL正硅酸四乙酯加入步骤1)中的分散液的溶液,置于磁力搅拌器上搅拌30min,形成均匀的白色溶液;2) Measure 1 mL of perfluorooctyltrichlorosilane and 200 μL of tetraethyl orthosilicate to the dispersion liquid in step 1), and place it on a magnetic stirrer to stir for 30 minutes to form a uniform white solution;

3)在步骤2)的所有白色溶液中滴加4mL质量分数为25%~28%的氨水,边滴加边搅拌,滴加完毕之后再继续搅拌10min,边超声边搅拌,至形成均匀悬浮液,搅拌6h;3) Add 4 mL of ammonia water with a mass fraction of 25% to 28% dropwise to all the white solution in step 2), and stir while adding dropwise, and continue stirring for 10 minutes after the dropwise addition is completed, stirring while ultrasonically until a uniform suspension is formed , stirring for 6h;

4)将步骤3)中所有溶液,超声分散12min,并搅拌获得均匀的改性气相二氧化硅涂层材料;4) Ultrasonic disperse all the solutions in step 3) for 12 minutes, and stir to obtain a uniform modified fumed silica coating material;

5)将3mL步骤4)中的涂层材料喷涂3层在玻璃基片上,即可形成薄的透明超疏水超疏油涂层。5) Spray 3 mL of the coating material in step 4) on the glass substrate to form a thin transparent super-hydrophobic and super-oleophobic coating.

图1中涂层的水的接触角为156.2°,体现了良好的超疏水性质。图2中十六烷的接触角为152.6°,表明该涂层达到超疏油的效果。图3a为本发明实施例2中涂层的断面图,图3b为本发明实施例2中涂层的粗糙度三维图,实施例2制备的超疏水超疏油涂层具有较大的粗糙度,粗糙度越大,表面留住的空气越多,固液接触面积越小,油或水接触角也越大。The water contact angle of the coating in Figure 1 is 156.2°, reflecting good superhydrophobic properties. The contact angle of hexadecane in Figure 2 is 152.6°, indicating that the coating achieves superoleophobic effect. Fig. 3 a is the sectional view of coating in the embodiment of the present invention 2, and Fig. 3 b is the three-dimensional figure of the roughness of the coating in the embodiment of the present invention 2, and the superhydrophobic superoleophobic coating prepared in embodiment 2 has larger roughness , the greater the roughness, the more air is retained on the surface, the smaller the solid-liquid contact area, and the larger the oil or water contact angle.

实施例3Example 3

1)一次量取20mg气相二氧化硅分散在10mL乙醇和10mL异丙醇中,置于超声机中超声18min,得到1mg/mL的均匀分散液;1) Disperse 20mg of fumed silica at one time in 10mL of ethanol and 10mL of isopropanol, and place it in an ultrasonic machine for 18min to obtain a uniform dispersion of 1mg/mL;

2)量取1mL全氟辛基三氯硅烷及200μL正硅酸四乙酯加入步骤1)中的分散液的溶液,置于磁力搅拌器上搅拌25min,形成均匀的白色溶液;2) Measure 1 mL of perfluorooctyltrichlorosilane and 200 μL of tetraethyl orthosilicate to the dispersion in step 1), and place on a magnetic stirrer to stir for 25 minutes to form a uniform white solution;

3)在步骤2)的所有白色溶液中滴加4mL质量分数为25%~28%的氨水,边滴加边搅拌,滴加完毕之后再继续搅拌15min,边超声边搅拌,至形成均匀悬浮液,搅拌6h;3) Add 4 mL of ammonia water with a mass fraction of 25% to 28% dropwise to all the white solution in step 2), and stir while adding dropwise, and continue stirring for 15 minutes after the dropwise addition, and stir while ultrasonically until a uniform suspension is formed , stirring for 6h;

4)将步骤3)中的溶液,超声分散15min,并搅拌获得均匀的改性气相二氧化硅涂层材料;4) Ultrasonic disperse the solution in step 3) for 15 minutes, and stir to obtain a uniform modified fumed silica coating material;

5)将4mL步骤4)中的涂层材料喷涂3层在玻璃基片上,即可形成薄的透明超疏水超疏油涂层。5) Spray 4 mL of the coating material in step 4) 3 layers on the glass substrate to form a thin transparent super-hydrophobic and super-oleophobic coating.

表1透明超疏水超疏油涂层的润湿性和透明性Table 1 Wettability and transparency of transparent superhydrophobic and superoleophobic coatings

表1为本发明实施例1,2,3中涂层的润湿性和透明性比较。实施例1中制备的涂层原子力显微镜(AFM)为132±15nm,透明度75.6%;实施例2中原子力显微镜(AFM)为104±26nm,透明度82.3%,实施例3中原子力显微镜(AFM)为61±13nm,透明度84.2%。AFM越大,粗糙度越大,导致涂层的透明度越小,而实施例2和3的透明度相近。实施例3的油(正十六烷)和水接触角分别为150.8°和153.5°,均低于实施例2制备的涂层152.6°和156.2°,而滚动角相差不大,结果表明,透明度不变的条件下,粗糙度越大,其接触角也就越大。Table 1 is a comparison of the wettability and transparency of the coatings in Examples 1, 2, and 3 of the present invention. The coating atomic force microscope (AFM) prepared in embodiment 1 is 132 ± 15nm, transparency 75.6%; In embodiment 2, atomic force microscope (AFM) is 104 ± 26nm, transparency 82.3%, in embodiment 3 atomic force microscope (AFM) is 61±13nm, transparency 84.2%. The larger the AFM, the larger the roughness, resulting in less transparency of the coating, while the transparency of Examples 2 and 3 is similar. The oil (n-hexadecane) of embodiment 3 and water contact angle are respectively 150.8 ° and 153.5 °, are all lower than the coating 152.6 ° and 156.2 ° that embodiment 2 prepares, and rolling angle differs little, and the result shows, transparency Under the same conditions, the greater the roughness, the greater the contact angle.

最后应该说明的是:以上实施例仅用于说明本发明的技术方案而非对其限制,尽管参照上述实施例对本发明进行了详细说明,所属领域的普通技术人员应当理解:依然可以对本发明的具体实施方式进行修改或者等同替换,而未脱离本发明精神和范围的任何修改或者等同替换,其均应涵盖在本权利要求范围当中。Finally, it should be noted that: the above embodiments are only used to illustrate the technical solutions of the present invention and not to limit them. Although the present invention has been described in detail with reference to the above embodiments, those of ordinary skill in the art should understand that: the present invention can still be Modifications or equivalent replacements to the specific embodiments, any modification or equivalent replacement that does not depart from the spirit and scope of the present invention, shall be covered by the scope of the present claims.

Claims (7)

1. the preparation method of the modification fumed silica coating material for protecting silicate cultural relic, it is characterised in that including Following steps:
1) it once measures fumed silica and is dispersed in the mixed solvent, obtain the fumed silica that concentration is 1~10mg/mL Dispersion liquid;
2) be 1:20 by the volume ratio of perfluoro capryl trichlorosilane and fumed silica dispersion liquid, perfluoro capryl trichlorosilane with Tetraethyl orthosilicate volume ratio is 5:1, measures perfluoro capryl trichlorosilane and point that step 1) obtains is added in tetraethyl orthosilicate Uniform white solution is formed in dispersion liquid, after magnetic agitation;
3) ammonium hydroxide that mass fraction is 25%~28% is added dropwise in the white solution of step 2), stirs, drips when being added dropwise 10~15min of stirring is further continued for after finishing, Bian Chaosheng is stirred on side to formation unit for uniform suspension;
4) by the solution ultrasonic disperse in step 3) and the uniform modified fumed silica coating material of stirring 10~15min acquisition Material.
2. the preparation of the modification fumed silica coating material according to claim 1 for protecting silicate cultural relic Method, which is characterized in that the perfluoro capryl trichlorosilane volume ratio that the ammonium hydroxide being added dropwise in the step 3) is added with step 2) is 4:1.
3. the preparation side of the modification fumed silica coating material as described in claim 1 for protecting silicate cultural relic Method, it is characterised in that: mixed solvent is ethyl alcohol and isopropanol in the step 1), and volume ratio is 1:1.
4. the preparation side of the modification fumed silica coating material as described in claim 1 for protecting silicate cultural relic Method, it is characterised in that: the magnetic agitation time is 20-30min in the step 2).
5. the preparation side of the modification fumed silica coating material as described in claim 1 for protecting silicate cultural relic Method, it is characterised in that: mixing time is 6h in the step 3).
6. the preparation side of the modification fumed silica coating material as described in claim 1 for protecting silicate cultural relic Method, it is characterised in that: fumed silica is dispersed in the mixed solvent in the step 1), and ultrasonic vibration 15-20min sufficiently divides It dissipates, obtains fumed silica dispersion liquid.
7. the preparation of the modification fumed silica coating material according to claim 1 for protecting silicate cultural relic Method, which is characterized in that the step 2) and step 3) stir process process carry out under the conditions of 25~30 DEG C of room temperature.
CN201910976885.1A 2019-10-15 2019-10-15 Preparation method of modified fumed silica coating material for protecting silicate cultural relics Pending CN110511600A (en)

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Application publication date: 20191129