CN112359361A - Super-hydrophobic surface treating agent and preparation method and application thereof - Google Patents
Super-hydrophobic surface treating agent and preparation method and application thereof Download PDFInfo
- Publication number
- CN112359361A CN112359361A CN202011103301.9A CN202011103301A CN112359361A CN 112359361 A CN112359361 A CN 112359361A CN 202011103301 A CN202011103301 A CN 202011103301A CN 112359361 A CN112359361 A CN 112359361A
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- Prior art keywords
- treating agent
- surface treating
- silica sol
- super
- nano silica
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- Pending
Links
- 230000003075 superhydrophobic effect Effects 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title abstract description 14
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 58
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 38
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000002253 acid Substances 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 15
- 239000003381 stabilizer Substances 0.000 claims abstract description 14
- 239000011259 mixed solution Substances 0.000 claims description 26
- 239000012756 surface treatment agent Substances 0.000 claims description 22
- 238000003756 stirring Methods 0.000 claims description 18
- 230000002209 hydrophobic effect Effects 0.000 claims description 14
- 239000000243 solution Substances 0.000 claims description 14
- ZNQVEEAIQZEUHB-UHFFFAOYSA-N 2-ethoxyethanol Chemical compound CCOCCO ZNQVEEAIQZEUHB-UHFFFAOYSA-N 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 8
- LYCAIKOWRPUZTN-UHFFFAOYSA-N ethylene glycol Natural products OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- -1 siloxane, ethylene Chemical group 0.000 claims description 4
- OAYXUHPQHDHDDZ-UHFFFAOYSA-N 2-(2-butoxyethoxy)ethanol Chemical compound CCCCOCCOCCO OAYXUHPQHDHDDZ-UHFFFAOYSA-N 0.000 claims description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 3
- 238000004381 surface treatment Methods 0.000 claims 1
- 230000005661 hydrophobic surface Effects 0.000 abstract description 14
- 239000002184 metal Substances 0.000 abstract description 8
- 239000002994 raw material Substances 0.000 abstract description 4
- 230000003670 easy-to-clean Effects 0.000 abstract description 3
- 239000007787 solid Substances 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 28
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 229940028356 diethylene glycol monobutyl ether Drugs 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- JCGNDDUYTRNOFT-UHFFFAOYSA-N oxolane-2,4-dione Chemical compound O=C1COC(=O)C1 JCGNDDUYTRNOFT-UHFFFAOYSA-N 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F14/00—Inhibiting incrustation in apparatus for heating liquids for physical or chemical purposes
- C23F14/02—Inhibiting incrustation in apparatus for heating liquids for physical or chemical purposes by chemical means
Abstract
The invention discloses a super-hydrophobic surface treating agent and a preparation method thereof, wherein the super-hydrophilic surface treating agent comprises the following components in percentage by mass: 5.0-8.0% of modified nano silica sol, 0.1-0.5% of stabilizer, 0.5-1.5% of fluosilicic acid and the balance of pure water. The hydrophobic surface treating agent provided by the invention is reasonable in components, safe and effective, can be used for a long time, has the density of 0.93-1.00 relative to water and the pH of 3-4, and thus lays a solid foundation for a process for treating a metal surface by selecting the hydrophobic surface treating agent; in addition, the surface treating agent provided by the invention is simple in preparation process, easy in raw material obtaining, excellent in easy-to-clean property and worthy of great popularization and application.
Description
Technical Field
The invention belongs to the technical field of metal surface processing, and particularly relates to a super-hydrophobic surface treating agent, and a preparation method and application thereof.
Background
The steam generating device of the steam box and the steam baking all-in-one machine can heat water to convert the water into high-temperature steam, and the surface of the steam generating device can be scaled after the steam generating device is used for a long time, so that the heating efficiency of the steam generating device can be reduced, and the temperature control precision can be influenced; part of the massive scale can fall off in a massive mode, and the fallen scale can block a pipeline, so that the machine cannot be normally used.
In order to solve the problems, the scale removal method of the products on the market at present adopts a scale remover such as citric acid and the like for cleaning, but the frequent use can affect the health of the human body; the water pump is additionally arranged for cleaning, but the scale cleaning effect is not ideal because the scale is adhered to the surface of the evaporator; therefore, the research on new surface treatment agents capable of solving the problem of easy scaling of metal surfaces is still a major challenge at the present stage.
Disclosure of Invention
In view of the above, the main object of the present invention is to provide a super-hydrophobic surface treatment agent, which enables a metal surface to be in a super-hydrophobic state after the metal surface is treated by the surface treatment agent, thereby solving the problem that the metal surface is easy to scale after long-term use.
The invention also aims to provide a preparation method of the super-hydrophobic surface treating agent;
the invention also aims to provide application of the super-hydrophobic surface treating agent.
In order to achieve the purpose, the technical scheme of the invention is realized as follows: the super-hydrophobic surface treatment agent comprises the following components in percentage by weight:
preferably, 5-8% of modified nano silica sol, 0.1-0.5% of stabilizer, 0.5-1.5% of fluosilicic acid and the balance of pure water.
Preferably, the modified nano silica sol is hydrophobic nano silica sol.
Preferably, the stabilizer is at least one of ethylene glycol ethyl ether, dimethyl siloxane, ethylene glycol butyl ether and diethylene glycol butyl ether.
Preferably, the relative density of the super-hydrophobic surface treatment agent is 0.93-1.00; the pH value is 3-4.
The second technical scheme of the invention is realized as follows: the preparation method of the super-hydrophobic surface treating agent is realized by the following steps:
s1, respectively weighing the following components in percentage by weight: 5-8% of modified nano silica sol, 0.1-0.5% of stabilizer, 0.5-1.5% of fluosilicic acid and the balance of pure water;
s2, heating the water in the S1 to 45-55 ℃, adding the modified nano silica sol into the water, keeping the temperature of 45-55 ℃, stirring for at least 10min, and cooling to room temperature to obtain a first intermediate mixed solution;
s3, adding the stabilizer obtained in the S1 into the first intermediate mixed solution obtained in the S2, and stirring for at least 30min to obtain a second intermediate mixed solution;
s4, adding the fluosilicic acid obtained in the step S1 into the second intermediate mixed solution obtained in the step S3, and adjusting the pH value to 3-4 to obtain a crude surface treating agent solution;
s5, filtering the crude surface treating agent solution obtained in the step S4 to obtain the colorless transparent liquid super-hydrophobic surface treating agent.
Preferably, in the step S2, the stirring time is 10-20 min;
preferably, in the step S3, the stirring time is 30-40 min.
Preferably, in S5, a 400-450 mesh screen is used for filtering.
Compared with the prior art, the hydrophobic surface treating agent provided by the invention is reasonable in components, safe and effective, can be used for a long time, has the density of 0.93-1.00 relative to water and the pH of 3-4, and thus lays a solid foundation for the process of treating the metal surface by selecting the hydrophobic surface treating agent; in addition, the surface treating agent provided by the invention is simple in preparation process, easy in raw material obtaining, excellent in easy-to-clean property and worthy of great popularization and application.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
It should be noted that: the raw material components used in the examples of the present invention may be prepared by themselves or purchased.
The super-hydrophobic surface treating agent provided by the embodiment of the invention comprises the following components in percentage by weight:
5-8% of modified nano silica sol, 0.1-0.5% of stabilizer, 0.5-1.5% of fluosilicic acid and the balance of pure water.
Wherein the modified nano silica sol is hydrophobic nano silica sol; the stabilizer is at least one of ethylene glycol ethyl ether, dimethyl siloxane, ethylene glycol butyl ether and diethylene glycol butyl ether.
Furthermore, the method is simple. The relative density of the super-hydrophobic surface treatment agent is 0.93-1.00; the pH value is 3-4.
The embodiment of the invention also provides a preparation method of the super-hydrophobic surface treating agent, which is realized by the following steps:
s1, respectively weighing the following components in percentage by weight: 5-8% of modified nano silica sol, 0.1-0.5% of stabilizer, 0.5-1.5% of fluosilicic acid and the balance of pure water;
s2, heating the water in the S1 to 45-55 ℃, adding the modified nano silica sol into the water, keeping the temperature of 45-55 ℃, stirring for at least 10min, preferably 10-20 min, and cooling to room temperature to obtain a first intermediate mixed solution;
s3, adding the stabilizer obtained in the S1 into the first intermediate mixed solution obtained in the S2, and stirring for at least 30min, preferably 30-40 min to obtain a second intermediate mixed solution;
s4, adding the fluosilicic acid obtained in the step S1 into the second intermediate mixed solution obtained in the step S3, and adjusting the pH value to 3-4 to obtain a crude surface treating agent solution;
and S5, filtering the crude surface treating agent solution obtained in the step S4 by using a 400-450-mesh filter screen to obtain a colorless transparent liquid super-hydrophobic surface treating agent.
The following are specific examples
Example 1
The hydrophobic surface treating agent provided by the embodiment 1 of the invention comprises the following components in percentage by weight:
6.5 percent of hydrophobic nano silica sol, 0.3 percent of ethylene glycol ethyl ether, 1.0 percent of fluosilicic acid and the balance of pure water.
The hydrophobic surface treating agent provided by the embodiment 1 of the invention is obtained by the following steps:
s1, respectively weighing the following components in percentage by weight: 6.5 percent of hydrophobic nano silica sol, 0.3 percent of ethylene glycol ethyl ether, 1.0 percent of fluosilicic acid and the balance of pure water;
s2, heating the water in the S1 to 50 ℃, adding the hydrophobic nano silica sol into the water, keeping the temperature of 50 ℃, stirring for 15min, and cooling to room temperature to obtain a first intermediate mixed solution;
s3, adding the ethylene glycol ethyl ether obtained in the S1 into the first intermediate mixed solution obtained in the S2, and stirring for 35min to obtain a second intermediate mixed solution;
s4, adding the fluosilicic acid obtained in the step S1 into the second intermediate mixed solution obtained in the step S3, and adjusting the pH value to 3-4 to obtain a crude surface treating agent solution;
and S5, filtering the crude surface treating agent solution obtained in the step S4 by using a 400-450-mesh filter screen to obtain a colorless transparent liquid super-hydrophobic surface treating agent.
Example 2
The hydrophobic surface treating agent provided by the embodiment 2 of the invention comprises the following components in percentage by weight:
5.0 percent of hydrophobic nano silica sol, 0.1 percent of ethylene glycol ethyl ether, 0.5 percent of fluosilicic acid and the balance of pure water.
The hydrophobic surface treating agent provided by the embodiment 2 of the invention is obtained by the following steps:
s1, respectively weighing the following components in percentage by weight: 5.0 percent of hydrophobic nano silica sol, 0.1 percent of ethylene glycol ethyl ether, 0.5 percent of fluosilicic acid and the balance of pure water;
s2, heating the water in the S1 to 50 ℃, adding the hydrophobic nano silica sol into the water, keeping the temperature at 45 ℃, stirring for 10min, and cooling to room temperature to obtain a first intermediate mixed solution;
s3, adding the ethylene glycol ethyl ether obtained in the S1 into the first intermediate mixed solution obtained in the S2, and stirring for 30min to obtain a second intermediate mixed solution;
s4, adding the fluosilicic acid obtained in the step S1 into the second intermediate mixed solution obtained in the step S3, and adjusting the pH value to 3-4 to obtain a crude surface treating agent solution;
and S5, filtering the crude surface treating agent solution obtained in the step S4 by using a 400-450-mesh filter screen to obtain a colorless transparent liquid super-hydrophobic surface treating agent.
Example 3
The hydrophobic surface treating agent provided by the embodiment 3 of the invention comprises the following components in percentage by weight:
8.0 percent of hydrophobic nano silica sol, 0.5 percent of ethylene glycol ethyl ether, 1.5 percent of fluosilicic acid and the balance of pure water.
The hydrophobic surface treating agent provided by the embodiment 3 of the invention is obtained by the following steps:
s1, respectively weighing the following components in percentage by weight: 8.0 percent of hydrophobic nano silica sol, 0.5 percent of ethylene glycol ethyl ether, 1.5 percent of fluosilicic acid and the balance of pure water;
s2, heating the water in the S1 to 55 ℃, adding the hydrophobic nano silica sol into the water, keeping the temperature of 55 ℃, stirring for 20min, and cooling to room temperature to obtain a first intermediate mixed solution;
s3, adding the ethylene glycol ethyl ether obtained in the S1 into the first intermediate mixed solution obtained in the S2, and stirring for 40min to obtain a second intermediate mixed solution;
s4, adding the fluosilicic acid obtained in the step S1 into the second intermediate mixed solution obtained in the step S3, and adjusting the pH value to 3-4 to obtain a crude surface treating agent solution;
and S5, filtering the crude surface treating agent solution obtained in the step S4 by using a 400-450-mesh filter screen to obtain a colorless transparent liquid super-hydrophobic surface treating agent.
Example 4
The hydrophobic surface treating agent provided by the embodiment 4 of the invention comprises the following components in percentage by weight:
5.0 percent of hydrophobic nano-silica sol, 0.5 percent of dimethyl siloxane, 0.5 percent of fluosilicic acid and the balance of pure water.
The preparation method of the hydrophobic surface treating agent provided by the embodiment 4 of the invention is the same as that of the embodiment 1.
Example 5
The hydrophobic surface treating agent provided by the embodiment 5 of the invention comprises the following components in percentage by weight:
8.0 percent of hydrophobic nano silica sol, 0.1 percent of diethylene glycol monobutyl ether, 1.5 percent of fluosilicic acid and the balance of pure water.
The preparation method of the hydrophobic surface treating agent provided by the embodiment 5 of the invention is the same as that of the embodiment 1.
Comparative example 1
The components and content of a surface treatment agent provided in comparative example 1 of the present invention are substantially the same as those of the surface treatment agent of example 1, except that comparative example 1 does not contain a modified nano silica sol.
In addition, comparative example 1 of the present invention provides a surface treating agent prepared by the same method as example 1.
Comparative example 2
The components and content of the surface treating agent provided by comparative example 2 of the invention are basically the same as those of the surface treating agent in example 1, except that the modified nano silica sol in comparative example 2 is 4.0%.
In addition, comparative example 2 of the present invention provides a surface treating agent prepared by the same method as example 1.
Comparative example 3
The components and content of the surface treating agent provided by comparative example 3 of the present invention are substantially the same as those of the surface treating agent of example 1, except that the modified nano silica sol of comparative example 3 is 9.0%.
In addition, comparative example 3 of the present invention provides a surface treating agent prepared by the same method as example 1.
Comparative example 4
Comparative example 4 of the present invention provides a surface treatment agent having the same composition and content as those of the surface treatment agent of example 1, but the preparation method of the surface treatment agent of comparative example 4 is different from that of example 1 in that: heating the water in S1 to 40 ℃, adding the modified nano-silica sol into the water, keeping the temperature of 40 ℃, stirring for at least 10min, and cooling to room temperature to obtain a first intermediate mixed solution.
Comparative example 5
Comparative example 5 of the present invention provides a surface treatment agent having the same composition and content as those of the surface treatment agent composition of example 1, but the preparation method of the surface treatment agent of comparative example 5 is different from that of example 1 in that: heating the water in S1 to 60 ℃, adding the modified nano-silica sol into the water, keeping the temperature of 60 ℃, stirring for at least 10min, and cooling to room temperature to obtain a first intermediate mixed solution.
In order to verify the density of the phase and the pH of the surface treatment agents obtained in examples 1 to 5 and comparative examples 1 to 5 of the present invention, the density of the phase and the pH of the surface treatment agents obtained in examples 1 to 5 and comparative examples 1 to 5 were measured, and the results were as follows:
TABLE 1 results of examining the properties of the surface-treating agents obtained in examples 1 to 5 and comparative examples 1 to 5
Density of phase density | pH value | |
Example 1 | 1.00 | 3~4 |
Example 2 | 0.98 | 3~4 |
Example 3 | 0.95 | 3~4 |
Example 4 | 0.93 | 3~4 |
Example 5 | 0.94 | 3~4 |
Comparative example 1 | 0.70 | 2~2.5 |
Comparative example 2 | 0.80 | 2~2.5 |
Comparative example 3 | 0.85 | 2~2.5 |
Comparative example 4 | 0.84 | 3.5~4 |
Comparative example 5 | 0.81 | 3.5~4 |
According to the specific contents of the examples 1 to 5 and the comparative examples 1 to 5 and by combining the data in the table 1, when any one of the selected modified nano silica sol, the stabilizer and the fluosilicic acid and the content of each component are not in the content range set by the scheme of the application, or the modified nano silica sol is not contained, the relative density of the obtained surface treating agent is not in the range of 0.93-1.00, and the pH value is not in the range of 3-4; in addition, according to the specific contents of example 1 and comparative examples 4 and 5 and the data in table 1, in the process of preparing the surface treating agent, when the heating temperature of water is not in the temperature range set by the scheme of the application, the relative density of the obtained surface treating agent is not in the range of 0.93-1.00, and the pH value is not in the range of 3-4; therefore, in order to obtain a surface treatment agent having a relative density of 0.93 to 1.00 and a pH of 3 to 4, the components and the content ranges of the components set in the present embodiment should be satisfied, and the process parameters for preparing the surface treatment agent should be within the ranges set in the present embodiment.
In conclusion, the surface treating agent provided by the invention is reasonable in components, safe and effective, can be used for a long time, has the density of 0.93-1.00 relative to water and the pH value of 3-4, and lays a solid foundation for the process for treating the metal surface by selecting the surface treating agent; in addition, the surface treating agent provided by the invention is simple in preparation process, easy in raw material obtaining, excellent in easy-to-clean property and worthy of great popularization and application.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (8)
1. The super-hydrophobic surface treatment agent is characterized by comprising the following components in percentage by weight:
5.0-8.0% of modified nano silica sol, 0.1-0.5% of stabilizer, 0.5-1.5% of fluosilicic acid and the balance of pure water.
2. The super-hydrophobic surface treating agent according to claim 1, wherein the modified nano silica sol is a hydrophobic nano silica sol.
3. The superhydrophobic surface treatment according to claim 1, wherein the stabilizer is at least one of ethylene glycol ethyl ether, dimethyl siloxane, ethylene glycol butyl ether, and diethylene glycol butyl ether.
4. The superhydrophobic surface treatment agent according to any one of claims 1-3, wherein the relative density of the superhydrophobic surface treatment agent is 0.93-1.00; the pH value is 3-4.
5. A method for preparing the superhydrophobic surface treatment agent according to any one of claims 1-4, wherein the method is realized by the following steps:
s1, respectively weighing the following components in percentage by weight: 5-8% of modified nano silica sol, 0.1-0.5% of stabilizer, 0.5-1.5% of fluosilicic acid and the balance of pure water;
s2, heating the water in the S1 to 45-55 ℃, adding the modified nano silica sol into the water, keeping the temperature of 45-55 ℃, stirring for at least 10min, and cooling to room temperature to obtain a first intermediate mixed solution;
s3, adding the stabilizer obtained in the S1 into the first intermediate mixed solution obtained in the S2, and stirring for at least 30min to obtain a second intermediate mixed solution;
s4, adding the fluosilicic acid obtained in the step S1 into the second intermediate mixed solution obtained in the step S3, and adjusting the pH value to 3-4 to obtain a crude surface treating agent solution;
s5, filtering the crude surface treating agent solution obtained in the step S4 to obtain the colorless transparent liquid super-hydrophobic surface treating agent.
6. The method of claim 5, wherein the stirring time in S2 is 10-20 min.
7. The method of claim 6, wherein the stirring time in S3 is 30-40 min.
8. The method according to claim 7, wherein in S5, a 400-450 mesh screen is used for filtering.
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CN202011103301.9A CN112359361A (en) | 2020-10-15 | 2020-10-15 | Super-hydrophobic surface treating agent and preparation method and application thereof |
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CN102220036A (en) * | 2011-06-02 | 2011-10-19 | 北京化工大学 | Method for preparing white carbon black modified by silane coupling agent |
CN104854203A (en) * | 2012-12-21 | 2015-08-19 | 荷兰联合利华有限公司 | Composition for hydrophobic coating |
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Application publication date: 20210212 |