CN111663133A - Silane treatment fluid and preparation method thereof - Google Patents

Silane treatment fluid and preparation method thereof Download PDF

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Publication number
CN111663133A
CN111663133A CN201910166590.8A CN201910166590A CN111663133A CN 111663133 A CN111663133 A CN 111663133A CN 201910166590 A CN201910166590 A CN 201910166590A CN 111663133 A CN111663133 A CN 111663133A
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CN
China
Prior art keywords
silane
silane treatment
stirring
water
treatment liquid
Prior art date
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Pending
Application number
CN201910166590.8A
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Chinese (zh)
Inventor
石琴
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Nanjing Painuo Metal Surface Treatment Technology Co ltd
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Nanjing Painuo Metal Surface Treatment Technology Co ltd
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Publication date
Application filed by Nanjing Painuo Metal Surface Treatment Technology Co ltd filed Critical Nanjing Painuo Metal Surface Treatment Technology Co ltd
Priority to CN201910166590.8A priority Critical patent/CN111663133A/en
Publication of CN111663133A publication Critical patent/CN111663133A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C22/00Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C22/05Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
    • C23C22/06Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
    • C23C22/48Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 not containing phosphates, hexavalent chromium compounds, fluorides or complex fluorides, molybdates, tungstates, vanadates or oxalates

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  • Chemical & Material Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Application Of Or Painting With Fluid Materials (AREA)

Abstract

The invention discloses a silane treating fluid, which comprises 10-30% of epoxy silane, 2-20% of oxalic acid and 60-80% of water, wherein the thickness of a silane film of a cold-rolled sheet formed by the cold-rolled sheet treated by the silane treating fluid is micron-sized and far thicker than the original nanometer-sized thickness, and the silane treating fluid can be placed in the air for at least 20 days without rusting.

Description

Silane treatment fluid and preparation method thereof
[ technical field ] A method for producing a semiconductor device
The invention relates to the field of chemical industry, in particular to a silane treatment fluid and a preparation method thereof.
[ background of the invention ]
In the face of environmental protection pressure, the phosphating treatment of the cold-rolled sheet before coating is gradually replaced by a silane technology, but the silane has extremely poor corrosion resistance, a silane treatment film formed by the cold-rolled sheet can only be placed for 2 to 3 days generally, and the silane treatment film can rust in one day basically in plum rain season, so that the popularization and the use of the silane are greatly restricted.
Accordingly, there is a need to provide an improved silane treatment fluid and method of making the same that is a problem in the art that needs to be addressed.
[ summary of the invention ]
Aiming at the problems, the invention provides the silane treatment fluid and the preparation method thereof, and the silane treatment film has good bonding force with paint and strong corrosion resistance.
In order to solve the problems, the invention provides a silane treatment fluid, which comprises 10-30% of epoxy silane, 2-20% of oxalic acid and 60-80% of water.
Further, 25% of epoxy silane, 5% of oxalic acid and 70% of water.
In order to solve the above problems, the present invention also provides a method for preparing a silane treatment liquid, comprising the steps of: firstly, taking a certain amount of water, then adding epoxy silane, stirring while adding epoxy silane, finally adding a certain amount of oxalic acid after forming a uniform and clear solution, and stirring for a certain time.
Further, the stirring time during the addition of the epoxy silane is 1.5h-3 h.
Further, the stirring time after adding the oxalic acid is 25-35 min.
Compared with the prior art, the invention has the following advantages:
1. the thickness of the cold-rolled sheet silane film formed by the cold-rolled sheet treated by the silane treatment solution is micron-sized, is far thicker than the original nanometer-sized thickness, and can not rust after being placed in the air for at least 20 days.
2. The film layer formed by the silane treatment fluid has good binding force with paint, and the binding force of the paint after paint spraying reaches 0 grade or 1 grade.
[ description of the drawings ]
Is free of
[ detailed description ] embodiments
The silane treatment fluid comprises 10-30% of epoxy silane, 2-20% of oxalic acid and 60-80% of water, and the preparation method of the silane treatment fluid comprises the following steps: adding water into a stirring kettle, adding epoxy silane at normal temperature, adding epoxy silane into water while stirring for 2 hours, adding a certain amount of oxalic acid after a uniform and clear solution is formed, stirring for 30 minutes, and taking out of the kettle.
Coating silane treatment liquid with the concentration of 0.1-10% on the surface of the cold-rolled plate, wherein the treatment time is 30 s-10 min.
Example 1:
the silane treatment fluid comprises the following raw material components in percentage by weight: 25% of epoxy silane, 5% of oxalic acid and 70% of water, and the preparation method of the silane treatment fluid comprises the following steps: firstly, adding water into a stirring kettle, then adding epoxy silane into the water while stirring for 1.5 hours, finally adding a certain amount of oxalic acid after a uniform and clear solution is formed, stirring for 40 minutes, and taking out of the kettle. And adding water into the prepared silane treatment liquid to dilute the silane treatment liquid to the concentration of 5%, then coating the silane treatment liquid on the surface of the cold-rolled plate, wherein the treatment time is 3min, the treated cold-rolled plate does not rust after being placed in the air for 35 days, and the bonding force between the silane treatment liquid and the paint reaches 0 grade after the paint is sprayed on the surface of the cold-rolled plate treated by the silane treatment liquid.
Example 2:
the silane treatment fluid comprises the following raw material components in percentage by weight: 10% of epoxy silane, 20% of oxalic acid and 70% of water, and the preparation method of the silane treatment fluid comprises the following steps: firstly, adding water into a stirring kettle, then adding epoxy silane into the water while stirring for 3 hours, finally adding a certain amount of oxalic acid after a uniform and clear solution is formed, stirring for 35 minutes, and taking out of the kettle. And adding water into the prepared silane treatment liquid to dilute the silane treatment liquid to the concentration of 0.1%, then coating the silane treatment liquid on the surface of the cold-rolled plate, wherein the treatment time is 10min, the treated cold-rolled plate is not rusted after being placed in the air for 25 days, and after the surface of the cold-rolled plate treated by the silane treatment liquid is sprayed with paint, the bonding force between the silane treatment liquid and the paint reaches level 1.
Example 3:
the silane treatment fluid comprises the following raw material components in percentage by weight: 30% of epoxy silane, 2% of oxalic acid and 65% of water, and the preparation method of the silane treatment fluid comprises the following steps: firstly, adding water into a stirring kettle, then adding epoxy silane into the water while stirring for 2 hours, finally adding a certain amount of oxalic acid after a uniform and clear solution is formed, stirring for 38 minutes, and taking out of the kettle. And adding water into the prepared silane treatment liquid to dilute the silane treatment liquid to the concentration of 5%, then coating the silane treatment liquid on the surface of the cold-rolled plate, wherein the treatment time is 8min, the treated cold-rolled plate does not rust after being placed in the air for 20 days, and after the surface of the cold-rolled plate treated by the silane treatment liquid is sprayed with paint, the bonding force between the silane treatment liquid and the paint reaches level 1.
Example 4:
the silane treatment fluid comprises the following raw material components in percentage by weight: 30% of epoxy silane, 10% of oxalic acid and 60% of water, and the preparation method of the silane treatment fluid comprises the following steps: firstly, adding water into a stirring kettle, then adding epoxy silane into the water while stirring for 3 hours, finally adding a certain amount of oxalic acid after a uniform and clear solution is formed, stirring for 25 minutes, and taking out of the kettle. And adding water into the prepared silane treatment liquid to dilute the silane treatment liquid to the concentration of 2%, then coating the silane treatment liquid on the surface of a cold-rolled plate, wherein the treatment time is 30s, the treated cold-rolled plate does not rust after being placed in the air for 30 days, and after the surface of the cold-rolled plate treated by the silane treatment liquid is sprayed with paint, the bonding force between the silane treatment liquid and the paint reaches 0 grade.
Example 5:
the silane treatment fluid comprises the following raw material components in percentage by weight: 15% of epoxy silane, 5% of oxalic acid and 80% of water, and the preparation method of the silane treatment fluid comprises the following steps: firstly, adding water into a stirring kettle, then adding epoxy silane into the water while stirring for 2 hours, finally adding a certain amount of oxalic acid after a uniform and clear solution is formed, stirring for 30 minutes, and taking out of the kettle. And adding water into the prepared silane treatment liquid to dilute the silane treatment liquid to a concentration of 10%, then coating the silane treatment liquid on the surface of a cold-rolled plate, wherein the treatment time is 3min, the treated cold-rolled plate does not rust after being placed in the air for 28 days, and after the surface of the cold-rolled plate treated by the silane treatment liquid is sprayed with paint, the bonding force between the silane treatment liquid and the paint reaches 0 grade.
The invention has the advantages that:
1. the thickness of the cold-rolled sheet silane film formed by the cold-rolled sheet treated by the silane treatment solution is micron-sized, is far thicker than the original nanometer-sized thickness, and can not rust after being placed in the air for at least 20 days.
2. The film layer formed by the silane treatment fluid has good binding force with paint, and the binding force of the paint after paint spraying reaches 0 grade or 1 grade.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.

Claims (5)

1. The silane treatment fluid is characterized by comprising 10-30% of epoxy silane, 2-20% of oxalic acid and 60-80% of water.
2. The silane treatment liquid according to claim 1, wherein the epoxy silane comprises 25% by weight of epoxy silane, 5% by weight of oxalic acid, and 70% by weight of water.
3. A method for producing the silane treatment liquid according to any one of claims 1 to 2, comprising the steps of: firstly, taking a certain amount of water, then adding epoxy silane, stirring while adding epoxy silane, finally adding a certain amount of oxalic acid after forming a uniform and clear solution, and stirring for a certain time.
4. The method of producing a silane treatment liquid according to claim 3, wherein the time for stirring when the epoxysilane is added is 1.5 hours to 3 hours.
5. The method of claim 3, wherein the stirring time after the oxalic acid is added is 25 to 35 min.
CN201910166590.8A 2019-03-06 2019-03-06 Silane treatment fluid and preparation method thereof Pending CN111663133A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201910166590.8A CN111663133A (en) 2019-03-06 2019-03-06 Silane treatment fluid and preparation method thereof

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Application Number Priority Date Filing Date Title
CN201910166590.8A CN111663133A (en) 2019-03-06 2019-03-06 Silane treatment fluid and preparation method thereof

Publications (1)

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CN111663133A true CN111663133A (en) 2020-09-15

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Country Status (1)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103215630A (en) * 2013-04-23 2013-07-24 沈阳理工大学 Method for sealing aluminum alloy anode oxide film pore by adopting organic-inorganic composite silica sol
CN104630765A (en) * 2013-11-11 2015-05-20 安徽未来表面技术有限公司 Environmental-protection type metal coating pre-treatment agent and preparation method thereof
CN106756976A (en) * 2016-11-26 2017-05-31 浙江五源科技股份有限公司 Silane compound and its application for chemical composition coating post processing

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103215630A (en) * 2013-04-23 2013-07-24 沈阳理工大学 Method for sealing aluminum alloy anode oxide film pore by adopting organic-inorganic composite silica sol
CN104630765A (en) * 2013-11-11 2015-05-20 安徽未来表面技术有限公司 Environmental-protection type metal coating pre-treatment agent and preparation method thereof
CN106756976A (en) * 2016-11-26 2017-05-31 浙江五源科技股份有限公司 Silane compound and its application for chemical composition coating post processing

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
宣兆龙编著: "《装备环境工程 第2版》", 31 July 2015 *
屠振密,李宁,朱永明编著: "《钛及钛合金表面处理技术和应用》", 30 November 2010 *

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Application publication date: 20200915

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