CN110863194A - Phosphating and silanization composite treatment fluid and preparation method thereof - Google Patents

Phosphating and silanization composite treatment fluid and preparation method thereof Download PDF

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CN110863194A
CN110863194A CN201911277417.1A CN201911277417A CN110863194A CN 110863194 A CN110863194 A CN 110863194A CN 201911277417 A CN201911277417 A CN 201911277417A CN 110863194 A CN110863194 A CN 110863194A
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composite
treating fluid
treatment liquid
prepared
composite treatment
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孙振东
李庆鹏
管勇
赵丽娜
张文强
尹晓伟
王黎明
彭胡
盖宇
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Shenyang Institute of Engineering
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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
    • C23C22/40Chemical 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 containing molybdates, tungstates or vanadates
    • C23C22/44Chemical 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 containing molybdates, tungstates or vanadates containing also fluorides or complex fluorides
    • 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
    • C23C2222/00Aspects relating to chemical surface treatment of metallic material by reaction of the surface with a reactive medium
    • C23C2222/20Use of solutions containing silanes

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  • General Chemical & Material Sciences (AREA)
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  • Engineering & Computer Science (AREA)
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  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Treatment Of Metals (AREA)

Abstract

The invention discloses a phosphatizing and silanizing composite treating fluid and a preparation method thereof, which relate to the technical field of steel production, the phosphatizing and silanizing composite treating fluid comprises a composite treating fluid A and a composite treating fluid B, wherein the composite treating fluid A comprises ammonium molybdate, zinc oxide, calcium oxide, phosphoric acid, zinc nitrate, Marshall salt, nickel sulfate, triethanolamine, a compound surfactant, sodium fluoride, citric acid, an accelerant A and an accelerant B, the composite treating fluid B comprises absolute ethyl alcohol, deionized water, gamma-GPS, BTSE, silane and glacial acetic acid, the components required for phosphatizing and silanizing are integrated to form the components for preparing the phosphatizing and silanizing composite treating fluid together, and after the phosphatizing and silanizing composite treating fluid is prepared, Q235 steel is treated, so that the Q235 steel has the respective advantages of phosphatizing and silanizing when used at the later stage, the use performance of the Q235 steel is better.

Description

Phosphating and silanization composite treatment fluid and preparation method thereof
Technical Field
The invention relates to the technical field of steel production, in particular to a phosphating and silanization composite treating fluid and a preparation method thereof.
Background
In the production process of the Q235 steel, in order to improve the corrosion resistance and the adhesion effect of paint on the surface of the Q235 steel when the Q235 steel is used at a later stage, in the production process, the surface of the Q235 steel is usually treated by adopting a phosphorization or silanization process.
Phosphorization is a process for forming a phosphate chemical conversion film through chemical and electrochemical reactions, the formed phosphate conversion film is called a phosphorization film, phosphorization is a common pretreatment technology, belongs to chemical conversion film treatment in principle, and is mainly applied to steel surface phosphorization, nonferrous metal (such as aluminum and zinc) pieces can also be applied to phosphorization, and silanization is a process for carrying out surface treatment on metal or nonmetal materials by taking an organic silane aqueous solution as a main component.
In the above description, no matter the surface of the Q235 steel is phosphated or silanized, there are corresponding advantages, and therefore, how to prepare a liquid having both phosphatization and silanization advantages and make the Q235 steel perform better after using the liquid is a problem to be solved.
In summary, the technical personnel in the field provide a phosphatization and silanization composite treatment fluid and a preparation method thereof.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a phosphating and silanization composite treating fluid and a preparation method thereof, and solves the problem that how to prepare a fluid with both phosphating and silanization advantages and the Q235 steel has better performance after the fluid is used.
In order to achieve the purpose, the invention is realized by the following technical scheme: a phosphatization silanization composite treatment fluid, which comprises a composite treatment fluid A and a composite treatment fluid B,
the composite treating fluid A comprises ammonium molybdate, zinc oxide, calcium oxide, phosphoric acid, zinc nitrate, Marshall salt, nickel sulfate, triethanolamine, a compound surfactant, sodium fluoride, citric acid, an accelerator A and an accelerator B, and is prepared from the following components in parts by weight: 3-7g/L of ammonium molybdate, 10-14g/L of zinc oxide, 5-9g/L of calcium oxide, 45-55g/L of phosphoric acid, 20-25g/L of zinc nitrate, 6-10g/L of Marshall salt, 0.6-1.2g/L of nickel sulfate, 42-49g/L of triethanolamine, 4-8g/L of compound surfactant, 1-6g/L of sodium fluoride, 0.6-1.2g/L of citric acid, 1.5-3g/L of accelerator A and 1.6-2.4g/L of accelerator B.
The compound treatment liquid B comprises the following components in parts by weight: 18-28g/L of absolute ethyl alcohol, 5-9g/L of deionized water, 8-8 g/L, BTSE3-10g/L of gamma-GPS 1, 12-17g/L of silane and 1-3g/L of glacial acetic acid.
Preferably, the composite treatment fluid A is prepared from the following components in proportion by weight: 4g/L of ammonium molybdate, 11g/L of zinc oxide, 6g/L of calcium oxide, 49g/L of phosphoric acid, 21g/L of zinc nitrate, 7g/L of marzif salt, 0.9g/L of nickel sulfate, 45g/L of triethanolamine, 5g/L of compound surfactant, 2g/L of sodium fluoride, 0.9g/L of citric acid, 1.9g/L of accelerator A1.9g/L and 2.1g/L of accelerator B2;
the composite treating fluid B is prepared from the following components in proportion by weight: 18g/L of absolute ethyl alcohol, 6g/L of deionized water, 6g/L of gamma-GPS 6g/L, BTSE9g/L, 14g/L of silane and 1/L of glacial acetic acid.
Preferably, the composite treatment fluid A is prepared from the following components in proportion by weight: 6g/L of ammonium molybdate, 13g/L of zinc oxide, 8g/L of calcium oxide, 51g/L of phosphoric acid, 23g/L of zinc nitrate, 9g/L of marzif salt, 1.1g/L of nickel sulfate, 17g/L of triethanolamine, 7g/L of compound surfactant, 4g/L of sodium fluoride, 1.1g/L of citric acid, 2.1g/L of accelerator and 1.8g/L of accelerator;
the composite treating fluid B is prepared from the following components in proportion by weight: 21g/L of absolute ethyl alcohol, 7g/L of deionized water, gamma-GPS 4g/L, BTSE6g/L, 16g/L of silane and 3g/L of glacial acetic acid.
Preferably, the composite treatment fluid A is prepared from the following components in proportion by weight: 5g/L of ammonium molybdate, 12g/L of zinc oxide, 7g/L of calcium oxide, 50g/L of phosphoric acid, 22g/L of zinc nitrate, 8g/L of mazel salt, 1g/L of nickel sulfate, 46g/L of triethanolamine, 6g/L of compound surfactant, 3g/L of sodium fluoride, 1g/L of citric acid, 2.4g/L of accelerator and 2.2g/L of accelerator B;
the composite treating fluid B is prepared from the following components in proportion by weight: 27g/L of absolute ethyl alcohol, 9g/L of deionized water, gamma-GPS 2g/L, BTSE3g/L, 15g/L of silane and 2g/L of glacial acetic acid.
The preparation method of the phosphatization and silanization composite treating fluid comprises the following steps:
s1, preparing a composite treating fluid A: measuring each component in the composite treatment liquid A according to a certain mixing proportion, pouring all the components of the composite treatment liquid A into a stirring container after the components are measured, and fully stirring to obtain the composite treatment liquid A;
s2, preparing a composite treatment liquid B: according to a certain mixing proportion, metering each component in the composite treatment liquid B, adding absolute ethyl alcohol and deionized water in the composite treatment liquid B into a stirring container for mixing after metering, adding gamma-GPS and BTSE after fully mixing, then adding silane, adding glacial acetic acid after fully stirring to adjust the pH value of the solution, stirring, standing, and using after clarifying and transparentizing;
s3, preparing a mixed solution of the composite treatment solution A and the composite treatment solution B: the composite treatment liquid a prepared in step S1 and the composite treatment liquid B prepared in step S2 were added to a stirring vessel at a volume ratio of 2: 1, and were thoroughly mixed to obtain a phosphatized silanized composite treatment liquid.
Preferably, in step S2, when the absolute ethyl alcohol and the deionized water in the composite treating liquid B are metered, the volume ratio of the absolute ethyl alcohol to the deionized water is 3: 1.
Preferably, in the step S2, when the γ -GPS and BTSE are measured in the composite treatment liquid B, the volume ratio of γ -GPS and BTSE is 2: 3, the total volume fraction of silane is 4-8%, the stirring time in the step S2 is 2-3h, and the standing time of the prepared composite treatment liquid B is 72 h.
Preferably, the pH of the complex treatment liquid A prepared in the step S1 is 3 to 4, the pH of the complex treatment liquid B prepared in the step S2 is 3.5 to 4.5, and the pH of the phosphatized and silanized complex treatment liquid prepared in the step S3 is 3 to 4.
Advantageous effects
The invention provides a phosphatization and silanization composite treating fluid and a preparation method thereof. Compared with the prior art, the method has the following beneficial effects:
1. the phosphorization and silanization composite treating fluid comprises a composite treating fluid A and a composite treating fluid B, wherein the composite treating fluid A comprises ammonium molybdate, zinc oxide, calcium oxide, phosphoric acid, zinc nitrate, Marshall salt, nickel sulfate, triethanolamine, compound surfactant, sodium fluoride, citric acid, accelerator A and accelerator B, the composite treating liquid B comprises absolute ethyl alcohol, deionized water, gamma-GPS, BTSE, silane and glacial acetic acid, the components required by phosphorization and silanization are integrated together to form the components for preparing the phosphorization and silanization composite treatment fluid, and after the component is prepared, the obtained composite treatment fluid, the Q235 steel is processed, so that when the Q235 steel is used at a later stage, the advantages of both phosphorization and silanization are achieved, and the use performance of the Q235 steel is better.
Drawings
FIG. 1 is a graph comparing data of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
the invention provides a technical scheme that: a phosphatization silanization composite treatment fluid, which comprises a composite treatment fluid A and a composite treatment fluid B,
the composite treating fluid A comprises ammonium molybdate, zinc oxide, calcium oxide, phosphoric acid, zinc nitrate, Marshall salt, nickel sulfate, triethanolamine, a compound surfactant, sodium fluoride, citric acid, an accelerator A and an accelerator B, and is prepared from the following components in parts by weight: 4g/L of ammonium molybdate, 11g/L of zinc oxide, 6g/L of calcium oxide, 49g/L of phosphoric acid, 21g/L of zinc nitrate, 7g/L of marzif salt, 0.9g/L of nickel sulfate, 45g/L of triethanolamine, 5g/L of compound surfactant, 2g/L of sodium fluoride, 0.9g/L of citric acid, 1.9g/L of accelerator and 2.1g/L of accelerator.
The compound treatment liquid B comprises the following components in parts by weight: 18g/L of absolute ethyl alcohol, 6g/L of deionized water, 6g/L of gamma-GPS 6g/L, BTSE9g/L, 14g/L of silane and 1/L of glacial acetic acid.
The preparation method of the phosphatization and silanization composite treating fluid comprises the following steps:
s1, preparing a composite treating fluid A: measuring each component in the composite treatment liquid A according to a certain mixing proportion, pouring all the components of the composite treatment liquid A into a stirring container after the components are measured, and fully stirring to obtain the composite treatment liquid A;
s2, preparing a composite treatment liquid B: according to a certain mixing proportion, metering each component in the composite treatment liquid B, adding absolute ethyl alcohol and deionized water in the composite treatment liquid B into a stirring container for mixing after metering, adding gamma-GPS and BTSE after fully mixing, then adding silane, adding glacial acetic acid after fully stirring to adjust the pH value of the solution, stirring, standing, and using after clarifying and transparentizing;
s3, preparing a mixed solution of the composite treatment solution A and the composite treatment solution B: the composite treatment liquid a prepared in step S1 and the composite treatment liquid B prepared in step S2 were added to a stirring vessel at a volume ratio of 2: 1, and were thoroughly mixed to obtain a phosphatized silanized composite treatment liquid.
In the present invention, in step S2, when the absolute ethyl alcohol and the deionized water in the composite treatment liquid B are measured, the volume ratio of the absolute ethyl alcohol to the deionized water is 3: 1.
In the present invention, in the step S2, when the gamma-GPS and BTSE in the composite treatment liquid B were measured, the volume ratio of the gamma-GPS to the BTSE was 2: 3, the total volume fraction of silane was 5%, the stirring time in the step S2 was 2 hours, and the standing time of the composite treatment liquid B thus obtained was 72 hours.
In the present invention, the composite treating liquid A prepared in the step S1 has a pH of 3, the composite treating liquid B prepared in the step S2 has a pH of 3.5, and the phosphatized silanized composite treating liquid prepared in the step S3 has a pH of 3.
Example 2:
the invention provides a technical scheme that: a phosphatization silanization composite treatment fluid, which comprises a composite treatment fluid A and a composite treatment fluid B,
the composite treating fluid A comprises ammonium molybdate, zinc oxide, calcium oxide, phosphoric acid, zinc nitrate, Marshall salt, nickel sulfate, triethanolamine, a compound surfactant, sodium fluoride, citric acid, an accelerator A and an accelerator B, and is prepared from the following components in parts by weight: 6g/L of ammonium molybdate, 13g/L of zinc oxide, 8g/L of calcium oxide, 51g/L of phosphoric acid, 23g/L of zinc nitrate, 9g/L of marzif salt, 1.1g/L of nickel sulfate, 17g/L of triethanolamine, 7g/L of compound surfactant, 4g/L of sodium fluoride, 1.1g/L of citric acid, 2.1g/L of accelerator and 1.8g/L of accelerator.
The compound treatment liquid B comprises the following components in parts by weight: 21g/L of absolute ethyl alcohol, 7g/L of deionized water, gamma-GPS 4g/L, BTSE6g/L, 16g/L of silane and 3g/L of glacial acetic acid.
The preparation method of the phosphatization and silanization composite treating fluid comprises the following steps:
s1, preparing a composite treating fluid A: measuring each component in the composite treatment liquid A according to a certain mixing proportion, pouring all the components of the composite treatment liquid A into a stirring container after the components are measured, and fully stirring to obtain the composite treatment liquid A;
s2, preparing a composite treatment liquid B: according to a certain mixing proportion, metering each component in the composite treatment liquid B, adding absolute ethyl alcohol and deionized water in the composite treatment liquid B into a stirring container for mixing after metering, adding gamma-GPS and BTSE after fully mixing, then adding silane, adding glacial acetic acid after fully stirring to adjust the pH value of the solution, stirring, standing, and using after clarifying and transparentizing;
s3, preparing a mixed solution of the composite treatment solution A and the composite treatment solution B: the composite treatment liquid a prepared in step S1 and the composite treatment liquid B prepared in step S2 were added to a stirring vessel at a volume ratio of 2: 1, and were thoroughly mixed to obtain a phosphatized silanized composite treatment liquid.
In the present invention, in step S2, when the absolute ethyl alcohol and the deionized water in the composite treatment liquid B are measured, the volume ratio of the absolute ethyl alcohol to the deionized water is 3: 1.
In the present invention, in the step S2, when the gamma-GPS and BTSE in the composite treatment liquid B were measured, the volume ratio of the gamma-GPS to the BTSE was 2: 3, the total volume fraction of silane was 7%, the stirring time in the step S2 was 3 hours, and the standing time of the composite treatment liquid B thus obtained was 72 hours.
In the present invention, the composite treating liquid A prepared in the step S1 has a pH of 4, the composite treating liquid B prepared in the step S2 has a pH of 4.5 the phosphated silanized composite treating liquid prepared in the step S3 has a pH of 4.
Example 3:
the invention provides a technical scheme that: a phosphatization silanization composite treatment fluid, which comprises a composite treatment fluid A and a composite treatment fluid B,
the composite treating fluid A comprises ammonium molybdate, zinc oxide, calcium oxide, phosphoric acid, zinc nitrate, Marshall salt, nickel sulfate, triethanolamine, a compound surfactant, sodium fluoride, citric acid, an accelerator A and an accelerator B, and is prepared from the following components in parts by weight: 5g/L of ammonium molybdate, 12g/L of zinc oxide, 7g/L of calcium oxide, 50g/L of phosphoric acid, 22g/L of zinc nitrate, 8g/L of mazel salt, 1g/L of nickel sulfate, 46g/L of triethanolamine, 6g/L of compound surfactant, 3g/L of sodium fluoride, 1g/L of citric acid, 2.4g/L of accelerator and 2.2g/L of accelerator.
The compound treatment liquid B comprises the following components in parts by weight: 27g/L of absolute ethyl alcohol, 9g/L of deionized water, gamma-GPS 2g/L, BTSE3g/L, 15g/L of silane and 2g/L of glacial acetic acid.
The preparation method of the phosphatization and silanization composite treating fluid comprises the following steps:
s1, preparing a composite treating fluid A: measuring each component in the composite treatment liquid A according to a certain mixing proportion, pouring all the components of the composite treatment liquid A into a stirring container after the components are measured, and fully stirring to obtain the composite treatment liquid A;
s2, preparing a composite treatment liquid B: according to a certain mixing proportion, metering each component in the composite treatment liquid B, adding absolute ethyl alcohol and deionized water in the composite treatment liquid B into a stirring container for mixing after metering, adding gamma-GPS and BTSE after fully mixing, then adding silane, adding glacial acetic acid after fully stirring to adjust the pH value of the solution, stirring, standing, and using after clarifying and transparentizing;
s3, preparing a mixed solution of the composite treatment solution A and the composite treatment solution B: the composite treatment liquid a prepared in step S1 and the composite treatment liquid B prepared in step S2 were added to a stirring vessel at a volume ratio of 2: 1, and were thoroughly mixed to obtain a phosphatized silanized composite treatment liquid.
In the present invention, in step S2, when the absolute ethyl alcohol and the deionized water in the composite treatment liquid B are measured, the volume ratio of the absolute ethyl alcohol to the deionized water is 3: 1.
In the present invention, in the step S2, when the gamma-GPS and BTSE were measured in the composite treatment liquid B, the volume ratio of the gamma-GPS to the BTSE was 2: 3, the total volume fraction of silane was 6%, the stirring time in the step S2 was 2.5 hours, and the standing time of the composite treatment liquid B thus obtained was 72 hours.
In the present invention, the pH of the composite treating liquid A prepared in the step S1 was 3.5, the pH of the composite treating liquid B prepared in the step S2 was 4, and the pH of the phosphatized silanized composite treating liquid prepared in the step S3 was 3.5.
According to the phosphating and silanization composite treating fluid prepared in the three embodiments, compared with the actual performance of singly adopting phosphating or silanization process treatment in the prior art in the using process at the later stage, the following tests are made:
taking five steel samples of Q235 steel with the same specification, wherein three steel samples are respectively immersed into the phosphating and silanization composite treatment liquid prepared in the three embodiments, and the other two steel samples are respectively immersed into the phosphating liquid and the silanization liquid, the five steel samples of Q235 steel with the same specification are immersed into different liquids for 10min and then taken out, then dried for 30min at the temperature of 120 ℃, and then the surfaces of the five dried steel samples of Q235 steel are coated with a layer of antirust paint, and then placed in the same environment for standing and observation for 60 days, so as to obtain the corresponding performance data shown in figure 1;
from the data in fig. 1, the following conclusions can be drawn: the performance of the steel sample of Q235 steel treated by the phosphating solution or the silanization solution after 60 days is far inferior to that of the steel sample of Q235 steel treated by the phosphating and silanization composite treatment solution prepared in the three examples, and the performance of the phosphating and silanization composite treatment solution prepared in the three examples is the best.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (8)

1. A phosphating and silanization composite treatment liquid comprises a composite treatment liquid A and a composite treatment liquid B, and is characterized in that:
the composite treating fluid A comprises ammonium molybdate, zinc oxide, calcium oxide, phosphoric acid, zinc nitrate, Marshall salt, nickel sulfate, triethanolamine, a compound surfactant, sodium fluoride, citric acid, an accelerator A and an accelerator B, and is prepared from the following components in parts by weight: 3-7g/L of ammonium molybdate, 10-14g/L of zinc oxide, 5-9g/L of calcium oxide, 45-55g/L of phosphoric acid, 20-25g/L of zinc nitrate, 6-10g/L of Marshall salt, 0.6-1.2g/L of nickel sulfate, 42-49g/L of triethanolamine, 4-8g/L of compound surfactant, 1-6g/L of sodium fluoride, 0.6-1.2g/L of citric acid, 1.5-3g/L of accelerator A and 1.6-2.4g/L of accelerator B;
the compound treatment liquid B comprises the following components in parts by weight: 18-28g/L of absolute ethyl alcohol, 5-9g/L of deionized water, 8-8 g/L, BTSE3-10g/L of gamma-GPS 1, 12-17g/L of silane and 1-3g/L of glacial acetic acid.
2. The phosphating and silanization composite treating fluid according to claim 1, which is characterized in that: the composite treating fluid A is prepared from the following components in parts by weight: 4g/L of ammonium molybdate, 11g/L of zinc oxide, 6g/L of calcium oxide, 49g/L of phosphoric acid, 21g/L of zinc nitrate, 7g/L of marzif salt, 0.9g/L of nickel sulfate, 45g/L of triethanolamine, 5g/L of compound surfactant, 2g/L of sodium fluoride, 0.9g/L of citric acid, 1.9g/L of accelerator A1.9g/L and 2.1g/L of accelerator B2;
the composite treating fluid B is prepared from the following components in proportion by weight: 18g/L of absolute ethyl alcohol, 6g/L of deionized water, 6g/L of gamma-GPS 6g/L, BTSE9g/L, 14g/L of silane and 1/L of glacial acetic acid.
3. The phosphating and silanization composite treating fluid according to claim 1, which is characterized in that: the composite treating fluid A is prepared from the following components in parts by weight: 6g/L of ammonium molybdate, 13g/L of zinc oxide, 8g/L of calcium oxide, 51g/L of phosphoric acid, 23g/L of zinc nitrate, 9g/L of marzif salt, 1.1g/L of nickel sulfate, 17g/L of triethanolamine, 7g/L of compound surfactant, 4g/L of sodium fluoride, 1.1g/L of citric acid, 2.1g/L of accelerator and 1.8g/L of accelerator;
the composite treating fluid B is prepared from the following components in proportion by weight: 21g/L of absolute ethyl alcohol, 7g/L of deionized water, gamma-GPS 4g/L, BTSE6g/L, 16g/L of silane and 3g/L of glacial acetic acid.
4. The phosphating and silanization composite treating fluid according to claim 1, which is characterized in that: the composite treating fluid A is prepared from the following components in parts by weight: 5g/L of ammonium molybdate, 12g/L of zinc oxide, 7g/L of calcium oxide, 50g/L of phosphoric acid, 22g/L of zinc nitrate, 8g/L of mazel salt, 1g/L of nickel sulfate, 46g/L of triethanolamine, 6g/L of compound surfactant, 3g/L of sodium fluoride, 1g/L of citric acid, 2.4g/L of accelerator and 2.2g/L of accelerator B;
the composite treating fluid B is prepared from the following components in proportion by weight: 27g/L of absolute ethyl alcohol, 9g/L of deionized water, gamma-GPS 2g/L, BTSE3g/L, 15g/L of silane and 2g/L of glacial acetic acid.
5. The phosphating and silanization composite treatment fluid according to any one of claims 1 to 4, which is characterized in that: the preparation method comprises the following steps:
s1, preparing a composite treating fluid A: measuring each component in the composite treatment liquid A according to a certain mixing proportion, pouring all the components of the composite treatment liquid A into a stirring container after the components are measured, and fully stirring to obtain the composite treatment liquid A;
s2, preparing a composite treatment liquid B: according to a certain mixing proportion, metering each component in the composite treatment liquid B, adding absolute ethyl alcohol and deionized water in the composite treatment liquid B into a stirring container for mixing after metering, adding gamma-GPS and BTSE after fully mixing, then adding silane, adding glacial acetic acid after fully stirring to adjust the pH value of the solution, stirring, standing, and using after clarifying and transparentizing;
s3, preparing a mixed solution of the composite treatment solution A and the composite treatment solution B: the composite treatment liquid a prepared in step S1 and the composite treatment liquid B prepared in step S2 were added to a stirring vessel at a volume ratio of 2: 1, and were thoroughly mixed to obtain a phosphatized silanized composite treatment liquid.
6. The method for preparing the phosphatized silanized composite treating fluid according to claim 5, wherein the method comprises the following steps: in the step S2, when the absolute ethyl alcohol and the deionized water in the composite treatment liquid B are measured, the volume ratio of the absolute ethyl alcohol to the deionized water is 3: 1.
7. The method for preparing the phosphatized silanized composite treating fluid according to claim 5, wherein the method comprises the following steps: in the step S2, when the gamma-GPS and the BTSE in the composite processing liquid B are measured, the volume ratio of the gamma-GPS to the BTSE is 2: 3, the total volume fraction of the silane is 4-8%, the stirring time in the step S2 is 2-3h, and the standing time of the prepared composite processing liquid B is 72 h.
8. The method for preparing the phosphatized silanized composite treating fluid according to claim 5, wherein the method comprises the following steps: the pH of the composite treating fluid A prepared in the step S1 is 3-4, the pH of the composite treating fluid B prepared in the step S2 is 3.5-4.5, and the pH of the phosphatized silanized composite treating fluid prepared in the step S3 is 3-4.
CN201911277417.1A 2019-12-06 2019-12-06 Phosphating and silanization composite treatment fluid and preparation method thereof Pending CN110863194A (en)

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CN110527995A (en) * 2019-09-29 2019-12-03 中国石油大学(华东) Application of the compound silane film of MXene/ silane surfaces in metal erosion protection

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CN102409325A (en) * 2011-12-06 2012-04-11 中国科学院金属研究所 Environmentally-friendly corrosion-resistant chromium-free chemical conversion liquid and method for preparing chemical conversion film
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Application publication date: 20200306