CN105483666A - Preparing method of titanium salt surface conditioning agent - Google Patents

Preparing method of titanium salt surface conditioning agent Download PDF

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Publication number
CN105483666A
CN105483666A CN201510937019.3A CN201510937019A CN105483666A CN 105483666 A CN105483666 A CN 105483666A CN 201510937019 A CN201510937019 A CN 201510937019A CN 105483666 A CN105483666 A CN 105483666A
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China
Prior art keywords
mass parts
sodium
powder
parts
water content
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Pending
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CN201510937019.3A
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Chinese (zh)
Inventor
钱文华
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Changshu Yudong Phosphide Material Co Ltd
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Changshu Yudong Phosphide Material Co Ltd
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Priority to CN201510937019.3A priority Critical patent/CN105483666A/en
Publication of CN105483666A publication Critical patent/CN105483666A/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
    • C23C22/07Chemical 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 phosphates
    • C23C22/23Condensed phosphates
    • 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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  • 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)
  • Agricultural Chemicals And Associated Chemicals (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)

Abstract

The invention discloses a preparing method of a titanium salt surface conditioning agent. The preparing method comprises the following steps that firstly, 30 parts of anhydrous disodium hydrogen phosphate is prepared into a water solution with the concentration of 50%; secondly, 1-2 parts of sodium pyrophosphate, 0.8 part of titanyl sulfate, 3.5 parts of sodium pyrophosphate, 2.1 parts of sodium bicarbonate, 1.8 parts of sodium tetraborate, 3.6 parts of sodium hexametaphosphate, 0.3 part of polycarboxylic acid anion organic matter and 0.3 part of N-butyl naphthalene sulfonate are sequentially added in the water solution of disodium hydrogen phosphate, and a mixed solution is obtained; thirdly, the mixed solution is heated to 70 DEG C and fully stirred, and white powder with the water content below 2% is obtained; and fourthly, powder continues to be stirred at the temperature of 75 DEG C, 2.7 parts of sodium pyrophosphate, 1.2 parts of acetic acid, 0.7 part of methyltrimethoxysilane and 3.3 parts of magnesium sulfate are added into the powder at the same time, stirring continues, and drying is carried out till the water content is smaller than 1%. The prepared surface conditioning agent is good in scattering stability and can be stored for a long term.

Description

The preparation method of titanium salt surface conditioner
Technical field
The present invention relates to the preparation method of titanium salt surface conditioner.
Background technology
The dispersion stabilization of existing surface conditioner has much room for improvement, and can not preserve for a long time.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of titanium salt surface conditioner, its surface conditioner dispersion stabilization prepared is excellent, can preserve for a long time.
For achieving the above object, technical scheme of the present invention designs a kind of preparation method of titanium salt surface conditioner, comprises the steps to comprise the steps:
1) the light disodium of 30 mass parts anhydrous phosphoric acid is made the aqueous solution that concentration is 50%;
2) 1 ~ 2 mass parts trisodium phosphate, 0.8 mass parts titanyl sulfate, 3.5 mass parts trisodium phosphates, 2.1 mass parts sodium bicarbonates, 1.8 mass parts sodium tetraborates, 3.6 mass parts Sodium hexametaphosphate 99s, 0.3 mass parts poly carboxylic acid negatively charged ion there are is organism, 0.3 mass parts normal-butyl sodium naphthalene sulfonate joins in the aqueous solution of Sodium phosphate dibasic successively, obtain mixed solution;
3) mixed solution be heated to 70 DEG C and fully stir, obtaining the white powder of water content less than 2%;
4) continue to stir powder at 75 DEG C, simultaneously in powder, add 2.7 mass parts trisodium phosphates, 1.2 mass parts acetic acid, 0.7 mass parts methyltrimethoxy silane, 3.3 mass parts magnesium sulfate, then continue stirring and be dried to water content and be less than 1%.
Preferably, the preparation method of titanium salt surface conditioner, comprises the steps to comprise the steps:
1) the light disodium of 30 mass parts anhydrous phosphoric acid is made the aqueous solution that concentration is 50%;
2) 1 mass parts trisodium phosphate, 0.8 mass parts titanyl sulfate, 3.5 mass parts trisodium phosphates, 2.1 mass parts sodium bicarbonates, 1.8 mass parts sodium tetraborates, 3.6 mass parts Sodium hexametaphosphate 99s, 0.3 mass parts poly carboxylic acid negatively charged ion there are is organism, 0.3 mass parts normal-butyl sodium naphthalene sulfonate joins in the aqueous solution of Sodium phosphate dibasic successively, obtain mixed solution;
3) mixed solution be heated to 70 DEG C and fully stir, obtaining the white powder of water content less than 2%;
4) continue to stir powder at 75 DEG C, simultaneously in powder, add 2.7 mass parts trisodium phosphates, 1.2 mass parts acetic acid, 0.7 mass parts methyltrimethoxy silane, 3.3 mass parts magnesium sulfate, then continue stirring and be dried to water content and be less than 1%.
Preferably, the preparation method of titanium salt surface conditioner, comprises the steps to comprise the steps:
1) the light disodium of 30 mass parts anhydrous phosphoric acid is made the aqueous solution that concentration is 50%;
2) 2 mass parts trisodium phosphates, 0.8 mass parts titanyl sulfate, 3.5 mass parts trisodium phosphates, 2.1 mass parts sodium bicarbonates, 1.8 mass parts sodium tetraborates, 3.6 mass parts Sodium hexametaphosphate 99s, 0.3 mass parts poly carboxylic acid negatively charged ion there are is organism, 0.3 mass parts normal-butyl sodium naphthalene sulfonate joins in the aqueous solution of Sodium phosphate dibasic successively, obtain mixed solution;
3) mixed solution be heated to 70 DEG C and fully stir, obtaining the white powder of water content less than 2%;
4) continue to stir powder at 75 DEG C, simultaneously in powder, add 2.7 mass parts trisodium phosphates, 1.2 mass parts acetic acid, 0.7 mass parts methyltrimethoxy silane, 3.3 mass parts magnesium sulfate, then continue stirring and be dried to water content and be less than 1%.
Advantage of the present invention and beneficial effect are: the preparation method providing a kind of titanium salt surface conditioner, and its surface conditioner dispersion stabilization prepared is excellent, can preserve for a long time.
Embodiment
Below in conjunction with embodiment, the specific embodiment of the present invention is further described.Following examples only for technical scheme of the present invention is clearly described, and can not limit the scope of the invention with this.
The technical scheme that the present invention specifically implements is:
Embodiment 1
A preparation method for titanium salt surface conditioner, comprises the steps to comprise the steps:
1) the light disodium of 30 mass parts anhydrous phosphoric acid is made the aqueous solution that concentration is 50%;
2) 1 ~ 2 mass parts trisodium phosphate, 0.8 mass parts titanyl sulfate, 3.5 mass parts trisodium phosphates, 2.1 mass parts sodium bicarbonates, 1.8 mass parts sodium tetraborates, 3.6 mass parts Sodium hexametaphosphate 99s, 0.3 mass parts poly carboxylic acid negatively charged ion there are is organism, 0.3 mass parts normal-butyl sodium naphthalene sulfonate joins in the aqueous solution of Sodium phosphate dibasic successively, obtain mixed solution;
3) mixed solution be heated to 70 DEG C and fully stir, obtaining the white powder of water content less than 2%;
4) continue to stir powder at 75 DEG C, simultaneously in powder, add 2.7 mass parts trisodium phosphates, 1.2 mass parts acetic acid, 0.7 mass parts methyltrimethoxy silane, 3.3 mass parts magnesium sulfate, then continue stirring and be dried to water content and be less than 1%.
Embodiment 2
The preparation method of titanium salt surface conditioner, comprises the steps to comprise the steps:
1) the light disodium of 30 mass parts anhydrous phosphoric acid is made the aqueous solution that concentration is 50%;
2) 1 mass parts trisodium phosphate, 0.8 mass parts titanyl sulfate, 3.5 mass parts trisodium phosphates, 2.1 mass parts sodium bicarbonates, 1.8 mass parts sodium tetraborates, 3.6 mass parts Sodium hexametaphosphate 99s, 0.3 mass parts poly carboxylic acid negatively charged ion there are is organism, 0.3 mass parts normal-butyl sodium naphthalene sulfonate joins in the aqueous solution of Sodium phosphate dibasic successively, obtain mixed solution;
3) mixed solution be heated to 70 DEG C and fully stir, obtaining the white powder of water content less than 2%;
4) continue to stir powder at 75 DEG C, simultaneously in powder, add 2.7 mass parts trisodium phosphates, 1.2 mass parts acetic acid, 0.7 mass parts methyltrimethoxy silane, 3.3 mass parts magnesium sulfate, then continue stirring and be dried to water content and be less than 1%.
Embodiment 3
The preparation method of titanium salt surface conditioner, comprises the steps to comprise the steps:
1) the light disodium of 30 mass parts anhydrous phosphoric acid is made the aqueous solution that concentration is 50%;
2) 2 mass parts trisodium phosphates, 0.8 mass parts titanyl sulfate, 3.5 mass parts trisodium phosphates, 2.1 mass parts sodium bicarbonates, 1.8 mass parts sodium tetraborates, 3.6 mass parts Sodium hexametaphosphate 99s, 0.3 mass parts poly carboxylic acid negatively charged ion there are is organism, 0.3 mass parts normal-butyl sodium naphthalene sulfonate joins in the aqueous solution of Sodium phosphate dibasic successively, obtain mixed solution;
3) mixed solution be heated to 70 DEG C and fully stir, obtaining the white powder of water content less than 2%;
4) continue to stir powder at 75 DEG C, simultaneously in powder, add 2.7 mass parts trisodium phosphates, 1.2 mass parts acetic acid, 0.7 mass parts methyltrimethoxy silane, 3.3 mass parts magnesium sulfate, then continue stirring and be dried to water content and be less than 1%.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the prerequisite not departing from the technology of the present invention principle; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.

Claims (3)

1. the preparation method of titanium salt surface conditioner, is characterized in that, comprises the steps to comprise the steps:
1) the light disodium of 30 mass parts anhydrous phosphoric acid is made the aqueous solution that concentration is 50%;
2) 1 ~ 2 mass parts trisodium phosphate, 0.8 mass parts titanyl sulfate, 3.5 mass parts trisodium phosphates, 2.1 mass parts sodium bicarbonates, 1.8 mass parts sodium tetraborates, 3.6 mass parts Sodium hexametaphosphate 99s, 0.3 mass parts poly carboxylic acid negatively charged ion there are is organism, 0.3 mass parts normal-butyl sodium naphthalene sulfonate joins in the aqueous solution of Sodium phosphate dibasic successively, obtain mixed solution;
3) mixed solution be heated to 70 DEG C and fully stir, obtaining the white powder of water content less than 2%;
4) continue to stir powder at 75 DEG C, simultaneously in powder, add 2.7 mass parts trisodium phosphates, 1.2 mass parts acetic acid, 0.7 mass parts methyltrimethoxy silane, 3.3 mass parts magnesium sulfate, then continue stirring and be dried to water content and be less than 1%.
2. the preparation method of titanium salt surface conditioner according to claim 1, is characterized in that, comprises the steps to comprise the steps:
1) the light disodium of 30 mass parts anhydrous phosphoric acid is made the aqueous solution that concentration is 50%;
2) 1 mass parts trisodium phosphate, 0.8 mass parts titanyl sulfate, 3.5 mass parts trisodium phosphates, 2.1 mass parts sodium bicarbonates, 1.8 mass parts sodium tetraborates, 3.6 mass parts Sodium hexametaphosphate 99s, 0.3 mass parts poly carboxylic acid negatively charged ion there are is organism, 0.3 mass parts normal-butyl sodium naphthalene sulfonate joins in the aqueous solution of Sodium phosphate dibasic successively, obtain mixed solution;
3) mixed solution be heated to 70 DEG C and fully stir, obtaining the white powder of water content less than 2%;
4) continue to stir powder at 75 DEG C, simultaneously in powder, add 2.7 mass parts trisodium phosphates, 1.2 mass parts acetic acid, 0.7 mass parts methyltrimethoxy silane, 3.3 mass parts magnesium sulfate, then continue stirring and be dried to water content and be less than 1%.
3. the preparation method of titanium salt surface conditioner according to claim 1, is characterized in that, comprises the steps to comprise the steps:
1) the light disodium of 30 mass parts anhydrous phosphoric acid is made the aqueous solution that concentration is 50%;
2) 2 mass parts trisodium phosphates, 0.8 mass parts titanyl sulfate, 3.5 mass parts trisodium phosphates, 2.1 mass parts sodium bicarbonates, 1.8 mass parts sodium tetraborates, 3.6 mass parts Sodium hexametaphosphate 99s, 0.3 mass parts poly carboxylic acid negatively charged ion there are is organism, 0.3 mass parts normal-butyl sodium naphthalene sulfonate joins in the aqueous solution of Sodium phosphate dibasic successively, obtain mixed solution;
3) mixed solution be heated to 70 DEG C and fully stir, obtaining the white powder of water content less than 2%;
4) continue to stir powder at 75 DEG C, simultaneously in powder, add 2.7 mass parts trisodium phosphates, 1.2 mass parts acetic acid, 0.7 mass parts methyltrimethoxy silane, 3.3 mass parts magnesium sulfate, then continue stirring and be dried to water content and be less than 1%.
CN201510937019.3A 2015-12-14 2015-12-14 Preparing method of titanium salt surface conditioning agent Pending CN105483666A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20190144688A1 (en) * 2016-05-10 2019-05-16 Hoden Seimitsu Kako Kenkyusyo Co., Ltd. Aqueous anti-rust surface treatment composition and surface-coated metal member

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101974743A (en) * 2010-10-27 2011-02-16 大连三达奥克化学股份有限公司 Ti-Mg-B surface conditioner for zinc-phosphating and preparation method thereof

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101974743A (en) * 2010-10-27 2011-02-16 大连三达奥克化学股份有限公司 Ti-Mg-B surface conditioner for zinc-phosphating and preparation method thereof

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20190144688A1 (en) * 2016-05-10 2019-05-16 Hoden Seimitsu Kako Kenkyusyo Co., Ltd. Aqueous anti-rust surface treatment composition and surface-coated metal member
EP3456862A4 (en) * 2016-05-10 2020-01-08 Hoden Seimitsu Kako Kenkyusho Co., Ltd. Aqueous anti-rust surface treatment composition and surface-coated metal member
US10907053B2 (en) 2016-05-10 2021-02-02 Hoden Seimitsu Kako Kenkyusyo Co., Ltd. Aqueous anti-rust surface treatment composition and surface-coated metal member
TWI732867B (en) * 2016-05-10 2021-07-11 日商放電精密加工研究所股份有限公司 Aqueous rust preventive surface treatment composition and surface coated metal member

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Application publication date: 20160413