CN112011791A - Formation agent based on phosphoric acid without surface conditioning process and sodium sulfite promoter and preparation method thereof - Google Patents
Formation agent based on phosphoric acid without surface conditioning process and sodium sulfite promoter and preparation method thereof Download PDFInfo
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- CN112011791A CN112011791A CN202010885902.3A CN202010885902A CN112011791A CN 112011791 A CN112011791 A CN 112011791A CN 202010885902 A CN202010885902 A CN 202010885902A CN 112011791 A CN112011791 A CN 112011791A
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- corrosion inhibitor
- acid
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- 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
- C23C—COATING 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
- C23C22/00—Chemical 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
- C23C22/05—Chemical 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
- C23C22/06—Chemical 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
- C23C22/34—Chemical 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 fluorides or complex fluorides
- C23C22/36—Chemical 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 fluorides or complex fluorides containing also phosphates
- C23C22/362—Chemical 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 fluorides or complex fluorides containing also phosphates containing also zinc cations
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- 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
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
- C23G1/04—Cleaning or pickling metallic material with solutions or molten salts with acid solutions using inhibitors
-
- 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
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
- C23G1/04—Cleaning or pickling metallic material with solutions or molten salts with acid solutions using inhibitors
- C23G1/06—Cleaning or pickling metallic material with solutions or molten salts with acid solutions using inhibitors organic inhibitors
- C23G1/061—Cleaning or pickling metallic material with solutions or molten salts with acid solutions using inhibitors organic inhibitors nitrogen-containing compounds
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- 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
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
- C23G1/08—Iron or steel
- C23G1/088—Iron or steel solutions containing organic acids
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Treatment Of Metals (AREA)
Abstract
The invention relates to the technical field of formation agents, in particular to a formation agent based on phosphoric acid without surface conditioning procedures and sodium sulfite accelerators, which takes water as a solvent and phosphoric acid as a film forming agent, and is added with a first corrosion inhibitor, a second corrosion inhibitor, a third corrosion inhibitor, an acidity regulator, a surface conditioning agent, a first accelerator, a second accelerator, a third accelerator, an antirust agent, a first corrosion inhibitor, a second corrosion inhibitor and a chelating agent in percentage by weight: 5-30% of phosphoric acid, 0.5-10% of first corrosion inhibitor, 0.5-5% of second corrosion inhibitor, 0.5-5% of third corrosion inhibitor, 0.5-10% of acidity regulator, 0.1-2% of first accelerator, 0.01-5% of second accelerator, 0.001-0.5% of third accelerator, 0.1-2% of chelating agent, 0.1-2% of antirust agent, 0.1-2% of corrosion inhibitor, 0.01-0.5% of second corrosion inhibitor, 0.1-5% of surface conditioning agent and the balance of water. The conversion film of the invention does not need surface adjustment in the generation process, the bonding force of the film layer and the metal matrix is large, and different plates such as cold-rolled plates, galvanized plates, aluminum and the like can be processed in a collinear way.
Description
Technical Field
The invention relates to the technical field of chemical agents, in particular to a chemical agent based on phosphoric acid without a surface conditioning process and a sodium sulfite promoter and a preparation method thereof.
Background
The metal material is damaged by the action of the surrounding medium, which is called metal corrosion. When metal is corroded, the metal and air, water and the like generate chemical or electrochemical multiphase reaction on the interface of the metal, so that the metal is converted into an oxidized (ionic) state, the mechanical properties such as strength, plasticity, toughness and the like of the metal material are obviously reduced, the geometric shape of a metal component is damaged, the abrasion among parts is increased, the physical properties such as electricity, optics and the like are deteriorated, and the service life of equipment is shortened. The surface of a steel plate metal workpiece needs to be treated to generate various conversion coatings so as to improve the corrosion resistance of the product; with the social development and the improvement of environmental awareness, the traditional phosphating cannot meet the requirements of the day-to-day pretreatment coating process, the phosphating solution contains nickel which can cause serious harm to the health of people and the environment, a sodium sulfite promoter needs to be additionally added in the actual production, and the prior process needs to be subjected to surface conditioning.
Disclosure of Invention
In view of the above, the present invention is to solve the above problems, and provide a forming agent based on phosphoric acid without a surface modification step and a sodium sulfite promoter with good corrosion resistance, and a preparation method thereof, wherein the forming agent has a simple process flow, does not need to add an additional promoter, and does not need a surface modification step.
In order to achieve the purpose, the invention provides the following technical scheme: a chemical forming agent based on phosphoric acid without surface conditioning procedure and sodium sulfite accelerant takes water as solvent, phosphoric acid as film forming agent, and is added with a first corrosion inhibitor, a second corrosion inhibitor, a third corrosion inhibitor, an acidity regulator, a surface regulator, a first accelerant, a second accelerant, a third accelerant, an antirust agent, a first corrosion inhibitor, a second corrosion inhibitor and a chelating agent, and the weight percentages are as follows: 5-30% of phosphoric acid, 0.5-10% of first corrosion inhibitor, 0.5-5% of second corrosion inhibitor, 0.5-5% of third corrosion inhibitor, 0.5-10% of acidity regulator, 0.1-2% of first accelerator, 0.01-5% of second accelerator, 0.001-0.5% of third accelerator, 0.1-2% of chelating agent, 0.1-2% of antirust agent, 0.1-2% of corrosion inhibitor, 0.01-0.5% of second corrosion inhibitor, 0.1-5% of surface conditioning agent and the balance of water.
Further, the first corrosion inhibitor is zinc oxide, the second corrosion inhibitor is zinc nitrate or zinc sulfate or zinc phosphate, the third corrosion inhibitor is ammonium dihydrogen phosphate or sodium dihydrogen phosphate, the acidity regulator is nitric acid, the first accelerant is hydrofluoric acid, the second accelerant is reserve salt or p-nitrobenzenesulfonic acid or 3-nitrobenzenesulfonic acid or sodium m-nitrobenzenesulfonate, the third accelerant is copper nitrate or copper sulfate or basic copper carbonate, the chelating agent is hydroxylamine sulfate or hydroxylamine hydrochloride, the antirust agent is tartaric acid, the first corrosion inhibitor is triethanolamine or diethanolamine or hexamethylenetetramine, the second corrosion inhibitor is ferric nitrate or reduced ferric powder or ferric phosphate, and the surface conditioning agent is citric acid.
Further, the water is pure water or industrial water.
The invention also discloses a preparation method of the formation agent based on phosphoric acid without surface adjustment process and sodium sulfite promoter, which comprises the following steps:
s1, sequentially adding phosphoric acid, nitric acid and hydrofluoric acid into water and stirring;
s2, adding zinc oxide into the solution of S1, adding zinc nitrate or zinc sulfate or zinc phosphate, and stirring;
s3, adding ammonium dihydrogen phosphate or sodium dihydrogen phosphate, citric acid and tartaric acid into the solution of S2, and stirring;
s4, sequentially adding a dye-proof salt or p-nitrobenzenesulfonic acid or 3-nitrobenzenesulfonic acid or m-nitrobenzenesulfonic acid sodium salt, copper nitrate or copper sulfate or basic copper carbonate, hydroxylamine sulfate or hydroxylamine hydrochloride into the solution of S3, and stirring;
s5, sequentially adding triethanolamine, diethanolamine or hexamethylenetetramine, ferric nitrate, reduced iron powder or ferric phosphate into the solution of S4, and stirring to obtain the product.
Compared with the prior art, the invention has the beneficial effects that:
1. the zinc content in the phosphating agent provided by the invention is increased, so that the corrosion resistance can be better improved;
2. compared with the traditional phosphorization, the invention does not contain sodium sulfite accelerator substances, and has the advantages of less sediment, simple process flow and the like;
3. the surface adjustment is not needed in the conversion film generation process, the bonding force between the film layer and the metal matrix is large, and different plates such as cold-rolled plates, galvanized plates, aluminum and the like can be treated in a collinear manner;
4. the invention can be processed at low temperature, does not need additional heating, can greatly save energy and reduce cost;
5. the citric acid in the invention can adjust the surface state of the steel plate, remove oxide scale and the like, make the surface state of the steel plate uniform and prepare for coating.
Detailed Description
The present invention is further described with reference to specific examples to enable those skilled in the art to better understand the present invention and to practice the same, but the examples are not intended to limit the present invention.
Meanwhile, the invention is further explained below with reference to specific examples,
in preferred embodiment 1, a chemical forming agent based on phosphoric acid without requiring a surface preparation process and a sodium sulfite promoter, which comprises using water as a solvent, using phosphoric acid as a film forming agent, and adding zinc nitrate or zinc sulfate or zinc phosphate, zinc oxide, ammonium dihydrogen phosphate or sodium dihydrogen phosphate, nitric acid, citric acid, hydrofluoric acid, a stain-proofing salt or p-nitrobenzenesulfonic acid or 3-nitrobenzenesulfonic acid or sodium m-nitrobenzenesulfonate, copper nitrate or copper sulfate or basic copper carbonate, hydroxylamine sulfate or hydroxylamine hydrochloride, tartaric acid, triethanolamine or diethanolamine or hexamethylenetetramine, ferric nitrate or ferric oxide powder or ferric phosphate, in the following weight percentages: 5% of phosphoric acid, 0.5% of zinc nitrate or zinc sulfate or zinc phosphate, 0.5% of zinc oxide, 0.5% of ammonium dihydrogen phosphate or sodium dihydrogen phosphate, 0.5% of nitric acid, 0.1% of hydrofluoric acid, 0.01% of a stain-proofing salt or p-nitrobenzenesulfonic acid or 3-nitrobenzenesulfonic acid or sodium m-nitrobenzenesulfonate, 0.001% of copper nitrate or copper sulfate or basic copper carbonate, 0.1% of hydroxylamine sulfate or hydroxylamine hydrochloride, 0.1% of tartaric acid, 0.1% of triethanolamine or diethanolamine or hexamethylenetetramine, 0.1% of citric acid, 0.01% of ferric nitrate or ferric oxide powder or ferric phosphate and the balance of water.
In preferred embodiment 2, a forming agent based on phosphoric acid without requiring a surface preparation process and a sodium sulfite promoter, which comprises using water as a solvent, using phosphoric acid as a film forming agent, and adding zinc nitrate or zinc sulfate or zinc phosphate, zinc oxide, ammonium dihydrogen phosphate or sodium dihydrogen phosphate, nitric acid, citric acid, hydrofluoric acid, a stain-proofing salt or p-nitrobenzenesulfonic acid or 3-nitrobenzenesulfonic acid or sodium m-nitrobenzenesulfonate, copper nitrate or copper sulfate or basic copper carbonate, hydroxylamine sulfate or hydroxylamine hydrochloride, tartaric acid, triethanolamine or diethanolamine or hexamethylenetetramine, ferric nitrate or ferric oxide powder or ferric phosphate, in the following weight percentages: 15% of phosphoric acid, 2.5% of zinc nitrate or zinc sulfate or zinc phosphate, 5% of zinc oxide, 2.5% of ammonium dihydrogen phosphate or sodium dihydrogen phosphate, 5% of nitric acid, 1% of hydrofluoric acid, 2.5% of a stain-proofing salt or p-nitrobenzenesulfonic acid or 3-nitrobenzenesulfonic acid or sodium m-nitrobenzenesulfonate, 0.25% of copper nitrate or copper sulfate or basic copper carbonate, 1% of hydroxylamine sulfate or hydroxylamine hydrochloride, 1% of tartaric acid, 1% of triethanolamine or diethanolamine or hexamethylenetetramine, 2.5% of citric acid, 0.25% of iron nitrate or ferric oxide powder or iron phosphate and the balance of water.
In preferred embodiment 3, a forming agent based on phosphoric acid without requiring a surface preparation process and a sodium sulfite promoter, which comprises using water as a solvent, using phosphoric acid as a film forming agent, and adding zinc nitrate or zinc sulfate or zinc phosphate, zinc oxide, ammonium dihydrogen phosphate or sodium dihydrogen phosphate, nitric acid, citric acid, hydrofluoric acid, a stain-proofing salt or p-nitrobenzenesulfonic acid or 3-nitrobenzenesulfonic acid or sodium m-nitrobenzenesulfonate, copper nitrate or copper sulfate or basic copper carbonate, hydroxylamine sulfate or hydroxylamine hydrochloride, tartaric acid, triethanolamine or diethanolamine or hexamethylenetetramine, ferric nitrate or ferric oxide powder or ferric phosphate, in the following weight percentages: 30% of phosphoric acid, 5% of zinc nitrate or zinc sulfate or zinc phosphate, 10% of zinc oxide, 5% of ammonium dihydrogen phosphate or sodium dihydrogen phosphate, 10% of nitric acid, 2% of hydrofluoric acid, 5% of a stain-proofing salt or p-nitrobenzenesulfonic acid or 3-nitrobenzenesulfonic acid or sodium m-nitrobenzenesulfonate, 0.5% of copper nitrate or copper sulfate or basic copper carbonate, 2% of hydroxylamine sulfate or hydroxylamine hydrochloride, 2% of tartaric acid, 2% of triethanolamine or diethanolamine or hexamethylenetetramine, 5% of citric acid, 0.5% of ferric nitrate or ferric oxide powder or ferric phosphate and the balance of water. The water is pure water or industrial water.
Example 4: the invention also discloses a preparation method of the chemical forming agent based on phosphoric acid without a surface adjusting process and a sodium sulfite promoter, which comprises the following steps:
s1, sequentially adding phosphoric acid, nitric acid and hydrofluoric acid into water and stirring for 10-20 minutes;
s2, adding zinc oxide into the solution of S1, adding zinc nitrate or zinc sulfate or zinc phosphate, and stirring for 10-30 minutes until the zinc oxide is completely dissolved;
s3, adding ammonium dihydrogen phosphate or sodium dihydrogen phosphate, citric acid and tartaric acid into the solution of S2, and stirring for 5-10 minutes;
s4, sequentially adding a dye-proof salt or p-nitrobenzenesulfonic acid or 3-nitrobenzenesulfonic acid or m-nitrobenzenesulfonic acid sodium salt, copper nitrate or copper sulfate or basic copper carbonate, hydroxylamine sulfate or hydroxylamine hydrochloride into the solution of S3, and stirring for 5-10 percent;
s5, sequentially adding triethanolamine, diethanolamine or hexamethylenetetramine, ferric nitrate, reduced-oxygen iron powder or ferric phosphate into the solution of S4, and stirring for 10-30 minutes until the ferric nitrate, the reduced-oxygen iron powder or the ferric phosphate is completely dissolved, thereby finally obtaining the product.
The plate treatment process comprises the following steps:
firstly, degreasing the plate;
washing the surface of the plate with degreasing residual liquid;
processing (spraying or soaking) by using the phosphating agent, and the main parameters are as follows: the concentration of the product is 5-10% by weight, the temperature is 30-50 ℃, FA:0.1-2, TA:10-30(FA is free acid, TA is total acid, and is acid-base reaction drop point), the treatment time is as follows: 1-5 minutes;
fourthly, removing the plate and washing the residual treatment liquid of the phosphating agent on the surface of the plate;
fifthly, drying the plate (direct electrophoresis wet film electrophoresis without drying)
Sixthly, coating treatment such as powder coating or paint spraying after drying, or electrophoresis operation is directly carried out on the plate.
The above-mentioned embodiments are merely preferred embodiments for fully illustrating the present invention, and the scope of the present invention is not limited thereto. The equivalent substitution or change made by the technical personnel in the technical field on the basis of the invention is all within the protection scope of the invention. The protection scope of the invention is subject to the claims.
Claims (4)
1. A forming agent based on phosphoric acid without surface preparation process and sodium sulfite accelerant, which is characterized in that: water is used as a solvent, phosphoric acid is used as a film forming agent, and a first corrosion inhibitor, a second corrosion inhibitor, a third corrosion inhibitor, an acidity regulator, a surface conditioning agent, a first accelerator, a second accelerator, a third accelerator, an antirust agent, a first corrosion inhibitor, a second corrosion inhibitor and a chelating agent are added, wherein the weight percentages of the components are as follows: 5-30% of phosphoric acid, 0.5-10% of first corrosion inhibitor, 0.5-5% of second corrosion inhibitor, 0.5-5% of third corrosion inhibitor, 0.5-10% of acidity regulator, 0.1-2% of first accelerator, 0.01-5% of second accelerator, 0.001-0.5% of third accelerator, 0.1-2% of chelating agent, 0.1-2% of antirust agent, 0.1-2% of corrosion inhibitor, 0.01-0.5% of second corrosion inhibitor, 0.1-5% of surface conditioning agent and the balance of water.
2. The chemical conversion agent according to claim 1, which is based on phosphoric acid and does not require a surface preparation step and a sodium sulfite promoter, and which is characterized in that: the corrosion inhibitor comprises a first corrosion inhibitor, a second corrosion inhibitor, an acidity regulator, a chelating agent, a rust inhibitor, a first corrosion inhibitor, a second corrosion inhibitor, a surface conditioner and a surface conditioner, wherein the first corrosion inhibitor is zinc oxide, the second corrosion inhibitor is zinc nitrate, zinc sulfate or zinc phosphate, the third corrosion inhibitor is ammonium dihydrogen phosphate or sodium dihydrogen phosphate, the acidity regulator is nitric acid, the first promoter is hydrofluoric acid, the second promoter is dye-proof salt, p-nitrobenzenesulfonic acid, 3-nitrobenzenesulfonic acid or sodium m-nitrobenzenesulfonate, the third promoter is copper nitrate, copper sulfate or basic copper carbonate, the chelating agent is hydroxylamine sulfate or hydroxylamine hydrochloride, the rust inhibitor is tartaric acid, the first corrosion inhibitor is triethanolamine, diethanolamine or hexamethylenetetramine, the second corrosion inhibitor is ferric nitrate or deoxidized iron powder or ferric phosphate, and the surface conditioner.
3. The chemical conversion agent according to claim 1 or 2, which is based on phosphoric acid and does not require a surface preparation step and a sodium sulfite promoter, and which is characterized in that: the water is pure water or industrial water.
4. The method for preparing a chemical conversion agent based on phosphoric acid without requiring a surface preparation process and a sodium sulfite promoter according to any one of claims 1 to 3, wherein: the method comprises the following steps:
s1, sequentially adding phosphoric acid, nitric acid and hydrofluoric acid into water and stirring;
s2, adding zinc oxide into the solution of S1, adding zinc nitrate or zinc sulfate or zinc phosphate, and stirring;
s3, adding ammonium dihydrogen phosphate or sodium dihydrogen phosphate, citric acid and tartaric acid into the solution of S2, and stirring;
s4, sequentially adding a dye-proof salt or p-nitrobenzenesulfonic acid or 3-nitrobenzenesulfonic acid or m-nitrobenzenesulfonic acid sodium salt, copper nitrate or copper sulfate or basic copper carbonate, hydroxylamine sulfate or hydroxylamine hydrochloride into the solution of S3, and stirring;
s5, sequentially adding triethanolamine, diethanolamine or hexamethylenetetramine, ferric nitrate, reduced iron powder or ferric phosphate into the solution of S4, and stirring to obtain the product.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010885902.3A CN112011791A (en) | 2020-08-28 | 2020-08-28 | Formation agent based on phosphoric acid without surface conditioning process and sodium sulfite promoter and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010885902.3A CN112011791A (en) | 2020-08-28 | 2020-08-28 | Formation agent based on phosphoric acid without surface conditioning process and sodium sulfite promoter and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113621953A (en) * | 2021-07-08 | 2021-11-09 | 重庆信人科技发展有限公司 | Phosphating solution and preparation method thereof |
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| CN113621953A (en) * | 2021-07-08 | 2021-11-09 | 重庆信人科技发展有限公司 | Phosphating solution and preparation method thereof |
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