CN1057681A - Phosphating solution at room temperature and compound method thereof - Google Patents
Phosphating solution at room temperature and compound method thereof Download PDFInfo
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- CN1057681A CN1057681A CN 91104466 CN91104466A CN1057681A CN 1057681 A CN1057681 A CN 1057681A CN 91104466 CN91104466 CN 91104466 CN 91104466 A CN91104466 A CN 91104466A CN 1057681 A CN1057681 A CN 1057681A
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Abstract
The present invention relates to a kind of phosphating solution at room temperature and compound method thereof, this phosphatization liquid is made up of phosphoric acid, nitric acid, citric acid, zinc nitrate, nickelous nitrate, cupric nitrate, zinc oxide, hydrogen peroxide, phthalic anhydride and water.Its compound method be in acid groove container with phosphoric acid, nitric acid, citric acid mixing, the zinc oxide with water furnishing pasty state slowly adds in the acid again, the limit edged stirs; And then add entry, phthalic anhydride, hydrogen peroxide, cupric nitrate, nickelous nitrate, zinc nitrate successively, and be stirred to dissolving fully, use ammonium hydrogencarbonate regulator solution acidity below 50 o'clock then; This phosphatization liquid can be used for the metallic surface electrostatic painting of automobile, household electrical appliance etc. or the pre-treatment before the japanning.
Description
The present invention relates to phosphating solution at room temperature and compound method thereof in the Chemical Pretreatment process of a kind of metallic surface.
Bonderizing is one of ferrous metal method of chemical protection; along with developing rapidly of household electrical appliance; phosphating process is able to widespread use, but the bonderizing temperature of original phosphatization liquid is generally in middle temperature more than 35 ℃, and because phosphatization liquid is acidic medium; under the temperature more than the middle temperature; phosphatization equipment and heating installation are all had very strong corrosive nature, and general exchange device more just in two years is simultaneously owing to need heat; energy consumption is big, is unfavorable for save energy.
A kind of phosphate solution of used for phosphorization by dipping is disclosed in Chinese patent CN1032963A, contain zine ion 1-3 grams per liter in this solution, calcium ion 1.0-4.5 grams per liter, phosphate anion 21-32 grams per liter, m-nitrobenzene sodium sulfonate 0.1-3 grams per liter, chloranion 0.3-10 grams per liter, nitrate ion 0-15 grams per liter, nickel ion 0.1-0.3 grams per liter, disodium ethylene diamine tetraacetate 0.08-0.15 grams per liter, mn ion 0-0.8 grams per liter, zinc wherein, the ratio of calcium ion is 1: 1-1.5, zinc, the ratio of phosphate anion is 1: 7-19, m-nitrobenzene sodium sulfonate is 1 with the ratio of chloranion: 1-3.5, its characteristics, be that filmogen is based on calcium zinc orthophosphate activated by thallium, adopt m-nitrobenzene sodium sulfonate, chlorate anions, nitrate ion is as associating promotor, and other ion is as additive; The weak point of this solution is to adopt m-nitrobenzene sodium sulfonate and nitrate ion to unite when using, the concentration of m-nitrobenzene sodium sulfonate is controlled and can be made solution become tawny when bad, when using sodium chlorate to do promotor, the concentration of sodium chlorate is wayward, solution is poisoned, cause the passivation of steel surface portion, this formation to the phosphoric acid film brings unfavorable factor; And this phosphatization liquid in parkerizing process, need be heated on 58 ℃ of ability phosphatizations of temperature, phosphatization equipment and heating installation are all had very strong corrosive nature, and energy consumption is big, body refuse is many.
A kind of " phosphatization liquid and preparation method thereof " is disclosed in Chinese patent CN1037936A, form by pickle solution and phosphatization liquid two portions, the percentage component of pickle solution is phosphoric acid 5-50%, sulphur urine 0.005-0.015%, sodium laurylsulfonate 0.05-0.15%, peregal 0.05-0.15%, chlorination hexadecyl trimethylamine 0.05-0.15%, citric acid 1-10%, water 93.845-39.535%; The percentage component of phosphatization liquid is nitrocalcite 5-15%, zinc phosphate 5-15%, nickelous nitrate 0.15-0.25%, Xiao Suangu 0.045-0.55%, nitric acid tin 0.045-0.055%, citric acid 0.15-0.25%, tartrate 0.045-0.055%, E.D.T.A6.045-0.055%, tensio-active agent OP0.008-0.002%, water 89.512-69.26%; Its principal feature is earlier with metal pickling, and then under 65-70 ℃ condition phosphatization, its shortcoming is with metal pickling in strong inorganic acid, bring defective can for the formation of phosphatize phosphate coat, and phosphatization speed is slow, needs heating equally, has the identical shortcoming of above-mentioned prior art.
The objective of the invention is to provide for fear of above-mentioned the deficiencies in the prior art part a kind of low temperature, fast, low, the little slag of acidity, nontoxic phosphating solution at room temperature and compound method thereof.
The objective of the invention is to realize by following measure:
A kind of phosphating solution at room temperature contains phosphoric acid, nitric acid, citric acid, zinc nitrate, nickelous nitrate, cupric nitrate, zinc oxide, hydrogen peroxide and water, and its weight percent composition is:
Phosphoric acid 8-12% nitric acid 1.8-3.2%
Citric acid 1.1-2.9% zinc nitrate 15.5-22.8%
Nickelous nitrate 0.4-1.2% cupric nitrate 0.4-1.2%
Zinc oxide 3-4.5% hydrogen peroxide 0.2-0.7%
Phthalic anhydride 0.08-1%, its surplus is a water.
A kind of compound method of phosphating solution at room temperature, undertaken by following step: the phosphoric acid in 1. will filling a prescription earlier, nitric acid, citric acid are by its weight percent stirring and evenly mixing in acid-resistant container; 2. slowly add the burnett's solution of pressing its weight percent water furnishing pasty state in the prescription, the limit edged stirs; 3. and then successively add entry, phthalic anhydride, hydrogen peroxide, cupric nitrate, nickelous nitrate, zinc nitrate by weight percent in the prescription, be stirred to dissolving fully;
Purpose of the present invention can also realize by following measure:
Phosphate anion in a kind of phosphorization at room temperature liquid formula is 0.4-2.2 with the nitrate ion ratio, and its optimum formula ratio is 2.2; The Sodium Nitrite that needs to add 0.3-0.5% in phosphatization liquid is done promotor, and adds continuously in parkerizing process.
A kind of phosphating solution at room temperature, its weight percent are formed:
Phosphoric acid 8-8.8% nitric acid 1.8-2%
Citric acid 1.1-1.5% zinc nitrate 20-22.8%
Nickelous nitrate 0.5-0.7% cupric nitrate 0.5-0.7%
Zinc oxide 4.2-4.5% hydrogen peroxide 0.6-0.7%
Phthalic anhydride 0.5-1%, its surplus is a water.
A kind of phosphating solution at room temperature, its weight hundred for forming is:
Phosphatase 11 1-11.8% nitric acid 2.8-3.2%
Citric acid 2.0-2.1% zinc nitrate 15.5-17%
Nickelous nitrate 1-1.2% cupric nitrate 1-1.2%
Zinc oxide 3-3.3% hydrogen peroxide 0.2-0.4%
Phthalic anhydride 0.08-0.1%, its surplus is a water
Hydrogen peroxide in the phosphorization at room temperature liquid formula can replace with Sodium peroxoborate, and its weight percent is constant.
Reaction mechanism of the present invention is: the phosphatization liquid for preparing is the phosphoric acid dihydro zinc aqueous solution that contains a certain amount of free phosphoric acid, the matrix metal that needs phosphatization is after immersing phosphating solution at room temperature after rust cleaning, the degreasing, and the insoluble zinc phosphate that the primary zinc phosphate hydrolysis produces is deposited on base metal surface and forms undissolved film; And matrix metal dissolves in phosphatization liquid and generates generation ferrous phosphate and releasing hydrogen gas, the solvable and ionization generation ferrous ion of generation ferrous phosphate, and ferrous ion and primary zinc phosphate reaction generate phosphorus phyllite Zn
2Fe(PO
4)
24H
2O is deposited on base metal surface and forms not dissolving film; Matrix metal also can be directly and the primary zinc phosphate reaction generate phosphorus phyllite Zn
2Fe(PO
4)
24H
2O metal refining surface forms not dissolving film; Citric acid in the phosphatization liquid, nickel ion, cupric ion and hydrogen peroxide are accelerator, can quicken the dissolving of matrix metal, shorten film formation time, nitrate and nitrite in the phosphatization liquid is the oxidisability accelerator in addition, can make ferrous ion be oxidized to iron ion, generate Orthophosphoric acid Ferrum, keep in the solution and the stable content of the iron in the phosphatize phosphate coat on a certain numerical value.
Principal reaction formula of the present invention is:
The present invention has following advantage compared to existing technology:
1, phosphatization liquid of the present invention is easy to operate, need not heat, and bonderizing can carry out under room temperature 10-25 ℃; Less energy consumption, save energy.
2, the tank liquor free acidity of phosphatization liquid of the present invention is low, and its total acidity is also low, and need not heat, and has improved operating environment, has reduced the corrosion to phosphatization equipment and heating installation.
3, the phosphatization speed of phosphatization liquid of the present invention is fast, and the film outward appearance does not evenly have coarse grain, adhere firmly.
4, improved the ratio of phosphate anion and nitrate ion in the phosphatization liquid of the present invention, the body refuse that produces in parkerizing process is less, and body refuse is soft, removes easily.
5, phosphatization liquid of the present invention does not contain hazardous substance, and does not produce objectionable impurities in reaction process, and after waste liquid neutralized naturally, through precipitation, aggegation, slagging-off cleaning regularly, clear liquid can directly discharge.
6, phosphatization liquid of the present invention, through the phosphatize phosphate coat of parkerized metal, antirust ability is strong, and epoxy and polyester powder coating are adapted to very much, and crystallization is thin, whole coatings slip resistance height.
Embodiments of the invention one:
In water per ton, add 45 kilograms of phosphatization liquid, wherein the weight percent component of phosphatization liquid is phosphoric acid 8%, nitric acid 1.8%, citric acid 1.1%, zinc nitrate 15.5%, nickelous nitrate 0.4%, cupric nitrate 0.4%, zinc oxide 3%, hydrogen peroxide 0.2%, phthalic anhydride 0.08%, and its surplus is a water; Its compound method is undertaken by following step: 1. earlier the phosphoric acid in the above-mentioned prescription, nitric acid and citric acid are pressed its weight percent mixing in acid-resistant container; 2. and slowly add the burnett's solution of pressing its weight percent water furnishing pasty state in the above-mentioned prescription, the limit edged stirs; 3. and then successively the water, phthalic anhydride, hydrogen peroxide, cupric nitrate, nickelous nitrate, the zinc nitrate that add weight percent in the above-mentioned prescription are stirred to dissolving fully.
Metal after degreasing, washing, rust cleaning, surface adjustment are handled is immersed in the above-mentioned phosphating solution, and at room temperature, phosphatization generated uniform silver-gray phosphatize phosphate coat (zinc system) after 5 minutes, its thickness 2 μ m.
Embodiment two:
In water per ton, add 300 kilograms of phosphatization liquid, and add 0.4% Sodium Nitrite; Wherein the weight percent component of phosphatization liquid is phosphatase 11 2%, nitric acid 3.2%, citric acid 2.9%, zinc nitrate 22.8%, nickelous nitrate 1.2%, cupric nitrate 1.2%, zinc oxide 4.5%, hydrogen peroxide 0.7%, phthalic anhydride 1%, and its surplus is a water; Its compound method is identical with embodiment one.
Metal after degreasing, washing, rust cleaning, surface adjustment are handled is immersed in the above-mentioned phosphating solution, and at room temperature, phosphatization generated uniform silver-gray phosphatize phosphate coat (zinc system) after 6 minutes, its thickness 3 μ m.
Embodiment three:
In water per ton, add 90 kilograms of phosphatization liquid, and add 0.35% Sodium Nitrite; Wherein the weight percent component of phosphatization liquid is phosphoric acid 8.8%, nitric acid 2%, citric acid 1.5%, zinc nitrate 20%, nickelous nitrate 0.7%, cupric nitrate 0.7%, zinc oxide 4.2%, hydrogen peroxide 0.6%, phthalic anhydride 0.5%, and its surplus is a water; Its compound method is identical with embodiment one.
Metal after degreasing, washing, rust cleaning, surface adjustment are handled is immersed in the above-mentioned phosphating solution, and at room temperature, phosphatization generated uniform silver-gray phosphatize phosphate coat (zinc system) after 5 minutes, its thickness 2.5 μ m.
Embodiment four:
In water per ton, add 200 kilograms of phosphatization liquid, and add 0.5% Sodium Nitrite; Wherein the weight percent component of phosphatization liquid is phosphatase 11 1%, nitric acid 2.8%, citric acid 2%, zinc nitrate 17%, nickelous nitrate 1%, cupric nitrate 1%, zinc oxide 3.3%, hydrogen peroxide 0.4%, phthalic anhydride 0.1%, and its surplus is a water; Its compound method is identical with embodiment one.
Its treatment process and the foregoing description are together.
Embodiment five:
In water per ton, add 122.5 kilograms of phosphatization liquid, and add 0.45% Sodium Nitrite; Wherein the weight percent component of phosphatization liquid is phosphatase 11 1.8%, nitric acid 2.5%, citric acid 2.1%, zinc nitrate 22%, nickelous nitrate 0.6%, cupric nitrate 0.6%, zinc oxide 3.1%, hydrogen peroxide 0.3%, phthalic anhydride 0.11%, and its surplus is a water; Its compound method is identical with embodiment one.
Its treatment process and the foregoing description are together.
Embodiment six:
Hydrogen peroxide in the phosphatization liquid of the present invention can replace with Sodium peroxoborate, and its weight percent component is constant.
Metal is after phosphatization liquid of the present invention at room temperature floods or sprays processing, in air, place 48 hours stainless, and qualified through the rust prevention test of sodium-chlor and copper sulfate point examination destructive, this phosphatization liquid be suitable for the metallic surface electrostatic painting of automobile, bike, refrigerator, washing machine, steel sash and other daily daily necessitiess or the pre-treatment before the japanning and antirust, change dye, abrasion performance uses.
Claims (8)
1, a kind of phosphating solution at room temperature contains phosphoric acid, nitric acid, citric acid, zinc nitrate, nickelous nitrate, cupric nitrate, hydrogen peroxide and water, it is characterized in that the percentage component of phosphatization liquid is
Phosphoric acid 8-12% nitric acid 1.8-3.2%
Citric acid 1.1-2.9% zinc nitrate 15.5-22.8%
Nickelous nitrate 0.4-1.2% cupric nitrate 0.4-1.2%
Zinc oxide 3-4.5% hydrogen peroxide 0.2-0.7%
Phthalic anhydride 0.08-1%, its surplus is a water
2, a kind of compound method of phosphating solution at room temperature is characterized in that being undertaken by following step: phosphoric acid, nitric acid and the citric acid in 1. will filling a prescription earlier is by its weight percent mixing in acid-resistant container; 2. and slowly add the burnett's solution of pressing its weight percent water furnishing pasty state in the prescription, the limit edged stirs; 3. and then successively add entry, phthalic anhydride, hydrogen peroxide, cupric nitrate, nickelous nitrate, zinc nitrate by weight percent in the prescription, be stirred to dissolving fully;
3, phosphating solution at room temperature according to claim 1 is characterized in that phosphate anion and nitrate ion ratio are 0.4～2.2.
4, phosphating solution at room temperature as claimed in claim 1 is characterized in that the Sodium Nitrite of adding 0.3-0.5% in solution is done promotor, and adds continuously in parkerizing process.
5, phosphating solution at room temperature as claimed in claim 1 is characterized in that:
Phosphoric acid 8-8.8% nitric acid 1.8-2%
Citric acid 1.1-1.5% zinc nitrate 20-22.8%
Nickelous nitrate 0.5-0.7% cupric nitrate 0.5-0.7%
Zinc oxide 4.2-4.5% hydrogen peroxide 0.6-0.7%
Phthalic anhydride 0.5-1%, its surplus is a water.
6, phosphating solution at room temperature as claimed in claim 1 is characterized in that:
Phosphatase 11 1-11.8% nitric acid 2.8-3.2%
Citric acid 2.0-2.1% zinc nitrate 15.5-17%
Nickelous nitrate 1-1.2% cupric nitrate 1-1.2%
Zinc oxide 3-3.3% hydrogen peroxide 0.2-0.4%
Phthalic anhydride 0.08-0.1%, its surplus is a water.
7,, it is characterized in that the phosphate anion of phosphatization liquid optimum formula and nitrate ion ratio are 2.2 as claim 1,5 described phosphating solution at room temperature.
8, as claim 1,5,6 described phosphating solution at room temperature, the hydrogen peroxide in it is characterized in that filling a prescription can replace with Sodium peroxoborate, and its weight percent is constant.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 91104466 CN1022496C (en) | 1991-06-29 | 1991-06-29 | room temperature phosphating solution and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 91104466 CN1022496C (en) | 1991-06-29 | 1991-06-29 | room temperature phosphating solution and preparation method thereof |
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| Publication Number | Publication Date |
|---|---|
| CN1057681A true CN1057681A (en) | 1992-01-08 |
| CN1022496C CN1022496C (en) | 1993-10-20 |
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ID=4906645
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 91104466 Expired - Fee Related CN1022496C (en) | 1991-06-29 | 1991-06-29 | room temperature phosphating solution and preparation method thereof |
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|---|---|
| CN (1) | CN1022496C (en) |
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1092245C (en) * | 1992-12-22 | 2002-10-09 | 亨凯尔公司 | Substantially nickel-free phosphate conversion coating composition and process |
| CN101864563A (en) * | 2010-07-14 | 2010-10-20 | 西安北方光电有限公司 | Phosphating liquid of high corrosion resistance black phosphating production process |
| CN101705485B (en) * | 2009-11-16 | 2011-12-21 | 大连三达奥克化学股份有限公司 | Wiping type metal conversion treatment agent and preparation method |
| CN103184444A (en) * | 2013-03-29 | 2013-07-03 | 柳州煜华科技有限公司 | Phosphating solution suitable for metal fastening piece |
| CN103397324A (en) * | 2013-08-07 | 2013-11-20 | 彭万焜 | Multifunctional phosphating solution, and preparation method and application thereof |
| CN103469189A (en) * | 2013-08-23 | 2013-12-25 | 吴江龙硕金属制品有限公司 | Metal phosphatization liquid and preparation method thereof |
| CN104388914A (en) * | 2014-12-16 | 2015-03-04 | 常熟市东方特种金属材料厂 | Method for preparing phosphating liquid of carbon steel material |
| CN105463422A (en) * | 2015-12-31 | 2016-04-06 | 芜湖市金宇石化设备有限公司 | Phosphating method before coating automobile doors |
| CN105543822A (en) * | 2015-12-31 | 2016-05-04 | 芜湖市金宇石化设备有限公司 | Treatment liquid for phosphating before painting of automobile door |
| CN105603406A (en) * | 2015-12-31 | 2016-05-25 | 芜湖市金宇石化设备有限公司 | Method for preparing treatment fluid for phosphating treatment before coating automobile doors |
| CN106757280A (en) * | 2016-12-13 | 2017-05-31 | 河南恒星钢缆股份有限公司 | A kind of low temperature On-line electrolytic dissolution Phosphating Solution |
| CN107523820A (en) * | 2017-07-04 | 2017-12-29 | 安徽腾龙泵阀制造有限公司 | A kind of inorganic acid passivating solution for electro-galvanized layer |
| CN110129782A (en) * | 2019-05-20 | 2019-08-16 | 浙江伟星实业发展股份有限公司 | A kind of film agent, preparation method and pull head treatment process |
| CN111793793A (en) * | 2020-07-31 | 2020-10-20 | 张家港市升恒机械设备制造有限公司 | Phosphorization rust-proof treatment method for explosion-proof cabinet |
| CN113881934A (en) * | 2021-11-04 | 2022-01-04 | 湖南金化科技集团有限公司 | Zinc-based phosphating solution with less slag and ash |
-
1991
- 1991-06-29 CN CN 91104466 patent/CN1022496C/en not_active Expired - Fee Related
Cited By (20)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1092245C (en) * | 1992-12-22 | 2002-10-09 | 亨凯尔公司 | Substantially nickel-free phosphate conversion coating composition and process |
| CN101705485B (en) * | 2009-11-16 | 2011-12-21 | 大连三达奥克化学股份有限公司 | Wiping type metal conversion treatment agent and preparation method |
| CN101864563A (en) * | 2010-07-14 | 2010-10-20 | 西安北方光电有限公司 | Phosphating liquid of high corrosion resistance black phosphating production process |
| CN101864563B (en) * | 2010-07-14 | 2012-02-01 | 西安北方光电有限公司 | Phosphating liquid of high corrosion resistance black phosphating production process |
| CN103184444A (en) * | 2013-03-29 | 2013-07-03 | 柳州煜华科技有限公司 | Phosphating solution suitable for metal fastening piece |
| CN103184444B (en) * | 2013-03-29 | 2016-08-03 | 柳州煜华科技有限公司 | A kind of Phosphating Solution being applicable to metal fastenings |
| CN103397324A (en) * | 2013-08-07 | 2013-11-20 | 彭万焜 | Multifunctional phosphating solution, and preparation method and application thereof |
| CN103397324B (en) * | 2013-08-07 | 2016-04-13 | 彭万焜 | A kind of multifunction phosphide liquid and its production and use |
| CN103469189A (en) * | 2013-08-23 | 2013-12-25 | 吴江龙硕金属制品有限公司 | Metal phosphatization liquid and preparation method thereof |
| CN104388914A (en) * | 2014-12-16 | 2015-03-04 | 常熟市东方特种金属材料厂 | Method for preparing phosphating liquid of carbon steel material |
| CN105543822A (en) * | 2015-12-31 | 2016-05-04 | 芜湖市金宇石化设备有限公司 | Treatment liquid for phosphating before painting of automobile door |
| CN105603406A (en) * | 2015-12-31 | 2016-05-25 | 芜湖市金宇石化设备有限公司 | Method for preparing treatment fluid for phosphating treatment before coating automobile doors |
| CN105463422A (en) * | 2015-12-31 | 2016-04-06 | 芜湖市金宇石化设备有限公司 | Phosphating method before coating automobile doors |
| CN106757280A (en) * | 2016-12-13 | 2017-05-31 | 河南恒星钢缆股份有限公司 | A kind of low temperature On-line electrolytic dissolution Phosphating Solution |
| CN107523820A (en) * | 2017-07-04 | 2017-12-29 | 安徽腾龙泵阀制造有限公司 | A kind of inorganic acid passivating solution for electro-galvanized layer |
| CN110129782A (en) * | 2019-05-20 | 2019-08-16 | 浙江伟星实业发展股份有限公司 | A kind of film agent, preparation method and pull head treatment process |
| CN110129782B (en) * | 2019-05-20 | 2021-10-22 | 浙江伟星实业发展股份有限公司 | Skin membrane agent, preparation method thereof and puller treatment process |
| CN111793793A (en) * | 2020-07-31 | 2020-10-20 | 张家港市升恒机械设备制造有限公司 | Phosphorization rust-proof treatment method for explosion-proof cabinet |
| CN113881934A (en) * | 2021-11-04 | 2022-01-04 | 湖南金化科技集团有限公司 | Zinc-based phosphating solution with less slag and ash |
| CN113881934B (en) * | 2021-11-04 | 2023-04-21 | 湖南金化科技集团有限公司 | Zinc phosphating solution with less slag and ash |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1022496C (en) | 1993-10-20 |
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