CN104120418A - Room temperature fast phosphatization solution and preparation method thereof - Google Patents

Room temperature fast phosphatization solution and preparation method thereof Download PDF

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Publication number
CN104120418A
CN104120418A CN201310148650.6A CN201310148650A CN104120418A CN 104120418 A CN104120418 A CN 104120418A CN 201310148650 A CN201310148650 A CN 201310148650A CN 104120418 A CN104120418 A CN 104120418A
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China
Prior art keywords
solution
ordinary
fast bonderizing
temp fast
bonderizing liquor
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CN201310148650.6A
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CN104120418B (en
Inventor
易传贵
王瑞
刘永
史鸿威
陈延辉
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State Grid Corp of China SGCC
Pinggao Group Co Ltd
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State Grid Corp of China SGCC
Pinggao Group Co Ltd
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Abstract

The invention discloses a room temperature fast phosphatization solution and a preparation method thereof. The phosphatization solution provided by the invention comprises the following raw materials: 25-40g/L zinc oxide, 30-50ml/L phosphoric acid, 20-35ml/L nitric acid, 1.5-2.5g/L trisodium phosphate, 8.0-12.0g/L sodium polyphosphate, 5.0-8.0g/L nickel nitrate, 0.6-1.5g/L manganous nitrate, 3.0-5.0g/L sodium nitrate, 3.5-8.0g/L a promoting agent, and 12.0-18.0g/L a complexing agent. The preparation method includes: mixing the formula raw materials uniformly, adjusting the total acidity to 55-85, the free acidity to 3.0-6.0, and the concentration of the promoting agent to 0.8-4.0, and conducting dipping phosphorization on a steel workpiece for 1.5-3min, thus forming a good film with strong corrosion resistance. The formula is reasonable, the preparation method is simple, and the cost is low.

Description

A kind of ordinary-temp fast bonderizing liquor and preparation method thereof
Technical field
The present invention relates to a kind of ordinary-temp fast bonderizing liquor and preparation method thereof, belong to metal finishing and corrosion-resistant field.
Background technology
Phosphorization treatment process technology is widely used in the fields such as automotive industry, mechanical industry, household electrical appliance and weaponry manufacture, through development for many years, many new achievements have been obtained, particularly the industrial application of phosphatization is expanded greatly, makes it become the indispensable important process technology such as iron and steel processing, anticorrosion, decoration.In electric field switch cabinet body external coating, phosphorization membrane has a great impact the performance of whole rete as the bottom of application, require phosphorization membrane to there is good solidity to corrosion and there is good bonding force etc. with paint film and plastic-blasting rete, in prior art, Phosphating Solution major part is zinc-calcium system, exist treatment temp higher, the defect that phosphating time is longer.Therefore, studying a kind of ordinary-temp fast bonderizing liquor and preparation method thereof has great significance for increasing switch cabinet surface corrosion resistance ability.
Summary of the invention
The object of this invention is to provide a kind of ordinary-temp fast bonderizing liquor.
In addition, the present invention also aims to provide a kind of preparation method of ordinary-temp fast bonderizing liquor.
In order to realize above object, the technical solution adopted in the present invention is: a kind of ordinary-temp fast bonderizing liquor, and every liter of Phosphating Solution comprises following raw material:
Zinc oxide 25~40g
Phosphoric acid 30~50ml
Nitric acid 20~35ml
Tertiary sodium phosphate 1.5~2.5g
Sodium polyphosphate 8.0~12.0g
Nickelous nitrate 5.0~8.0g
Manganous nitrate 0.6~1.5g
SODIUMNITRATE 3.0~5.0g
Promotor 3.5~8.0g
Complexing agent 12.0~18.0g.
Mass percent >=85% of raw material phosphoric acid, raw material nitric acid mass percent is 65%~68%.
Ordinary-temp fast bonderizing liquor total acidity is 55~85 points, and free acidity is 3.0~6.0 points.
Promoter concentration is 0.8~4.0 point.
Promotor is a kind of or arbitrary combination in Sodium Nitrite, Potcrate, Sodium orthomolybdate, nitrobenzene sodium sulfonate.
Complexing agent is a kind of or arbitrary combination in Seignette salt, trisodium citrate, ethylenediamine tetraacetic acid (EDTA).
A preparation method for ordinary-temp fast bonderizing liquor, concrete operation step is as follows
(1) take zinc oxide, after water furnishing pasty state, add nitric acid, phosphoric acid, add until completely dissolved complexing agent to stir to clarify, be labeled as A solution;
(2) taking promotor and manganous nitrate adds water and is stirred to solution clarification and is labeled as B solution;
(3) B solution is joined in A solution, and add tertiary sodium phosphate, sodium polyphosphate, nickelous nitrate and SODIUMNITRATE, stir, be labeled as C solution;
(4) regulate total acidity to 55~85 point of C solution, free acidity to 3.0~6.0 point, promoter concentration to 0.8~4.0 point, obtains ordinary-temp fast bonderizing liquor.
The testing method of total acidity is: get Phosphating Solution 10ml to Erlenmeyer flask, with 2 of phenolphthalein indicators, with the NaOH standardized solution of 0.100mol/L, be titrated to incarnadine, the milliliter number that consumes NaOH solution is total acidity.
The testing method of free acidity is: get Phosphating Solution 10ml to Erlenmeyer flask, add 2 of bromophenol blue indicators, with the NaOH standardized solution of 0.100mol/L, be titrated to yellow disappearance, the milliliter number of the NaOH solution of consumption is free acidity.
The testing method of promoter concentration is: Phosphating Solution is injected in 10ml fermentation tube, ninety percent is full, with spoon, 2~3g thionamic acid is joined in fermentation tube, with hand, block the fermentation mouth of pipe and fermentation tube is inverted rapidly, treat that thionamic acid landing to bottom turns fermentation tube around rapidly again, after one minute, read the concentration that scale numerical value is promotor and count.
The present invention's chemical feedstocks used is analytical pure.
The integral part that in the present invention, phosphoric acid, nitric acid and zinc oxide are basal liquid; Tertiary sodium phosphate, sodium polyphosphate, SODIUMNITRATE and manganous nitrate, nickelous nitrate to crystallization of refinement, improve membranous layer binding force, solidity to corrosion and maintenance system stablely there is important effect; Promotor works to accelerate phosphorization filming speed; Complexing agent plays complexing to zinc, iron ion and the stable of maintenance system is played a role.
One's duty invention has following beneficial effect: formula of the present invention and preparation method be simple, rationally, and cost is lower, under room temperature, processed workpiece is placed in to Phosphating Solution and floods 1.5~3min and can form good rete, has good erosion resistance.
Embodiment
Below in conjunction with embodiment, a kind of ordinary-temp fast bonderizing liquor of the present invention and preparation method thereof is described further.
Embodiment 1
A kind of ordinary-temp fast bonderizing liquor of the present embodiment, every liter of Phosphating Solution comprises following raw material:
Zinc oxide 35g/L
Phosphatase 24 0ml/L
Nitric acid 25ml/L
Tertiary sodium phosphate 2.0g/L
Sodium polyphosphate 10.0g/L
Nickelous nitrate 6.0g/L
Manganous nitrate 1.0g/L
SODIUMNITRATE 4.0g/L
Sodium Nitrite 2.8g/L
Potcrate 1.5g/L
Sodium orthomolybdate 0.2g/L
Nitrobenzene sodium sulfonate 0.8g/L
Seignette salt 8.0g/L
Ethylenediamine tetraacetic acid (EDTA) 3.8g/L
Trisodium citrate 2.5g/L
Preparation method's concrete operation step of a kind of ordinary-temp fast bonderizing liquor of the present embodiment is as follows:
(1) take 35g Zinc oxide powder, with 100ml distilled water furnishing pasty state, stand-by; In the beaker of 1000mL, add 200ml distilled water, after the zinc oxide of furnishing pasty state being added in this beaker under whipped state, slowly add 40ml phosphoric acid, after stirring 20min, after Solution Dispersion is complete, slowly add again 25ml nitric acid, Seignette salt 8.0g, ethylenediamine tetraacetic acid (EDTA) 3.8g, trisodium citrate 2.5g, stir to clarify, be labeled as A solution;
(2) take Sodium Nitrite 2.8g, Potcrate 1.5g, Sodium orthomolybdate 0.2g, nitrobenzene sodium sulfonate 0.8g, manganous nitrate 1.0g, adds water and is stirred to solution clarification, is labeled as B solution;
(3) B solution is joined in A solution, and add nickelous nitrate 6.0g, tertiary sodium phosphate 2.0g, sodium polyphosphate 10.0g, SODIUMNITRATE 4.0g, adds water to 1000mL and stirs, and is labeled as C solution;
(4) with NaOH solution key joint C solution total acidity to 63 point of 1.0mol/L, free acidity to 4.5 point, and to record promoter concentration be 2.2 points, obtains ordinary-temp fast bonderizing liquor.
Under room temperature, iron plate is placed in to the performance of the phosphorization membrane recording after the Phosphating Solution dip phosphatizing 1.5min of the present embodiment as table 1.
Film performance after the Phosphating Solution phosphatization of table 1. embodiment 1
Test event Performance
The experiment of copper sulfate drop 40s
Thickness 2.5μm
Film weight 1.5g/m 2
Embodiment 2
A kind of ordinary-temp fast bonderizing liquor of the present embodiment, every liter of Phosphating Solution comprises following raw material:
Zinc oxide 40g/L
Phosphoric acid 50ml/L
Nitric acid 35ml/L
Tertiary sodium phosphate 2.5g/L
Sodium polyphosphate 12.0g/L
Nickelous nitrate 8.0g/L
Manganous nitrate 1.5g/L
SODIUMNITRATE 5.0g/L
Sodium Nitrite 4.0g/L
Potcrate 2.8g/L
Sodium orthomolybdate 0.2g/L
Nitrobenzene sodium sulfonate 1.0g/L
Seignette salt 12.0g/L
Ethylenediamine tetraacetic acid (EDTA) 2.2g/L
Trisodium citrate 3.8g/L
The preparation method's of a kind of ordinary-temp fast bonderizing liquor of the present embodiment concrete operation step is with embodiment 1, the carrying out that raw material and proportioning thereof provide according to the present embodiment.
With the NaOH solution of 1.0mol/L, regulate C solution total acidity to 85 point, free acidity to 6.0 point, and to record promoter concentration be 3.9 points, obtains ordinary-temp fast bonderizing liquor.
Under room temperature, iron plate is placed in to the performance of the phosphorization membrane recording after the Phosphating Solution dip phosphatizing 2.0min of the present embodiment as table 2.
Film performance after the Phosphating Solution phosphatization of table 2. embodiment 2
Test event Performance
The experiment of copper sulfate drop 35s
Thickness 2.2μm
Film weight 1.8g/m 2
Embodiment 3
A kind of ordinary-temp fast bonderizing liquor of the present embodiment, every liter of Phosphating Solution comprises following raw material:
Zinc oxide 25g/L
Phosphoric acid 30ml/L
Nitric acid 20ml/L
Tertiary sodium phosphate 1.5g/L
Sodium polyphosphate 8.0g/L
Nickelous nitrate 5.0g/L
Manganous nitrate 0.6g/L
SODIUMNITRATE 3.0g/L
Sodium Nitrite 2.0g/L
Potcrate 0.6g/L
Sodium orthomolybdate 0.4g/L
Nitrobenzene sodium sulfonate 0.8g/L
Seignette salt 9.0g/L
Ethylenediamine tetraacetic acid (EDTA) 1.7g/L
Trisodium citrate 1.3g/L
The preparation method's of a kind of ordinary-temp fast bonderizing liquor of the present embodiment concrete operation step is with embodiment 1, the carrying out that raw material and proportioning thereof provide according to the present embodiment.
With the NaOH solution of 1.0mol/L, regulate C solution total acidity to 57 point, free acidity to 3.2 point, and to record promoter concentration be 0.8 point, obtains ordinary-temp fast bonderizing liquor.
Under room temperature, iron plate is placed in to the performance of the phosphorization membrane recording after the present embodiment Phosphating Solution dip phosphatizing 3.0min as table 3.
Film performance after the Phosphating Solution phosphatization of table 3. embodiment 3
Test event Performance
The experiment of copper sulfate drop 42s
Thickness 3.0μm
Film weight 2.8g/m 2
Embodiment 4
A kind of ordinary-temp fast bonderizing liquor of the present embodiment, every liter of Phosphating Solution comprises following raw material:
Zinc oxide 28g/L
Phosphoric acid 35ml/L
Nitric acid 30ml/L
Tertiary sodium phosphate 2.5g/L
Sodium polyphosphate 10.0g/L
Nickelous nitrate 6.5g/L
Manganous nitrate 0.8g/L
SODIUMNITRATE 3.0g/L
Sodium Nitrite 3.8g/L
Seignette salt 15.0g/L
The preparation method's of a kind of ordinary-temp fast bonderizing liquor of the present embodiment concrete operation step is with embodiment 1, the carrying out that raw material and proportioning thereof provide according to the present embodiment.
With the NaOH solution of 1.0mol/L, regulate C solution total acidity to 68 point, free acidity to 5.2 point, and to record promoter concentration be 3.2 points, obtains ordinary-temp fast bonderizing liquor.
Under room temperature, iron plate is placed in to the performance of the phosphorization membrane recording after the present embodiment Phosphating Solution dip phosphatizing 3.0min as table 4.
Film performance after the Phosphating Solution phosphatization of table 4. embodiment 4
Test event Performance
The experiment of copper sulfate drop 38s
Thickness 3.3μm
Film weight 2.9g/m 2

Claims (7)

1. an ordinary-temp fast bonderizing liquor, is characterized in that, every liter of Phosphating Solution comprises following raw material:
Zinc oxide 25~40g
Phosphoric acid 30~50ml
Nitric acid 20~35ml
Tertiary sodium phosphate 1.5~2.5g
Sodium polyphosphate 8.0~12.0g
Nickelous nitrate 5.0~8.0g
Manganous nitrate 0.6~1.5g
SODIUMNITRATE 3.0~5.0g
Promotor 3.5~8.0g
Complexing agent 12.0~18.0g.
2. a kind of ordinary-temp fast bonderizing liquor according to claim 1, is characterized in that, mass percent >=85% of raw material phosphoric acid, and raw material nitric acid mass percent is 65%~68%.
3. a kind of ordinary-temp fast bonderizing liquor according to claim 1, is characterized in that, ordinary-temp fast bonderizing liquor total acidity is 55~85 points, and free acidity is 3.0~6.0 points.
4. a kind of ordinary-temp fast bonderizing liquor according to claim 1, is characterized in that, promoter concentration is 0.8~4.0 point.
5. a kind of ordinary-temp fast bonderizing liquor according to claim 1, is characterized in that, promotor is a kind of or arbitrary combination in Sodium Nitrite, Potcrate, Sodium orthomolybdate, nitrobenzene sodium sulfonate.
6. a kind of ordinary-temp fast bonderizing liquor according to claim 1, is characterized in that, complexing agent is a kind of or arbitrary combination in Seignette salt, trisodium citrate, ethylenediamine tetraacetic acid (EDTA).
7. a preparation method for ordinary-temp fast bonderizing liquor as claimed in claim 1, is characterized in that, concrete operation step is as follows:
(1) take zinc oxide, after water furnishing pasty state, add nitric acid, phosphoric acid, add until completely dissolved complexing agent to stir to clarify, be labeled as A solution;
(2) taking promotor and manganous nitrate adds water and is stirred to solution clarification and is labeled as B solution;
(3) B solution is joined in A solution, and add tertiary sodium phosphate, sodium polyphosphate, nickelous nitrate and SODIUMNITRATE, stir, be labeled as C solution;
(4) regulate total acidity to 55~85 point of C solution, free acidity to 3.0~6.0 point, promoter concentration to 0.8~4.0 point, obtains ordinary-temp fast bonderizing liquor.
CN201310148650.6A 2013-04-25 2013-04-25 A kind of ordinary-temp fast bonderizing liquor and preparation method thereof Active CN104120418B (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104711562A (en) * 2015-03-18 2015-06-17 周子豪 Ternary phosphating agent
WO2017219368A1 (en) * 2016-06-24 2017-12-28 深圳市恒兆智科技有限公司 Manganese series phosphating agent, metal piece and surface phosphating treatment method therefor
WO2017219372A1 (en) * 2016-06-24 2017-12-28 深圳市恒兆智科技有限公司 Zinc-manganese series phosphating agent, metal piece and surface phosphating treatment method therefor
CN111375649A (en) * 2018-12-29 2020-07-07 东莞科力线材技术有限公司 Preparation method of automobile fastener wire

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Publication number Priority date Publication date Assignee Title
US20020107133A1 (en) * 2000-05-19 2002-08-08 Tomasz Troczynski Process for making chemically bonded composite hydroxide ceramics
CN1401820A (en) * 2002-09-18 2003-03-12 中国重型汽车集团有限公司 Ordinary temp. parkerizing liquid
CN1847455A (en) * 2006-05-11 2006-10-18 武汉大学 Ternary Zn-Ni-Mn phosphorizing solution
CN101063200A (en) * 2006-04-24 2007-10-31 宋晨玮 Normal temperature phosphating liquor
CN101328583A (en) * 2007-06-22 2008-12-24 宝山钢铁股份有限公司 Manganese phosphating liquor, preparation and use thereof
CN101812682A (en) * 2009-02-24 2010-08-25 中化化工科学技术研究总院 Zinc phosphating solution of aluminium and aluminium alloy
CN102719874A (en) * 2011-03-30 2012-10-10 重庆市荣时金属表面处理剂有限公司 Cathode electrophoretic phosphatizing agent

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20020107133A1 (en) * 2000-05-19 2002-08-08 Tomasz Troczynski Process for making chemically bonded composite hydroxide ceramics
CN1401820A (en) * 2002-09-18 2003-03-12 中国重型汽车集团有限公司 Ordinary temp. parkerizing liquid
CN101063200A (en) * 2006-04-24 2007-10-31 宋晨玮 Normal temperature phosphating liquor
CN1847455A (en) * 2006-05-11 2006-10-18 武汉大学 Ternary Zn-Ni-Mn phosphorizing solution
CN101328583A (en) * 2007-06-22 2008-12-24 宝山钢铁股份有限公司 Manganese phosphating liquor, preparation and use thereof
CN101812682A (en) * 2009-02-24 2010-08-25 中化化工科学技术研究总院 Zinc phosphating solution of aluminium and aluminium alloy
CN102719874A (en) * 2011-03-30 2012-10-10 重庆市荣时金属表面处理剂有限公司 Cathode electrophoretic phosphatizing agent

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104711562A (en) * 2015-03-18 2015-06-17 周子豪 Ternary phosphating agent
CN104711562B (en) * 2015-03-18 2017-12-19 周子豪 A kind of ternary bonderite
WO2017219368A1 (en) * 2016-06-24 2017-12-28 深圳市恒兆智科技有限公司 Manganese series phosphating agent, metal piece and surface phosphating treatment method therefor
WO2017219372A1 (en) * 2016-06-24 2017-12-28 深圳市恒兆智科技有限公司 Zinc-manganese series phosphating agent, metal piece and surface phosphating treatment method therefor
CN111375649A (en) * 2018-12-29 2020-07-07 东莞科力线材技术有限公司 Preparation method of automobile fastener wire

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