CN103773234B - Silane surface treatment agent and preparation method thereof - Google Patents
Silane surface treatment agent and preparation method thereof Download PDFInfo
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- CN103773234B CN103773234B CN201410011960.8A CN201410011960A CN103773234B CN 103773234 B CN103773234 B CN 103773234B CN 201410011960 A CN201410011960 A CN 201410011960A CN 103773234 B CN103773234 B CN 103773234B
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- surface treatment
- acid
- treatment agent
- silane surface
- silane
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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
-
- 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
- C23C2222/00—Aspects relating to chemical surface treatment of metallic material by reaction of the surface with a reactive medium
- C23C2222/20—Use of solutions containing silanes
Abstract
A kind of silane surface treatment agent, by percentage to the quality, be made up of following raw material: fluorine zirconic acid 2-5%, hydrofluotitanic acid 2-5%, silane coupling agent 0.3-0.6%, basic zirconium chloride 0.8-1.5%, citric acid 0.5-1%, surplus is water.Silane surface treatment agent of the present invention can save sewage Solid state fermentation cost, saves former water consumption, can use by normal temperature, saves heating energy source, and can reduce maintenance cost, save human cost.
Description
Technical field
The present invention relates to metal conditioner field, in particular, relate to a kind of silane surface treatment agent and preparation method thereof.
Background technology
Along with the maturation of metal surface treatment process, traditional phosphate conversion and chromating process for treating surface because contaminate environment, easily to factors such as human body work the mischief gradually by the silanization treatment technical substitution of environmental protection and energy saving.Silanization treatment is for main component carries out surface-treated process to metal or non-metallic material with the organosilane aqueous solution.Silanization treatment has following multiple advantage compared with conventional phosphatizing: without harmful heavy metal ions, not phosphorous, without the need to heating.Silane treatment process does not produce sediment, and the treatment time is short, controls easy.Treatment step is few, and can save table and adjust operation, tank liquor is reusable.The sticking power of effective raising paint to base material.Can the multiple base material such as collineation processing iron plate, galvanized sheet, aluminium sheet.But the film forming properties of the dependence silane that present silanization treatment is mostly just simple, makes the rete that the surface of workpiece of solution of silane process is formed, Density inhomogeneity, have cavity, split sunken, and the sticking power of metallic object not strong.
Chinese patent CN103254782A discloses silane place, a kind of corrosion resistant metallic surface
Reason agent, it is by the formulated mixed solution of following component, and in often liter of mixed solution, the weight part (gram) of each component is: N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane 60-65, tolyltriazole 1-2, ethylene glycol 6-8, succinate sodium 2-ethylhexyl 3-4, ammonium chloride 2-3, ammonium fluozirconate 1-2, film coalescence aid 2-4, remaining for water; The corrosion resistant Metal surface silane treatment agent treating processes that this patent is produced does not produce sediment, and the treatment time is short, controls easy, without harmful heavy metal ions, safety and environmental protection, the silane coating formed with metallic surface has excellent corrosion resistance nature, extends the work-ing life of metal.But there is following shortcoming in this patent: N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane accounting in formula composition is heavy excessive, and certainly will cause the high cost of product, cause the market competitiveness to decline, CSAT declines.
Chinese patent CN103254783A discloses a kind of aqueous surface-treating agent, it is by the formulated mixed solution of following component, in often liter of mixed solution, the weight part (gram) of each component is: aminopropyltriethoxywerene werene 30-40, N-phenyl-3-TSL 8330 10-20, ammonium fluozirconate 1-2, Natvosol 2-4, sodium monoflurophosphate 2-3,1,4 cyclohexane dimethanol 6-8, film coalescence aid 2-4, remaining for water; This aqueous surface-treating agent treating processes does not produce sediment, and treatment time section controls easy, and without harmful heavy metal ions, safety and environmental protection, the silane coating formed with metallic surface has excellent corrosion resistance nature, extends the work-ing life of metal.But there is following shortcoming in this patent: aminopropyltriethoxywerene werene and N-phenyl-3-TSL 8330 accounting in formula composition is heavy excessive, and certainly will cause the high cost of product, cause the market competitiveness to decline, CSAT declines.
Chinese patent CN103409762A discloses a kind of metal detergent and preparation method thereof.By the raw material of following parts by weight; Sodium dodecylbenzene sulfonate 8-10 part, sodium bicarbonate 2-6 part, magnesiumcarbonate 10-12 part, tertiary sodium phosphate 4-6 part, basic zirconium chloride 2-9 part, butyl stearate 5-10 part, propylene glycol 10-15 part, oxyethane 20-22 part, zinc peroxide 10-20 part, water 30-40 part.This metal detergent can remove the dirt that metallic surface etc. is difficult to remove easily, exposes in atmosphere, can keep 30 days non-corrosives, and cost is low after metal cleaning.But this patent exists following shortcoming: (1) this metal detergent is basic solution, thus can not form compact film on processed workpiece surface, can only form antirust moisture film, after washing step, workpiece must return rust.(2) in formula, magnesiumcarbonate solubleness in water is minimum, affects result of use.
Summary of the invention
An object of the present invention is to overcome the deficiencies in the prior art, provides a kind of silane surface treatment agent, and the agent of this silane surface treatment can save sewage Solid state fermentation cost, save former water consumption, can normal temperature phosphating, save heating energy source, and can maintenance cost be reduced, save human cost.
Two of object of the present invention is the preparation method providing above-mentioned silane surface treatment agent.
For achieving the above object, the technical solution used in the present invention is as follows:
A kind of silane surface treatment agent, by percentage to the quality, be made up of following raw material:
Fluorine zirconic acid 2-5%, hydrofluotitanic acid 2-5%, silane coupling agent 0.3-0.6%, basic zirconium chloride 0.8-1.5%, citric acid 0.5-1%, surplus is water.
The preferred 3-5% of consumption of described fluorine zirconic acid, the preferred 2-3% of consumption of hydrofluotitanic acid.
Described silane coupling agent preferred γ-glycidyl ether oxygen propyl trimethoxy silicane (KH-560) consumption is excessive, can cause high cost, and the competitive power of product declines; Consumption is too small, can affect forming silane film speed and quality, therefore the preferred 0.5-0.6% of its consumption.
The preferred 0.9-1.1% of consumption of described basic zirconium chloride.
The preferred 0.6-0.7% of consumption of described citric acid.
The preparation method of silane surface treatment agent of the present invention in turn includes the following steps:
(1) in reactor, water is added;
(2) add silane coupling agent in a kettle., stir, until silane coupling agent complete hydrolysis;
(3) in reactor, add fluorine zirconic acid and hydrofluotitanic acid, stir and solution is clarified;
(4) in reactor, add basic zirconium chloride, stir and solution is clarified;
(5) in reactor, add citric acid, stir and solution is clarified.
Churning time wherein in step (2) is 7-9 hour; Churning time in step (3) is 0.5-1.5 hour; Churning time in step (4) is 0.5-1.5 hour; Churning time in step (5) is 20-40 minute.
The using method of silane surface treatment agent of the present invention is (to prepare lm
3for example):
(1) groove data are joined
Groove joined by the available tap water of silane surface treatment agent, and as conditions permit, suggestion pure water joins groove, can extend tank liquor work-ing life.
Every 1000 liters of cell bodies are long-pending to be added
1. silane surface treatment agent 50kg, and stir.
2. then add ammoniacal liquor 9kg, and stir.
Note: want slowly when ammoniacal liquor adds, can add several times, the change of pH value monitored in real time by the most handy pH meter.
(2) treatment condition
Concentration 8.0 ~ 14.0PH3.5 ~ 4.5
Temperature 5 ~ 40 DEG C
0.5 ~ 3.0 minute time
(3) tank liquor management
Along with the carrying out of streamline processing treatment, concentration, the pH value of tank liquor all can change.So want regularly to measure concentration, pH value, ensure to maintain in the variation range of regulation.
Concentration: add silane surface treatment agent 4kg in every 1000 liters of tank liquors, concentration rises 1 point.Often process 1000 squares of workpiece, about need to add 7-8kg.
PH value: the factor that take into account the significantly dynamic variation preventing pH value in operation during the exploitation of this medicament.If need to improve pH value, can by adding ammoniacal liquor to regulate (pH value when say above treatment condition scope near, add ammoniacal liquor 9g in every 1000 liters of tank liquors, pH value probably rises 0.1).Same, pH value be reduced, can by adding fluorine zirconic acid to regulate (add fluorine zirconic acid 8g in every 1000 liters of tank liquors, can probably reduce pH value 0.1).
(4) detection method
Concentration detection method:
Get 10ml tank liquor, be placed in triangular flask, add the buffered soln that 20mlpH is 1.4, then add the 5ml5% oxammonium hydrochloride aqueous solution, finally add a small amount of xylenol orange indicator.Then be heated to about 80 DEG C, drop to red disappearance with the EDTA solution of 1mmol/L, becoming glassy yellow is terminal, the milliliter number of the EDTA solution of consumption and the concentration of silane surface treatment agent.
The collocation method of pH=1.4 buffered soln; Solution preparation: measure 266mlc(HCL)=0.2mol/L solution and 250mlc(KCL)=0.2mol/L solution is in 1000ml volumetric flask, and adding distil water is diluted to scale, shakes up.
(5) detection method of pH value
1. before the assay, the damping fluid of PH meter PH4.01 and PH6.86 corrects.
2. treatment solution polythene container sampling (50 ~ 100mL).
3. the glass electrode that PH counts is immersed treatment solution, after 2 minutes, read pH value.
4. after PH measurement terminates, from treatment solution, take out glass electrode, horse back washed with de-ionized water after taking out, and put into the container that deionized water is housed and carry out keeping.
Main operational principle of the present invention is as follows:
-Si-OH group in silane hydrolysates and metallic surface Me-OH group form hydrogen bond, and quick adsorption is in metallic surface.
（RO）
3—Si—R‵﹢3H
2O→（OH）
3—Si—R‵﹢3ROH
In drying process ,-Si-OH group and Me-OH group condense further, and interface generates Si-O-Me covalent linkage.
-Si-OH(solution) ﹢ Me-OH(metallic surface) → Si-O-Me ﹢ H
2o
The aggregation that remaining silane molecule then passes through between-Si-OH group forms the organic membrane with Si-O-Si tridimensional network on the metal surface, 3HO-Si-R ‵ → R ‵ (OH)
2si-O-Si(OH)
2r ‵ ﹢ H2O.
The organic membrane of Si-O-Si tridimensional network has good closed performance, stops matrix by atomospheric corrosion, simultaneously the organic membrane of Si-O-Si tridimensional network and the matching capacity of enamelled coating splendid.
The beneficial effect of silane surface treatment agent of the present invention is as follows: (1) ecological dominance: without phosphorus, and without BOD/COD, heavy metal free, reduces by the quantity of slag of more than 90%, and slag toxicological harmless, reduce the discharge of wastewater of more than 90%; (2) process advantage: less operation, is in harmonious proportion without the need to table and closes, be applicable to zinc, aluminium, the various sheet material such as iron, can be supporting with various high temperature varnish, and controling parameters is less, and regulation range is wider, and film forming speed is fast, increase yield; (3) economic advantages: save sewage Solid state fermentation cost, save former water consumption, normal temperature uses, and saves heating energy source, reduces maintenance cost, saves human cost.
Embodiment
Embodiment 1
The agent of every 1000Kg silane surface treatment, be made up of following raw material:
Fluorine zirconic acid 20Kg, hydrofluotitanic acid 20Kg, silane coupling agent (KH-560) 3Kg, basic zirconium chloride 8Kg, citric acid 5Kg, water 944Kg.
Its preparation method in turn includes the following steps:
(1) in reactor, water is added;
(2) add silane coupling agent in a kettle., stir, until silane coupling agent complete hydrolysis, churning time is 7-9 hour;
(3) in reactor, add fluorine zirconic acid and hydrofluotitanic acid, stir and solution is clarified, churning time is 0.5-1.5 hour;
(4) in reactor, add basic zirconium chloride, stir and solution is clarified, churning time is 0.5-1.5 hour;
(5) in reactor, add citric acid, stir and solution is clarified, churning time is 20-40 minute.
(6) product is carried out physical and chemical index detection, packaging warehouse-in.
Embodiment 2
The agent of every 1000Kg silane surface treatment, be made up of following raw material:
Fluorine zirconic acid 20Kg, hydrofluotitanic acid 50Kg, silane coupling agent (KH-560) 3Kg, basic zirconium chloride 8Kg, citric acid 5Kg, water 914Kg.
Preparation method is with embodiment 1.
Embodiment 3
The agent of every 1000Kg silane surface treatment, be made up of following raw material:
Fluorine zirconic acid 40Kg, hydrofluotitanic acid 30Kg, silane coupling agent (KH-560) 5Kg, basic zirconium chloride 10Kg, citric acid 7Kg, water 908Kg.
Preparation method is with embodiment 1.
Embodiment 4
The agent of every 1000Kg silane surface treatment, be made up of following raw material:
Fluorine zirconic acid 30Kg, hydrofluotitanic acid 20Kg, silane coupling agent (KH-560) 4Kg, basic zirconium chloride 9Kg, citric acid 6Kg, water 931Kg.
Preparation method is with embodiment 1.
Embodiment 5
The agent of every 1000Kg silane surface treatment, be made up of following raw material:
Fluorine zirconic acid 50Kg, hydrofluotitanic acid 30Kg, silane coupling agent (KH-560) 6Kg, basic zirconium chloride 10Kg, citric acid 7Kg, water 897Kg.
Preparation method is with embodiment 1.
Embodiment 6
The agent of every 1000Kg silane surface treatment, be made up of following raw material:
Fluorine zirconic acid 40Kg, hydrofluotitanic acid 20Kg, silane coupling agent (KH-560) 5Kg, basic zirconium chloride 10Kg, citric acid 8Kg, water 917Kg.
Preparation method is with embodiment 1.
Embodiment 7
The agent of every 1000Kg silane surface treatment, be made up of following raw material:
Fluorine zirconic acid 40Kg, hydrofluotitanic acid 25Kg, silane coupling agent (KH-560) 6Kg, basic zirconium chloride 11Kg, citric acid 9Kg, water 909Kg.
Preparation method and using method are with embodiment 1.
Embodiment 8
The agent of every 1000Kg silane surface treatment, be made up of following raw material:
Fluorine zirconic acid 35Kg, hydrofluotitanic acid 25Kg, silane coupling agent (KH-560) 5Kg, basic zirconium chloride 11Kg, citric acid 9Kg, water 915Kg.
Preparation method is with embodiment 1.
Embodiment 9
The agent of every 1000Kg silane surface treatment, be made up of following raw material:
Fluorine zirconic acid 35Kg, hydrofluotitanic acid 30Kg, silane coupling agent (KH-560) 5Kg, basic zirconium chloride 11Kg, citric acid 6Kg, water 913Kg.
Preparation method is with embodiment 1.
Embodiment 10
The agent of every 1000Kg silane surface treatment, be made up of following raw material:
Fluorine zirconic acid 45Kg, hydrofluotitanic acid 30Kg, silane coupling agent (KH-560) 6Kg, basic zirconium chloride 15Kg, citric acid 9Kg, water 895Kg.
Preparation method is with embodiment 1.
Embodiment 11
The agent of every 1000Kg silane surface treatment, be made up of following raw material:
Fluorine zirconic acid 45Kg, hydrofluotitanic acid 30Kg, silane coupling agent (KH-560) 5Kg, basic zirconium chloride 15Kg, citric acid 9Kg, water 896Kg.
Preparation method is with embodiment 1.
The formula of embodiment of the present invention 1-11 calculates with the agent of 1000Kg silane surface treatment in table 1, table 2(respectively).
The formula of table 1 embodiment 1-6
The formula of table 2 embodiment 7-11
The result of use of embodiment of the present invention 1-11 is in table 3, table 4.
The result of use of table 3 embodiment 1-6
The result of use of table 4 embodiment 7-11
Consolidated statement 3 table 4 can be found out, the effect of embodiment 9 is carried out, and after its coating, the neutral salt spray test time reaches 1000h.Relative to conventional phosphatizing liquid technique (phosphating time 7-15min, phosphatization temperature 30-60 DEG C, phosphatize phosphate coat thickness 3-10 micron, neutral salt spray test time 800h, paint film adhesion grade 0 grade, sediment 2-5g/ ㎡, table is needed to adjust operation, cost of sewage disposal is high, is rich in heavy metal ion and phosphoric acid salt), silane surface treatment technique can substitute completely.
In table 3, comparative run object testing method is as follows:
Silane film thickness: measure method of magnetic according to non-magnetic capping layer cover thickness in GB4956-2003T magnetic matrix and test;
Neutral salt spray test after coating: test according to GB10125-1997 artificial atmosphere corrosion test salt-fog test standard;
Paint film adhesion grade: the cross cut test standard according to GB9286-1998 paint and varnish paint film is tested;
Paint film impact resistance: test according to the shock-resistant assay method of GB1732-1993 paint film.
Above content description ultimate principle of the present invention and principal character; the present invention is not restricted to the described embodiments; what describe in above-described embodiment and specification sheets just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.Application claims protection domain is defined by appending claims and equivalent thereof.
Claims (9)
1. a silane surface treatment agent, is characterized in that by percentage to the quality, is made up of following raw material: fluorine zirconic acid 2-5%, hydrofluotitanic acid 2-5%, γ-glycidyl ether oxygen propyl trimethoxy silicane 0.3-0.6%, basic zirconium chloride 0.8-1.5%, citric acid 0.5-1%, surplus is water.
2. silane surface treatment agent according to claim 1, is characterized in that the consumption of fluorine zirconic acid is 3-5%.
3. silane surface treatment agent according to claim 1, is characterized in that the consumption of hydrofluotitanic acid is 2-3%.
4. silane surface treatment agent according to claim 1, is characterized in that the consumption of described γ-glycidyl ether oxygen propyl trimethoxy silicane is 0.5-0.6%.
5. silane surface treatment agent according to claim 1, is characterized in that the consumption of described basic zirconium chloride is 0.9-1.1%.
6. silane surface treatment agent according to claim 1, is characterized in that the consumption of described citric acid is 0.6-0.7%.
7. silane surface treatment agent according to claim 1, is characterized in that, by percentage to the quality, be made up of following raw material: fluorine zirconic acid 3.5%, hydrofluotitanic acid 3%, γ-glycidyl ether oxygen propyl trimethoxy silicane 0.5%, basic zirconium chloride 1.1%, citric acid 0.6%, water 91.3%.
8. the preparation method of silane surface treatment agent according to claim 1, is characterized in that in turn including the following steps:
(1) in reactor, water is added;
(2) add γ-glycidyl ether oxygen propyl trimethoxy silicane in a kettle., stir, until γ-glycidyl ether oxygen propyl trimethoxy silicane complete hydrolysis;
(3) in reactor, add fluorine zirconic acid and hydrofluotitanic acid, stir and solution is clarified;
(4) in reactor, add basic zirconium chloride, stir and solution is clarified;
(5) in reactor, add citric acid, stir and solution is clarified.
9. the preparation method of silane surface treatment agent according to claim 8, is characterized in that: the churning time in step (2) is 7-9 hour; Churning time in step (3) is 0.5-1.5 hour; Churning time in step (4) is 0.5-1.5 hour; Churning time in step (5) is 20-40 minute.
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| FR3097880A1 (en) * | 2019-06-27 | 2021-01-01 | Socomore | COMPOSITION FOR THE SURFACE TREATMENT OF A METAL SUBSTRATE AND SURFACE TREATMENT PROCESS IMPLEMENTING SUCH COMPOSITION |
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| CN104099008A (en) * | 2014-06-19 | 2014-10-15 | 锐展(铜陵)科技有限公司 | Anti-grease aluminium alloy surface treatment agent |
| CN106702360A (en) * | 2016-04-16 | 2017-05-24 | 佛山瑞箭体育器材有限公司 | Environment-friendly surface treatment agent and preparation method thereof |
| CN113755097B (en) * | 2021-09-15 | 2022-05-31 | 湖南工程学院 | Surface treating agent for slowing down rust liquid sagging of weathering resistant steel at initial service stage as well as preparation method and use method thereof |
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