CN103773234A - Silane surface treating agent and preparation method thereof - Google Patents
Silane surface treating agent and preparation method thereof Download PDFInfo
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- CN103773234A CN103773234A CN201410011960.8A CN201410011960A CN103773234A CN 103773234 A CN103773234 A CN 103773234A CN 201410011960 A CN201410011960 A CN 201410011960A CN 103773234 A CN103773234 A CN 103773234A
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- surface treatment
- 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
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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
- 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
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- Chemical Kinetics & Catalysis (AREA)
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Abstract
The invention discloses a silane surface treating agent, which is prepared from the following raw materials by mass percent: 2-5% of hexafluorozirconic acid, 2-5% of hexafluorotitanic acid, 0.3-0.6% of silane coupling agent, 0.8-1.5% of zirconium oxychloride, 0.5-1% of citric acid and the balance of water. By adopting the silane surface treating agent disclosed by the invention, the sewage sludge treatment cost can be saved, consumption of raw water is saved, the silane surface treating agent can be used at normal temperature, a heating energy source is saved, the maintenance cost can be reduced, and the manpower cost is saved.
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 are because contaminate environment, easily substituted by the silanization treatment technology of environmental protection and energy saving gradually factors such as human body work the mischief.Silanization processing is, take the organosilane aqueous solution as main component, metal or non-metallic material are carried out to surface-treated process.Silanization is processed has following multiple advantage compared with conventional phosphatizing: without harmful heavy metal ion, not phosphorous, and without heating.Silane treatment process does not produce sediment, and the treatment time is short, controls easy.Treatment step is few, can save table and adjust operation, and tank liquor is reusable.Effectively improve the sticking power of paint to base material.Can collineation processing iron plate, the multiple base material such as galvanized sheet, aluminium sheet.But it is the film forming properties of simple dependence silane mostly that present silanization is processed, make the rete of the surface of workpiece formation that solution of silane processed, Density inhomogeneity, have cavity, split sunken, and the sticking power of metallic object not strong.
Chinese patent CN 103254782A discloses silane place, a kind of corrosion resistant metallic surface
Reason agent, it is the mixed solution formulated by following component, the weight part of each component in every liter of mixed solution (gram) be: N-(β-aminoethyl)-γ-aminopropyl trimethoxysilane 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 be water; The corrosion resistant metallic surface silane finish treating processes that this patent is produced does not produce sediment, and the treatment time is short, controls easy, without harmful heavy metal ion, safety and environmental protection, the silane coating forming with metallic surface has excellent corrosion resistance nature, has extended the work-ing life of metal.But this patent exists following shortcoming: N-(β-aminoethyl)-γ-aminopropyl trimethoxysilane accounting in formula composition heavy excessive, certainly will cause the high cost of product, cause the market competitiveness to decline, CSAT declines.
Chinese patent CN 103254783A discloses a kind of aqueous surface-treating agent, it is the mixed solution formulated by following component, the weight part of each component in every liter of mixed solution (gram) be: aminopropyltriethoxywerene werene 30-40, N-phenyl-3-TSL 8330 10-20, ammonium fluozirconate 1-2, Natvosol 2-4, sodium monoflurophosphate 2-3, Isosorbide-5-Nitrae-cyclohexanedimethanol 6-8, film coalescence aid 2-4, remaining be water; This aqueous surface-treating agent treating processes does not produce sediment, treatment time section, control easy, without harmful heavy metal ion, safety and environmental protection, with metallic surface form silane coating there is excellent corrosion resistance nature, extended 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, certainly will cause the high cost of product, causes the market competitiveness to decline, and CSAT declines.
Chinese patent CN103409762A discloses a kind of metal detergent and preparation method thereof.By the raw material of following weight part meter; 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 be removed easily metallic surface etc. and be difficult to the dirt of removing, and metal is exposed in air after cleaning, and can keep 30 days non-corrosives, and cost is low.But there is following shortcoming in this patent: (1) this metal detergent is basic solution, thereby can not form compact film on processed workpiece surface, can only form antirust moisture film, and after washing step, workpiece must return rust.(2) in formula, magnesiumcarbonate solubleness in water is minimum, affects result of use.
Summary of the invention
One of object of the present invention is to overcome the deficiencies in the prior art, and a kind of silane surface treatment agent is provided, and the agent of this silane surface treatment can be saved sewage waste residue processing cost, save former water consumption, can normal temperature phosphating, save heating energy source, and can reduce maintenance cost, save human cost.
Two of object of the present invention is to provide the preparation method of 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, made by 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.
Preferred γ-the glycidyl ether oxygen propyl trimethoxy silicane of described silane coupling agent (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, add water;
(2) in reactor, add silane coupling agent, stir, until silane coupling agent complete hydrolysis;
(3) in reactor, add fluorine zirconic acid and hydrofluotitanic acid, stir and make solution clarification;
(4) in reactor, add basic zirconium chloride, stir and make solution clarification;
(5) in reactor, add citric acid, stir and make solution clarification.
Wherein 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.
The using method of silane surface treatment agent of the present invention is (to prepare lm
3for example):
(1) join groove data
The available tap water of silane surface treatment agent is joined groove, and as conditions permit, suggestion is joined groove with pure water, 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 when ammoniacal liquor adds slowly, can add several times, the most handy pH meter is monitored the variation of pH value in real time.
(2) treatment condition
Concentration 8.0～14.0 PH 3.5～4.5
5～40 ℃ of temperature
0.5～3.0 minute time
(3) tank liquor management
Along with the carrying out of streamline processing treatment, the concentration of tank liquor, pH value all can change.So will regularly measure concentration, pH value, guarantee to maintain in the variation range of regulation.
Concentration: add silane surface treatment agent 4kg in every 1000 liters of tank liquors, 1 point of concentration rising.1000 squares of workpiece of every processing, approximately need to add 7-8kg.
PH value: considered the significantly factor of moving variation that prevents pH value in operation when this medicament exploitation.If need to improve pH value, can by add ammoniacal liquor regulate (pH value say above treatment condition scope near situation under, in every 1000 liters of tank liquors, add ammoniacal liquor 9g, pH value probably rises 0.1).Same, reduce pH value, can be 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, adding 20ml pH is 1.4 buffered soln, then adds the 5ml 5% oxammonium hydrochloride aqueous solution, finally adds a small amount of xylenol orange indicator.Then be heated to 80 ℃ of left and right, drop to redness disappear with the EDTA solution of 1m mol/L, becoming glassy yellow is terminal, and a milliliter number for the EDTA solution of consumption is the concentration of silane surface treatment agent.
The collocation method of pH=1.4 buffered soln; Solution preparation: measure 266ml c(HCL)=0.2mol/L solution and 250ml c(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 mensuration, PH meter is proofreaied and correct with the damping fluid of PH4.01 and PH6.86.
2. polythene container sampling (50～100mL) for treatment solution.
3. the glass electrode of PH meter is immersed to treatment solution, after 2 minutes, read pH value.
4., after PH measurement finishes, 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 take care of.
Groundwork principle of the present invention is as follows:
In silane hydrolyzate product-Si-OH group and metallic surface Me-OH group formation hydrogen bond, 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 further condense, and generate Si-O-Me covalent linkage on interface.
-Si-OH(solution) ﹢ Me-OH(metallic surface) → Si-O-Me ﹢ H
2o
Aggregation between pass through-Si-OH of remaining silane molecule group forms the organic membrane with Si-O-Si tridimensional network on metallic 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, and the organic membrane of Si-O-Si tridimensional network and the matching capacity of enamelled coating are splendid simultaneously.
The beneficial effect of silane surface treatment agent of the present invention is as follows: (1) ecological dominance: without phosphorus, without BOD/COD, heavy metal free, reduces more than 90% quantity of slag, and slag toxicological harmless, reduces more than 90% discharge of wastewater; (2) process advantage: operation still less, be in harmonious proportion and seal without table, be applicable to zinc, aluminium, the various sheet material such as iron, can be supporting with various high temperature varnishs, controls parameter still less, and regulation range is wider, and film forming speed is fast, increases output; (3) economic advantages: save sewage waste residue processing 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, made by following raw material:
Fluorine zirconic acid 20Kg, hydrofluotitanic acid 20 Kg, silane coupling agent (KH-560) 3 Kg, basic zirconium chloride 8 Kg, citric acid 5 Kg, water 944 Kg.
Its preparation method in turn includes the following steps:
(1) in reactor, add water;
(2) in reactor, add silane coupling agent, 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 make solution clarification, churning time is 0.5-1.5 hour;
(4) in reactor, add basic zirconium chloride, stir and make solution clarification, churning time is 0.5-1.5 hour;
(5) in reactor, add citric acid, stir and make solution clarification, churning time is 20-40 minute.
(6) product is carried out to physical and chemical index detection, packing warehouse-in.
Embodiment 2
The agent of every 1000Kg silane surface treatment, made by following raw material:
Fluorine zirconic acid 20Kg, hydrofluotitanic acid 50 Kg, silane coupling agent (KH-560) 3 Kg, basic zirconium chloride 8 Kg, citric acid 5 Kg, water 914 Kg.
Preparation method is with embodiment 1.
Embodiment 3
The agent of every 1000Kg silane surface treatment, made by following raw material:
Fluorine zirconic acid 40Kg, hydrofluotitanic acid 30 Kg, silane coupling agent (KH-560) 5 Kg, basic zirconium chloride 10 Kg, citric acid 7Kg, water 908 Kg.
Preparation method is with embodiment 1.
Embodiment 4
The agent of every 1000Kg silane surface treatment, made by following raw material:
Fluorine zirconic acid 30Kg, hydrofluotitanic acid 20 Kg, silane coupling agent (KH-560) 4 Kg, basic zirconium chloride 9 Kg, citric acid 6 Kg, water 931 Kg.
Preparation method is with embodiment 1.
Embodiment 5
The agent of every 1000Kg silane surface treatment, made by following raw material:
Fluorine zirconic acid 50Kg, hydrofluotitanic acid 30 Kg, silane coupling agent (KH-560) 6 Kg, basic zirconium chloride 10 Kg, citric acid 7 Kg, water 897 Kg.
Preparation method is with embodiment 1.
Embodiment 6
The agent of every 1000Kg silane surface treatment, made by following raw material:
Fluorine zirconic acid 40Kg, hydrofluotitanic acid 20 Kg, silane coupling agent (KH-560) 5 Kg, basic zirconium chloride 10 Kg, citric acid 8 Kg, water 917Kg.
Preparation method is with embodiment 1.
Embodiment 7
The agent of every 1000Kg silane surface treatment, made by following raw material:
Fluorine zirconic acid 40Kg, hydrofluotitanic acid 25 Kg, silane coupling agent (KH-560) 6Kg, basic zirconium chloride 11 Kg, citric acid 9Kg, water 909Kg.
Preparation method and using method are with embodiment 1.
Embodiment 8
The agent of every 1000Kg silane surface treatment, made by following raw material:
Fluorine zirconic acid 35Kg, hydrofluotitanic acid 25 Kg, silane coupling agent (KH-560) 5Kg, basic zirconium chloride 11 Kg, citric acid 9Kg, water 915Kg.
Preparation method is with embodiment 1.
Embodiment 9
The agent of every 1000Kg silane surface treatment, made by following raw material:
Fluorine zirconic acid 35Kg, hydrofluotitanic acid 30 Kg, silane coupling agent (KH-560) 5Kg, basic zirconium chloride 11 Kg, citric acid 6Kg, water 913Kg.
Preparation method is with embodiment 1.
Embodiment 10
The agent of every 1000Kg silane surface treatment, made by following raw material:
Fluorine zirconic acid 45Kg, hydrofluotitanic acid 30 Kg, silane coupling agent (KH-560) 6Kg, basic zirconium chloride 15 Kg, citric acid 9Kg, water 895Kg.
Preparation method is with embodiment 1.
Embodiment 11
The agent of every 1000Kg silane surface treatment, made by following raw material:
Fluorine zirconic acid 45Kg, hydrofluotitanic acid 30 Kg, silane coupling agent (KH-560) 5Kg, basic zirconium chloride 15 Kg, 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 tables 4 can find out, the effect of embodiment 9 is carried out, its apply after the neutral salt spray test time reach 1000h.With respect to conventional phosphatizing liquid technique (phosphating time 7-15min, phosphatization temperature 30-60 ℃, phosphatize phosphate coat thickness 3-10 micron, neutral salt spray test time 800h, 0 grade of paint film adhesion grade, sediment 2-5g/ ㎡, need table 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 tectum cover thickness in GB 4956-2003T magnetic matrix and test;
Neutral salt spray test after applying: test according to GB 10125-1997 artificial atmosphere corrosion test salt-fog test standard;
Paint film adhesion grade: test according to the cross cut test standard of GB 9286-1998 paint and varnish paint film;
Paint film impact resistance: test according to the shock-resistant assay method of GB 1732-1993 paint film.
Above content description ultimate principle of the present invention and principal character; the present invention is not restricted to the described embodiments; that in above-described embodiment and specification sheets, describes 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.The claimed scope of the present invention is defined by appending claims and equivalent thereof.
Claims (10)
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%, and 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.
2. silane surface treatment agent according to claim 1, the consumption that it is characterized in that fluorine zirconic acid is 3-5%.
3. silane surface treatment agent according to claim 1, the consumption that it is characterized in that hydrofluotitanic acid is 2-3%.
4. silane surface treatment agent according to claim 1, is characterized in that described silane coupling agent is γ-glycidyl ether oxygen propyl trimethoxy silicane.
5. silane surface treatment agent according to claim 4, the consumption that it is characterized in that described γ-glycidyl ether oxygen propyl trimethoxy silicane is 0.5-0.6%.
6. silane surface treatment agent according to claim 4, the consumption that it is characterized in that described basic zirconium chloride is 0.9-1.1%.
7. silane surface treatment agent according to claim 4, the consumption that it is characterized in that described citric acid is 0.6-0.7%.
8. silane surface treatment agent according to claim 4, is characterized in that, by percentage to the quality, made by 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%.
9. 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, add water;
(2) in reactor, add silane coupling agent, stir, until silane coupling agent complete hydrolysis;
(3) in reactor, add fluorine zirconic acid and hydrofluotitanic acid, stir and make solution clarification;
(4) in reactor, add basic zirconium chloride, stir and make solution clarification;
(5) in reactor, add citric acid, stir and make solution clarification.
10. the preparation method of silane surface treatment agent according to claim 9, 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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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN113755097A (en) * | 2021-09-15 | 2021-12-07 | 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 |
| CN115074028A (en) * | 2022-06-02 | 2022-09-20 | 西安焦视医疗器械有限责任公司 | Metal 3D printing mirror bracket paint film adhesion enhancing accelerant, preparation method and post-treatment process |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| FR3097880B1 (en) * | 2019-06-27 | 2021-12-31 | Socomore | COMPOSITION FOR THE SURFACE TREATMENT OF A METALLIC SUBSTRATE AND SURFACE TREATMENT METHOD USING SUCH A COMPOSITION |
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| CN115074028A (en) * | 2022-06-02 | 2022-09-20 | 西安焦视医疗器械有限责任公司 | Metal 3D printing mirror bracket paint film adhesion enhancing accelerant, preparation method and post-treatment process |
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