CN108165972A - A kind of preparation method of anti-corrosion silane surface treatment agent - Google Patents
A kind of preparation method of anti-corrosion silane surface treatment agent Download PDFInfo
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- CN108165972A CN108165972A CN201711279037.2A CN201711279037A CN108165972A CN 108165972 A CN108165972 A CN 108165972A CN 201711279037 A CN201711279037 A CN 201711279037A CN 108165972 A CN108165972 A CN 108165972A
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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
- C23C22/60—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 alkaline aqueous solutions with pH greater than 8
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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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- Preventing Corrosion Or Incrustation Of Metals (AREA)
Abstract
The invention discloses a kind of preparation methods of anti-corrosion silane surface treatment agent, the present invention handles three ammonium molybdates using silane coupling agent, non-rusting solution is handled using the alcoholic solution of tetramethyl disiloxane, is mixed with dodecenylsuccinic acid, effectively raises the rust-resisting property of finished product.
Description
Technical field
The invention belongs to Material Fields, and in particular to a kind of preparation method of anti-corrosion silane surface treatment agent.
Background technology
In field of metal surface treatment, although traditional phosphate conversion and chromating process for treating surface can obtain
Good effect is obtained, but there are larger defects for both the above processing method：Environment compatibility difference and use cost are high.Environment is endangered
Evil：Phosphatization uses nitrite containing heavy metal ion such as zinc, manganese, nickel and containing a large amount of phosphorus in the process of production and application
Accelerating agent is done, is serious carcinogen.
Silane finish does not have compression properties in the prior art, this causes its volume big, and transport, storage are inconvenient.
Application number：201510577331.6 disclosing a kind of Metal surface silane treatment agent, include silane in parts by weight
20-30 parts of coupling agent, 20-30 parts of film forming agent, 5-7 parts of complexing agent, 15-30 parts of pure water, the film forming agent is thickener, described
Complexing agent is sodium citrate, make the present invention have high timeliness, hyperconcetration and with low-carbon energy-saving, without slag, it is without phosphorus, without zinc, nothing
Chromium, free-floride, without the more superior environmental-protecting performance such as zirconium, but traditional silane finish functionality is single, and viscosity is low, adhesive force
Difference.
Invention content
In view of the defects and deficiencies of the prior art, the present invention intends to provide a kind of anti-corrosion silane surface treatment agent
Preparation method.
To achieve the above object, the present invention uses following technical scheme：
A kind of preparation method of anti-corrosion silane surface treatment agent, includes the following steps：
(1) lanolin of 2-3 parts by weight is taken, is added in the deionized water of 20-30 times of its weight, stirs evenly, is added in
The azodicarbonamide of 0.1-0.2 parts by weight, is sent in 60-67 DEG C of water bath with thermostatic control, insulated and stirred 1-2 hours, and 7-9 is added dropwise
The sodium hydroxide of parts by weight, a concentration of 4-5mol/l, discharges after being added dropwise, stirs evenly, and obtains acyl amine aqueous solution；
(2) three ammonium molybdates of 4-6 parts by weight, the silane coupling agent kh560 mixing of 0.3-0.5 parts by weight are taken, is added to mixed
In the absolute ethyl alcohol for closing 1.6-2 times of weight of material, raising temperature is 50-60 DEG C, and insulated and stirred 2-3 hours obtains silanol solution；
(3) allyl polyglycol of 5-7 parts by weight is taken, insulated and stirred 16-20 minutes at 70-80 DEG C, adds in 3-4 weights
The tetramethyl disiloxane of part, the non-rusting solution of 20-30 parts by weight are measured, continues insulated and stirred 10-20 minutes, is added to above-mentioned silicon
It is 3-4 minutes ultrasonic in alkanol solution, obtain compound alcohol dispersion liquid；
(4) acrylic acid of 3-4 parts by weight is taken, is added in the deionized water of 14-20 times of its weight, stirs evenly, it is and upper
Compound alcohol dispersion liquid mixing is stated, is stirred evenly, is added in the platinum dioxide of 0.1-0.2 parts by weight, nitrogen is passed through, at 40-50 DEG C
Insulation reaction 10-15 hours, obtains cross-linked disperse liquid；
(5) above-mentioned acyl amine aqueous solution, the mixing of cross-linked disperse liquid are taken, stirs evenly, adds in the laurylene of 0.1-0.3 parts by weight
Base succinic acid, 1600-2000 revs/min is stirred 1-2 hours to get the anti-corrosion silane surface treatment agent.
A kind of preparation method of anti-corrosion silane surface treatment agent, the non-rusting solution are the raw material groups by following weight parts
Into：
N-Methyl pyrrolidone 17-20, sodium metasilicate 3-4, calcium acetylacetonate 0.5-1, trimethyl hydroxyethylammonium ethylenediamine 1-2,
Lanolin 4-6, zinc pyrithione 2-3；
The preparation method of the non-rusting solution, includes the following steps：
(1) calcium acetylacetonate is taken, is added in the absolute ethyl alcohol of 6-9 times of its weight, the insulated and stirred 10- at 60-70 DEG C
20 minutes；
(2) lanolin is taken, is added in the deionized water of 15-20 times of its weight, stirs evenly, with above-mentioned calcium acetylacetonate
Alcoholic solution mixing, stir evenly, be added dropwise ammonium hydroxide, adjustings pH be 10-11, be stirred to react 30-40 minutes, obtain wool lipoprotein solution；
(3) sodium metasilicate, zinc pyrithione mixing are taken, is added in above-mentioned wool lipoprotein solution, stirs evenly, add in N- methyl
Pyrrolidones, raising temperature are 75-80 DEG C, add in trimethyl hydroxyethylammonium ethylenediamine, ultrasonic 10-15 minutes to get the antirust
Solvent.
A concentration of 10-12% of the ammonium hydroxide.
Advantages of the present invention：
The present invention disperses in amide aqueous solution first using lanolin as raw material, acyl amine aqueous solution is obtained, then with regard to tetramethyl
Disiloxane is distributed in alcoholic solution, is mixed with acrylic acid, uses platinum dioxide as catalyst so that carbon present in acrylic acid
The C=O bond of carbon double bond and tetramethyl disiloxane could be formed with the conjugation of effect, so as to which plurality of raw materials effectively be disperseed,
Improve the uniform and stable property of product handling system agent；
The present invention handles three ammonium molybdates using silane coupling agent, and antirust is handled using the alcoholic solution of tetramethyl disiloxane
Solvent is mixed with dodecenylsuccinic acid, effectively raises the rust-resisting property of finished product.
Specific embodiment
Embodiment 1
A kind of preparation method of anti-corrosion silane surface treatment agent, includes the following steps：
(1) lanolin of 2 parts by weight is taken, is added in the deionized water of 20 times of its weight, stirs evenly, adds in 0.1 weight
The azodicarbonamide of part is measured, is sent in 60 DEG C of water bath with thermostatic control, insulated and stirred 1 hour, it is 7 parts by weight of dropwise addition, a concentration of
The sodium hydroxide of 4mol/l discharges after being added dropwise, stirs evenly, and obtains acyl amine aqueous solution；
(2) three ammonium molybdates of 4 parts by weight, the silane coupling agent kh560 mixing of 0.3 parts by weight are taken, is added to mixture weight
In the absolute ethyl alcohol of 1.6 times of amount, raising temperature is 50 DEG C, and insulated and stirred 2 hours obtains silanol solution；
(3) allyl polyglycol of 5 parts by weight is taken, insulated and stirred 20 minutes at 80 DEG C, the tetramethyl of 3 parts by weight of addition
The non-rusting solution of base disiloxane, 30 parts by weight, continues insulated and stirred 20 minutes, is added in above-mentioned silanol solution, ultrasound 4
Minute, obtain compound alcohol dispersion liquid；
(4) acrylic acid of 4 parts by weight is taken, is added in the deionized water of 20 times of its weight, stirs evenly, it is and above-mentioned compound
Alcohol dispersion liquid mixes, and stirs evenly, and adds in the platinum dioxide of 0.2 parts by weight, is passed through nitrogen, insulation reaction 15 is small at 50 DEG C
When, obtain cross-linked disperse liquid；
(5) above-mentioned acyl amine aqueous solution, the mixing of cross-linked disperse liquid are taken, stirs evenly, adds in the laurylene base fourth of 0.3 parts by weight
Diacid, 2000 revs/min are stirred 2 hours to get the anti-corrosion silane surface treatment agent.
A kind of preparation method of anti-corrosion silane surface treatment agent, the non-rusting solution are the raw material groups by following weight parts
Into：
N-Methyl pyrrolidone 17, sodium metasilicate 3, calcium acetylacetonate 0.5, trimethyl hydroxyethylammonium ethylenediamine 1, lanolin 4, pyrrole
Pyridine thioketones zinc 2；
The preparation method of the non-rusting solution, includes the following steps：
(1) calcium acetylacetonate is taken, is added in the absolute ethyl alcohol of 6 times of its weight, insulated and stirred 10 minutes at 60 DEG C；
(2) lanolin is taken, is added in the deionized water of 15-20 times of its weight, stirs evenly, with above-mentioned calcium acetylacetonate
Alcoholic solution mixing, stir evenly, be added dropwise ammonium hydroxide, adjust pH be 10, be stirred to react 30 minutes, obtain wool lipoprotein solution；
(3) sodium metasilicate, zinc pyrithione mixing are taken, is added in above-mentioned wool lipoprotein solution, stirs evenly, add in N- methyl
Pyrrolidones, raising temperature are 75 DEG C, add in trimethyl hydroxyethylammonium ethylenediamine, ultrasonic 10 minutes to get the non-rusting solution.
Embodiment 2
A kind of preparation method of anti-corrosion silane surface treatment agent, includes the following steps：
(1) lanolin of 3 parts by weight is taken, is added in the deionized water of 30 times of its weight, stirs evenly, adds in 0.2 weight
The azodicarbonamide of part is measured, is sent in 67 DEG C of water bath with thermostatic control, insulated and stirred 2 hours, it is 9 parts by weight of dropwise addition, a concentration of
The sodium hydroxide of 5mol/l discharges after being added dropwise, stirs evenly, and obtains acyl amine aqueous solution；
(2) three ammonium molybdates of 6 parts by weight, the silane coupling agent kh560 mixing of 0.5 parts by weight are taken, is added to mixture weight
In the absolute ethyl alcohol of 2 times of amount, raising temperature is 60 DEG C, and insulated and stirred 23 hours obtains silanol solution；
(3) allyl polyglycol of 7 parts by weight is taken, insulated and stirred 20 minutes at 80 DEG C, the tetramethyl of 4 parts by weight of addition
The non-rusting solution of base disiloxane, 30 parts by weight, continues insulated and stirred 20 minutes, is added in above-mentioned silanol solution, ultrasound 4
Minute, obtain compound alcohol dispersion liquid；
(4) acrylic acid of 4 parts by weight is taken, is added in the deionized water of 20 times of its weight, stirs evenly, it is and above-mentioned compound
Alcohol dispersion liquid mixes, and stirs evenly, and adds in the platinum dioxide of 0.2 parts by weight, is passed through nitrogen, insulation reaction 15 is small at 50 DEG C
When, obtain cross-linked disperse liquid；
(5) above-mentioned acyl amine aqueous solution, the mixing of cross-linked disperse liquid are taken, stirs evenly, adds in the laurylene base fourth of 0.3 parts by weight
Diacid, 2000 revs/min are stirred 2 hours to get the anti-corrosion silane surface treatment agent.
The non-rusting solution is made of the raw material of following weight parts：
N-Methyl pyrrolidone 20, sodium metasilicate 4, calcium acetylacetonate 1, trimethyl hydroxyethylammonium ethylenediamine 2, lanolin 6, pyridine
Thioketones zinc 3；
The preparation method of the non-rusting solution, includes the following steps：
(1) calcium acetylacetonate is taken, is added in the absolute ethyl alcohol of 9 times of its weight, insulated and stirred 20 minutes at 70 DEG C；
(2) lanolin is taken, is added in the deionized water of 20 times of its weight, stirs evenly, with above-mentioned calcium acetylacetonate
Alcoholic solution mixes, and stirs evenly, and ammonium hydroxide is added dropwise, and it is 11 to adjust pH, is stirred to react 40 minutes, obtains wool lipoprotein solution；
(3) sodium metasilicate, zinc pyrithione mixing are taken, is added in above-mentioned wool lipoprotein solution, stirs evenly, add in N- methyl
Pyrrolidones, raising temperature are 80 DEG C, add in trimethyl hydroxyethylammonium ethylenediamine, ultrasonic 15 minutes to get the non-rusting solution.
Performance test：
Take the present invention surface conditioning agent handle aluminium alloy respectively, copper-iron alloy plank is tested, the specification of two kinds of plank
It is 80mm × 100mm × 4mm, which is laterally cut, carry out spray test, agents useful for same is a concentration of 5% chlorination
Sodium solution, test period 300 hours measure the bubbling width formed in cutting line side, and as a result bubbling width is 0；
Salt tolerance：
The above-mentioned two kinds of planks handled respectively are immersed in a concentration of 5% sodium chloride solution, are impregnated 300 hours, material
Expect that surface is substantially unchanged, impregnate 300 hours, no rust staining occurs.
Claims (3)
1. a kind of preparation method of anti-corrosion silane surface treatment agent, which is characterized in that include the following steps：
(1) lanolin of 2-3 parts by weight is taken, is added in the deionized water of 20-30 times of its weight, stirs evenly, adds in 0.1-
The azodicarbonamide of 0.2 parts by weight, is sent in 60-67 DEG C of water bath with thermostatic control, insulated and stirred 1-2 hours, and 7-9 weight is added dropwise
The sodium hydroxide of part, a concentration of 4-5mol/l, discharges after being added dropwise, stirs evenly, obtain acyl amine aqueous solution；
(2) three ammonium molybdates of 4-6 parts by weight, the silane coupling agent kh560 mixing of 0.3-0.5 parts by weight are taken, is added to mixture
In the absolute ethyl alcohol of 1.6-2 times of weight, raising temperature is 50-60 DEG C, and insulated and stirred 2-3 hours obtains silanol solution；
(3) allyl polyglycol of 5-7 parts by weight is taken, insulated and stirred 16-20 minutes at 70-80 DEG C, adds in 3-4 parts by weight
Tetramethyl disiloxane, 20-30 parts by weight non-rusting solution, continue insulated and stirred 10-20 minutes, be added to above-mentioned silanol
It is 3-4 minutes ultrasonic in solution, obtain compound alcohol dispersion liquid；
(4) acrylic acid of 3-4 parts by weight is taken, is added in the deionized water of 14-20 times of its weight, stirs evenly, it is and above-mentioned multiple
The mixing of alcohol dispersion liquid is closed, is stirred evenly, the platinum dioxide of 0.1-0.2 parts by weight is added in, is passed through nitrogen, is kept the temperature at 40-50 DEG C
Reaction 10-15 hours, obtains cross-linked disperse liquid；
(5) above-mentioned acyl amine aqueous solution, the mixing of cross-linked disperse liquid are taken, stirs evenly, adds in the laurylene base fourth of 0.1-0.3 parts by weight
Diacid, 1600-2000 revs/min is stirred 1-2 hours to get the anti-corrosion silane surface treatment agent.
2. the preparation method of a kind of anti-corrosion silane surface treatment agent according to claim 1, which is characterized in that described is anti-
Rust solvent is made of the raw material of following weight parts：
N-Methyl pyrrolidone 17-20, sodium metasilicate 3-4, calcium acetylacetonate 0.5-1, trimethyl hydroxyethylammonium ethylenediamine 1-2, wool
Fat 4-6, zinc pyrithione 2-3；
The preparation method of the non-rusting solution, includes the following steps：
(1) calcium acetylacetonate is taken, is added in the absolute ethyl alcohol of 6-9 times of its weight, insulated and stirred 10-20 points at 60-70 DEG C
Clock；
(2) lanolin is taken, is added in the deionized water of 15-20 times of its weight, stirs evenly, the alcohol with above-mentioned calcium acetylacetonate
Solution mixes, and stirs evenly, and ammonium hydroxide is added dropwise, and adjusting pH is 10-11, is stirred to react 30-40 minutes, obtains wool lipoprotein solution；
(3) sodium metasilicate, zinc pyrithione mixing are taken, is added in above-mentioned wool lipoprotein solution, stirs evenly, add in N- methylpyrroles
Alkanone, raising temperature are 75-80 DEG C, add in trimethyl hydroxyethylammonium ethylenediamine, ultrasonic 10-15 minutes to get the non-rusting solution.
A kind of 3. preparation method of anti-corrosion silane surface treatment agent according to claim 2, which is characterized in that the ammonia
A concentration of 10-12% of water.
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|---|---|---|---|
| CN201711279037.2A CN108165972A (en) | 2017-12-06 | 2017-12-06 | A kind of preparation method of anti-corrosion silane surface treatment agent |
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| CN201711279037.2A CN108165972A (en) | 2017-12-06 | 2017-12-06 | A kind of preparation method of anti-corrosion silane surface treatment agent |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107033740A (en) * | 2017-05-26 | 2017-08-11 | 赵阳 | A kind of preparation method of antibacterial anticorrosion waterborne epoxy coatings |
| CN107201151A (en) * | 2017-07-06 | 2017-09-26 | 董艺 | One kind conjugation anticorrosion water-soluble epoxy coating and preparation method thereof |
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2017
- 2017-12-06 CN CN201711279037.2A patent/CN108165972A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107033740A (en) * | 2017-05-26 | 2017-08-11 | 赵阳 | A kind of preparation method of antibacterial anticorrosion waterborne epoxy coatings |
| CN107201151A (en) * | 2017-07-06 | 2017-09-26 | 董艺 | One kind conjugation anticorrosion water-soluble epoxy coating and preparation method thereof |
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