CN104313559A - Vitrifying agent, preparation method of vitrifying agent and vitrifying treatment method using vitrifying agent - Google Patents
Vitrifying agent, preparation method of vitrifying agent and vitrifying treatment method using vitrifying agent Download PDFInfo
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- CN104313559A CN104313559A CN201410633281.4A CN201410633281A CN104313559A CN 104313559 A CN104313559 A CN 104313559A CN 201410633281 A CN201410633281 A CN 201410633281A CN 104313559 A CN104313559 A CN 104313559A
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- vitrifying
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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
- 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
- C23C22/73—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 characterised by the process
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- Chemical & Material Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Treatment Of Metals (AREA)
Abstract
The invention discloses a vitrifying agent which comprises the following materials in percentage by mass: 20%-30% of a titanium-zirconium compound, 5%-15% of fluosilicic acid, 0.1%-5% of nano silicon dioxide-aqueous emulsion, 10%-15% of water-soluble acrylic resin and the balance of water. The invention further discloses a preparation method of the vitrifying agent and a vitrifying treatment method using the vitrifying agent. According to the vitrifying agent, the pollution cannot be polluted as the vitrifying agent does not contain phosphorus or heavy metal which is harmful to a human body; when the metal surface is treated with the vitrifying agent, a layer of film can be formed on the metal surface to protect metal from being oxidized by air; vitrifying agent waste liquid after vitrifying treatment can be directly discharged after being subjected to pH adjustment, so that the wastewater discharge cost of producers is reduced; the vitrifying agent waste liquid also does not contain heavy metal harmful to the human body and phosphorus, so that the environment also cannot be polluted when the metal surface is treated with the vitrifying agent.
Description
Technical field
The present invention relates to and surface-treated vitrified agent is carried out to metal works (especially cold rolled plate, galvanized sheet and aluminium sheet), also relate to the preparation method of this vitrified agent, and it applies the method for carrying out vitrification process of this vitrified agent.
Background technology
Phosphatization is traditional anticorrosive metal process of surface treatment, and the chemical agent that phosphating process uses has: phosphoric acid zinc salt, containing nickelic compound, chromyl compound etc., its technical process as shown in Figure 1:
S001, carries out skimming treatment about 2 ~ 5 minutes to metallic surface;
S002, is undertaken the metal after skimming treatment washing about 30 seconds;
S003, carries out table and mediates reason about 30 seconds;
S004 is carry out bonderizing in the environment of 25 ~ 40 DEG C about 2 ~ 5 minutes in temperature;
S005, carries out twice washing by metallic surface, about 30 seconds at every turn;
Also need to comprise follow-up liquid waste disposal flow process after above-mentioned flow process completes:
S006, the heavy metal sediment cleaning that the chemical agent after bonderizing is formed;
S007, heavy metal sediment transport cleaning.
There is following shortcoming in bonderizing: (1) contains phosphorus and harmful heavy metal in the waste liquid of discharging after metal finishing, can cause great pollution to environment, destroys the eubiosis; (2) discharge capacity, waste of manpower and the material resources of sewage can be strengthened in the process of liquid waste disposal.
Summary of the invention
The object of the present invention is to provide a kind of vitrified agent, with at least one in solving the problems of the technologies described above.
Another object of the present invention is the preparation method providing above-mentioned vitrified agent, with at least one in solving the problems of the technologies described above.
Another object of the present invention is to provide the above-mentioned vitrified agent of application to carry out the method for vitrification process, with at least one in solving the problems of the technologies described above.
According to an aspect of the present invention, provide a kind of vitrified agent, comprise the material of following mass percent: titanium zirconium composite 20% ~ 30%, silicofluoric acid 5% ~ 15%, nano silicon-water miscible liquid 0.1% ~ 5%, water soluble acrylic resin 10% ~ 15%, all the other are water.Wherein, in nano silicon-water miscible liquid, the mass concentration of nano silicon is 10 ~ 30%.
Further, above-mentioned vitrified agent can comprise the material of following mass percent: titanium zirconium composite 22% ~ 27%, silicofluoric acid 8% ~ 10%, nano silicon-water miscible liquid 0.5% ~ 1.5% and water soluble acrylic resin 10% ~ 12%, and all the other are water.
Further, above-mentioned vitrified agent can comprise the material of following mass percent: titanium zirconium composite 24%, silicofluoric acid 8%, nano silicon-water miscible liquid 1% and water soluble acrylic resin 12%, and all the other are water.
In some embodiments, titanium zirconium composite can be compounded to form by the material of following mass fraction: fluorine zirconic acid 1 ~ 1.5 part, hydrofluotitanic acid 1 ~ 1.5 part and 0.05 ~ 0.3 part, hydrofluoric acid.
Vitrified agent of the present invention, for acidic liquid, iron and steel work slight erosion can be made, due in this corrosion process, thus make the pH value of vitrified agent and metallic surface near interface increase, and then cause the oxide compound of zirconium titanium and fluorine to be separated out, nanometer two sample SiClx is formed after acid organosilane with water soluble acrylic resin and is combined with above-mentioned precipitate, be attached to metallic surface by coordination compound effect, define one deck conversion film in metallic surface.Compared with traditional phosphatization, the present invention has the following advantages:
1, vitrified agent of the present invention is not containing heavy metal and phosphorus, and product is containing producing sediment, and tank liquor can directly discharge after PH adjustment, effectively decreases the input using producer for discharge of wastewater.
2, vitrified agent suitability of the present invention is comparatively wide, goes for various different sheet material, as: cold rolled plate, galvanized sheet and aluminium etc.
3, through measuring, use thinner than zinc phosphate of the epithelium of the formation of vitrified agent of the present invention, per kilogram stoste can process more workpiece, effectively provides cost savings.
According to another aspect of the present invention, provide the preparation method of above-mentioned vitrified agent, comprise the steps:
Titanium zirconium composite, fluorochemical, silica composite, organic-silicon-modified resin and water will be asked in proportion, stir 30 ~ 60 minutes with the speed of 80 ~ 120 revs/min in corrosion-resistant container (can be generally the container that the stainless steel of No. 316 or PE make), then elimination insolubles.
The preparation method of vitrified agent of the present invention, simple to operate, processing requirement is simple, suitable for large-scale promotion.
According to a further aspect of the invention, provide the method that the above-mentioned vitrified agent of application carries out vitrification process, comprise the following steps:
A) skimming treatment is carried out to pending metallic surface;
B) twice washing is carried out to the metal after step a) processes;
C) by through step b) metal after process puts into described vitrified agent, and carries out vitrification process;
D) to through step c) metal after process carries out washing and processes.
Vitrification technique of the present invention has the following advantages:
1, use vitrified agent of the present invention to carry out metal finishing, whole treating processes operates all at normal temperatures, does not need heating, effectively decreases the heat energy consumption of producer.
2, use the vitrification time >20 second of vitrified agent of the present invention, the time of relative zinc phosphate process (generally at 2-5 minute) is shorter.
3, after using vitrified agent of the present invention, vitrification technique is simpler, the process of tradition zinc phosphate needs degreasing, washing, table tune, phosphatization four basic steps, and vitrification process of the present invention only needs degreasing, washing, vitrification three steps, greatly reduces the equipment investment using producer.
Accompanying drawing explanation
Fig. 1 is the schema of traditional metal surface treatment process;
Fig. 2 is the schema of the preparation method of vitrified agent of the present invention;
Fig. 3 is the schema that this vitrified agent of application carries out vitrification process.
Embodiment
Below in conjunction with accompanying drawing, the present invention is further detailed explanation.
As shown in Figure 2, S101, will ask for each material by table 1 and table 2.
S102, is positioned over above-mentioned substance in corrosion-resistant reactor (can be generally the container that the stainless steel of No. 316 or PE make) with 80 ~ 120 revs/min of speed stirring mixtures 30 ~ 60 minutes;
S103, elimination insolubles, obtained vitrified agent of the present invention.
| ? | Titanium zirconium composite | Silicofluoric acid | Nano silicon-water miscible liquid | Water soluble acrylic resin | Water |
| Embodiment 1 | 20 | 11 | 2.5 | 15 | 51.5 |
| Embodiment 2 | 26 | 13 | 5 | 14 | 42 |
| Embodiment 3 | 30 | 15 | 0.1 | 13 | 41.9 |
| Embodiment 4 | 24 | 5 | 0.5 | 12.5 | 58 |
| Embodiment 5 | 25 | 6 | 1 | 12 | 56 |
| Embodiment 6 | 22 | 7 | 1.5 | 11.5 | 58 |
| Embodiment 7 | 23 | 8 | 2 | 11 | 56 |
| Embodiment 8 | 27 | 9 | 3 | 10.5 | 50.5 |
| Embodiment 9 | 28 | 10 | 4 | 10 | 48 |
Table 1 (unit: mass percent)
| ? | Titanium zirconium composite | Nano silicon-water miscible liquid mass concentration |
| Embodiment 1 | Fluorine zirconic acid 1 part, hydrofluotitanic acid 1 part and 0.05 part, hydrofluoric acid | 15 |
| Embodiment 2 | Fluorine zirconic acid 1.1 parts, hydrofluotitanic acid 1.4 parts and 0.08 part, hydrofluoric acid | 30 |
| Embodiment 3 | Fluorine zirconic acid 1.2 parts, hydrofluotitanic acid 1.3 parts and 0.1 part, hydrofluoric acid | 25 |
| Embodiment 4 | Fluorine zirconic acid 1.3 parts, hydrofluotitanic acid 1.2 parts and 0.12 part, hydrofluoric acid | 12 |
| Embodiment 5 | Fluorine zirconic acid 1.4 parts, hydrofluotitanic acid 1.1 parts and 0.15 part, hydrofluoric acid | 20 |
| Embodiment 6 | Fluorine zirconic acid 1.5 parts, hydrofluotitanic acid 1.2 parts and 0.17 part, hydrofluoric acid | 17 |
| Embodiment 7 | Fluorine zirconic acid 1.2 parts, hydrofluotitanic acid 1.3 parts and 0.30 part, hydrofluoric acid | 22 |
| Embodiment 8 | Fluorine zirconic acid 1.2 parts, hydrofluotitanic acid 1.4 parts and 0.20 part, hydrofluoric acid | 10 |
| Embodiment 9 | Fluorine zirconic acid 1.4 parts, hydrofluotitanic acid 1.5 parts and 0.25 part, hydrofluoric acid | 27 |
Table 2
Get above-mentioned obtained vitrified agent, respectively vitrification process is carried out to metal sample (cold-reduced sheet, galvanized sheet, aluminium sheet) surface by flow process shown in Fig. 3.The specification of metal sample is 5cm × 5cm, and thickness is no more than 1mm.The idiographic flow of vitrification process is as follows:
S201, carries out skimming treatment by pending metallic surface, is generally to be removed by the grease of metallic surface with the weakly alkaline solution that soda ash etc. is made into.Generally speaking, degreasing time is 2-5 minute
S202, the metal after skimming treatment is carried out twice washing (object of washing be by metallic surface because of material wash clean residual in step S201, facilitate subsequent operations), generally speaking, the time of washing is 30 seconds/time.
S203, puts into vitrified agent by metal, and carries out vitrification process; Vitrification process namely, after metal is put into vitrified agent, metallic surface and vitrified agent generation chemical reaction.Generally speaking, the vitrification time is about 20 seconds.
S204, carries out washing process by the metal after vitrification process.Then, metal is dried up (drying without stove), measure metal gross weight A, precisely to 0.1 milligram.
After vitrification process, measure the film weight of the film that metallic surface is formed according to the following steps:
First demoulding process is carried out to metallic surface.Cold-reduced sheet concentration is that the KOH solution of 45% (wt/wt) soaks 10min, under the temperature condition of 66 DEG C, carry out demoulding.The salt acid soak 10min of galvanized sheet 4mol/L, carries out demoulding.The salpeter solution of aluminium sheet 1:1 (mass percentage concentration is that 65% salpeter solution mixes with volume ratio 1:1 with water) soaks 10min demoulding.
After demoulding, first (at least 1 minute) is washed to completely clean to metal sheet, then dry up (drying without stove), and measure its weight B, be accurate to 0.1 milligram.Film weight according to following formulae discovery unit surface: (A-B)/surface-area, surface-area=2 × 5cm × 5cm=0.005m
2and result is charged in table 3.
Meanwhile, the metal sample getting same size carries out bonderizing with traditional phosphorization agent by the flow process in background technology.Metal is dried up (drying without stove), measure metal gross weight A, precisely to 0.1 milligram.Wherein, consisting of of phosphorization agent: mass ratio be 15 ~ 17% primary zinc phosphate, 14 ~ 16% zinc nitrate, 0.5 ~ 0.8% phosphoric acid, 4 ~ 6% SODIUMNITRATE, 0.04 ~ 0.05 cupric nitrate, the nickelous nitrate of 0.1 ~ 0.2%, appropriate hydrogen peroxide and water, phosphatization temperature is 20 DEG C, and phosphating time is 5 ~ 7min.
Metal after bonderizing carries out demoulding process by the method for demoulding in the GB9792-88 measuring method of film quality " in the conversion film unit surface on metallic substance ".
After demoulding, first (at least 1 minute) is washed to completely clean to metal sheet, then dry up (drying without stove), and measure its weight B, be accurate to 0.1 milligram.Film weight according to following formulae discovery unit surface: (A-B)/surface-area, surface-area=2 × 5cm × 5cm=0.005m
2and result is charged in table 3.
Table 3
As can be seen from Table 3: the film that the method for application vitrified agent process metal surfaces obtains is heavily 80.0 ~ 200.0mg/ ㎡, and the film that relative conventional phosphatizing method obtains weighs 2240.0 ~ 2300.0mg/ ㎡, and film is thinner, therefore can be cost-saving.
Above-described is only some embodiments of the present invention.For the person of ordinary skill of the art, without departing from the concept of the premise of the invention, can also make some distortion and improvement, these all belong to protection scope of the present invention.
Claims (7)
1. a vitrified agent, is characterized in that, comprises the material of following mass percent: titanium zirconium composite 20% ~ 30%, silicofluoric acid 5% ~ 15%, nano silicon-water miscible liquid 0.1% ~ 5%, water soluble acrylic resin 10% ~ 15%, and all the other are water.
2. vitrified agent according to claim 1, is characterized in that, described titanium zirconium composite is compounded to form by the material of following mass fraction: fluorine zirconic acid 1 ~ 1.5 part, hydrofluotitanic acid 1 ~ 1.5 part and 0.05 ~ 0.3 part, hydrofluoric acid.
3. vitrified agent according to claim 2, is characterized in that, in described nano silicon-water miscible liquid, the mass concentration of nano silicon is 10 ~ 30%.
4. vitrified agent according to claim 3, it is characterized in that, comprise the material of following mass percent: titanium zirconium composite 22% ~ 27%, silicofluoric acid 8% ~ 10%, nano silicon-water miscible liquid 0.5% ~ 1.5% and water soluble acrylic resin 10% ~ 12%, all the other are water.
5. vitrified agent according to claim 3, is characterized in that, comprises the material of following mass percent: titanium zirconium composite 24%, silicofluoric acid 8%, nano silicon-water miscible liquid 1% and water soluble acrylic resin 12%, and all the other are water.
6. a preparation method for vitrified agent according to any one of Claims 1 to 5, is characterized in that, comprises the steps:
Get titanium zirconium composite, fluorochemical, silica composite, organic-silicon-modified resin and water by the proportion requirement according to any one of Claims 1 to 4, in corrosion-resistant container, stir 30-60 minute, then elimination insolubles with the speed of 80 ~ 120 revs/min.
7. application rights requires that according to any one of 1 ~ 5, vitrified agent carries out a method for vitrification process, is characterized in that, comprises the following steps:
A) skimming treatment is carried out to pending metallic surface;
B) twice washing is carried out to the metal after step a) processes;
C) by through step b) metal after process puts into described vitrified agent, and carries out vitrification process;
D) to through step c) metal after process carries out washing and processes.
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| CN201410633281.4A CN104313559A (en) | 2014-11-11 | 2014-11-11 | Vitrifying agent, preparation method of vitrifying agent and vitrifying treatment method using vitrifying agent |
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| CN201410633281.4A CN104313559A (en) | 2014-11-11 | 2014-11-11 | Vitrifying agent, preparation method of vitrifying agent and vitrifying treatment method using vitrifying agent |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106435548A (en) * | 2016-09-28 | 2017-02-22 | 广州凯耀资产管理有限公司 | Automotive window metal processing solution and preparation method and application method thereof |
Citations (4)
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|---|---|---|---|---|
| EP0008942A1 (en) * | 1978-09-06 | 1980-03-19 | Amchem Products, Inc. a Corporation organised under the Laws of the State of Delaware United States of America | Compositions and processes for coating aluminium |
| US5129967A (en) * | 1988-05-03 | 1992-07-14 | Betz Laboratories, Inc. | Composition and method for non-chromate coating of aluminum |
| CN1441856A (en) * | 2000-07-25 | 2003-09-10 | 关西涂料株式会社 | Coating material for forming titanium oxide film, method for forming titanium oxide film and use of said coating material |
| CN101476120A (en) * | 2009-01-23 | 2009-07-08 | 合肥普庆新材料科技有限公司 | Environment-friendly type metal surface finishing agent and preparation thereof |
-
2014
- 2014-11-11 CN CN201410633281.4A patent/CN104313559A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0008942A1 (en) * | 1978-09-06 | 1980-03-19 | Amchem Products, Inc. a Corporation organised under the Laws of the State of Delaware United States of America | Compositions and processes for coating aluminium |
| US5129967A (en) * | 1988-05-03 | 1992-07-14 | Betz Laboratories, Inc. | Composition and method for non-chromate coating of aluminum |
| CN1441856A (en) * | 2000-07-25 | 2003-09-10 | 关西涂料株式会社 | Coating material for forming titanium oxide film, method for forming titanium oxide film and use of said coating material |
| CN101476120A (en) * | 2009-01-23 | 2009-07-08 | 合肥普庆新材料科技有限公司 | Environment-friendly type metal surface finishing agent and preparation thereof |
Non-Patent Citations (2)
| Title |
|---|
| PHILIP D. DECK ET AL.: "Investigation of fluoacid based conversion coatings on aluminum", 《PROGRESS IN ORGANIC COATINGS》 * |
| 邹洪庆: "铸铝合金锆系非铬化学成膜处理工艺应用", 《材料保护》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106435548A (en) * | 2016-09-28 | 2017-02-22 | 广州凯耀资产管理有限公司 | Automotive window metal processing solution and preparation method and application method thereof |
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Application publication date: 20150128 |