CN103866307A - Environment-friendly single-dose and double-color galvanized trivalent chromium passivation agent and preparation and application methods thereof - Google Patents
Environment-friendly single-dose and double-color galvanized trivalent chromium passivation agent and preparation and application methods thereof Download PDFInfo
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Abstract
The invention provides an environment-friendly single-dose and double-color galvanized trivalent chromium passivation agent, which is prepared from the following raw materials: 5-30g of chromic chloride, 6-10g of fluoride, 3-6g of sulfate, 5-10ml of nitric acid with the mass concentration of 98%, 0.01-0.1g of fatty alcohol-polyoxyethylene ether, and the balance being water and impurities in per liter. The environment-friendly single-dose and double-color galvanized trivalent chromium passivation agent disclosed by the invention is simple in components, fewer in materials, and low in cost, and can be obtained by a single dose, the production cost can be saved, the manufacturing procedure is simplified, the work efficiency is improved, the formed passivation coating does not contain a noxious substance of hexavalent chromium, and pollution of the harmful hexavalent chromium is avoided from the production process of the passivation agent. The generated wastewater does not contain hexavalent chromium and is small in content of trivalent chromium, the wastewater treatment process is simple, environment-friendly and low-carbon, and the history that harmful hexavalent chromium seriously pollutes the environment is completely avoided.
Description
Technical field
The present invention relates to a kind of environment-friendly type passivator, relate in particular to the double-colored zinc-plated trivalent chromium passivator of a kind of environment-friendly type potion and preparation and application thereof.
Background technology
Passivator is a kind of chemical agent, can carry out passivation to workpiece (especially metal works) under certain condition, forms one deck passive film at workpiece surface, and this layer of passive film can strengthen the antiseptic power of workpiece.Existing passivator has following deficiency: in the passive film forming, contain poisonous sexavalent chrome; Can not use a kind of passivator to form the passive film of two kinds of colors.
Summary of the invention
The technical problem to be solved in the present invention is: the passive film that existing passivator generates contains poisonous sexavalent chrome, can not use a kind of passivator to form the passive film of two kinds of colors.
In order to solve the problems of the technologies described above, the invention provides the double-colored zinc-plated trivalent chromium passivator of a kind of environment-friendly type potion, formed by chromium chloride, fluorochemical, vitriol, nitric acid, fatty alcohol-polyoxyethylene ether and water; In every liter of double-colored zinc-plated trivalent chromium passivator of environment-friendly type potion, contain 5～30g chromium chloride, 6～10g fluorochemical, 3～6g vitriol, the nitric acid that 5～10ml mass concentration is 98%, 0.01～0.1g fatty alcohol-polyoxyethylene ether, all the other are water and impurity.
Preferably, the pH value of the described double-colored zinc-plated trivalent chromium passivator of environment-friendly type potion is 1.8～2.3.
Preferably, described vitriol is rose vitriol, single nickel salt and/or magnesium sulfate.
Preferably, described fluorochemical is Sodium Fluoride and/or Neutral ammonium fluoride.
The present invention also provides the preparation method of the above-mentioned double-colored zinc-plated trivalent chromium passivator of environment-friendly type potion, comprises and carries out in order following steps:
Step 1: by chromium chloride, fluorochemical, vitriol and water mix and blend in non-metallic container;
Step 2: add nitric acid and fatty alcohol-polyoxyethylene ether and stir in the aqueous solution obtaining by step 1;
Step 3: to adding water in the aqueous solution obtaining by step 2 and obtaining product;
Wherein, make to contain 5～30g chromium chloride in every liter of double-colored zinc-plated trivalent chromium passivator of environment-friendly type potion by step 1 to step 3,6～10g fluorochemical, 3～6g vitriol, 5～10ml mass concentration is 98% nitric acid, 0.01～0.1g fatty alcohol-polyoxyethylene ether, and product pH value is adjusted into 1.8～2.3.
The present invention also provides a kind of using method of the above-mentioned double-colored zinc-plated trivalent chromium passivator of environment-friendly type potion, comprises and treats the step that passivation workpiece carries out the step of passivation and the workpiece after passivation is dried.
The time of preferably, carrying out passivation is 3 seconds to 20 seconds.
The time of preferably, carrying out passivation is 30 seconds to 50 seconds.
Preferably, the temperature of carrying out passivation is 5～50 ℃, and the temperature of drying is 50～80 ℃.
Beneficial effect of the present invention is as follows:
1. the double-colored zinc-plated trivalent chromium passivator component of environment-friendly type potion provided by the invention is simple, materials are few, cost is low; Can be by the control of the time of carrying out passivation being reached to the color (pearl opal or light colour) needing, potion gets both; Because component is simple, so can save production cost, simplify manufacturing procedure, increase work efficiency;
2. in the passive film obtaining by the double-colored zinc-plated trivalent chromium passivator of this environment-friendly type potion of use, without chromyl nuisance, from the production technique of passivator, eliminated harmful chromic pollution;
3. the waste water that the production technique of the double-colored zinc-plated trivalent chromium passivator of this environment-friendly type potion produces is not containing sexavalent chrome, chromic content is little, waste water treatment process is simple, compared with the production technique of existing passivator, there is feature simple to operate, environmental protection low-carbon (LC) (less energy-consumption), eliminated the history of poisonous hexavalent chromium serious environment pollution completely.
Embodiment
To the technical scheme in the embodiment of the present invention be clearly and completely described below.
In the following embodiments, carry out passivation and refer to workpiece is immersed to the operation in passivator, the time of carrying out passivation is the time that workpiece is detained in passivator, and the temperature of drying refers to the temperature when workpiece after passivation is at high temperature dried.
Embodiment 1
The present embodiment provides a kind of environment-friendly type passivator, and this environment-friendly type passivator is made up of chromium chloride, Sodium Fluoride, rose vitriol, nitric acid, fatty alcohol-polyoxyethylene ether and water; In every liter of environment-friendly type passivator, contain 5g chromium chloride, 8g Sodium Fluoride, 4g rose vitriol, the nitric acid that 10ml mass concentration is 98%, 0.07g fatty alcohol-polyoxyethylene ether, all the other are water and impurity, the pH value of this environment-friendly type passivator is 2.3.
The preparation method of above-mentioned environment-friendly type passivator comprises and carries out in order following steps:
Step 1: 5g chromium chloride, 8g Sodium Fluoride, 4g rose vitriol and water are mixed to solid in non-metallic container and fully dissolve, in this step, the mixture of chromium chloride, Sodium Fluoride and rose vitriol is 1:1.5 with the water volume ratio adding;
Step 2: to add 4ml mass concentration in the aqueous solution obtaining by step 1 be 98% nitric acid and 0.07g fatty alcohol-polyoxyethylene ether and stir, mixture is mixed;
Step 3: add water in the aqueous solution obtaining by step 2, the volume that makes product is 1 liter;
Wherein, product pH value being controlled to step 3 by step 1 is 2.3.
The using method of above-mentioned environment-friendly type passivator comprises treats the step that passivation workpiece carries out the step of passivation and the workpiece after passivation is dried.
Wherein, the time of carrying out passivation is 20 seconds, and the temperature of carrying out passivation is 45 ℃, and the temperature of drying is 50 ℃, is pearl opal through the workpiece of passivation.
Embodiment 2
The present embodiment provides a kind of environment-friendly type passivator, and this environment-friendly type passivator is made up of chromium chloride, Neutral ammonium fluoride, rose vitriol, nitric acid, fatty alcohol-polyoxyethylene ether and water; In every liter of environment-friendly type passivator, contain 30g chromium chloride, 9g Neutral ammonium fluoride, 5g rose vitriol, the nitric acid that 5ml mass concentration is 98%, 0.09g fatty alcohol-polyoxyethylene ether, all the other are water and impurity, the pH value of this environment-friendly type passivator is 1.8.
The preparation method of above-mentioned environment-friendly type passivator comprises and carries out in order following steps:
Step 1: 30g chromium chloride, 9g Neutral ammonium fluoride, 5g rose vitriol and water are mixed to solid in non-metallic container and fully dissolve, in this step, the mixture of chromium chloride, Neutral ammonium fluoride and rose vitriol is 1:1.6 with the water volume ratio adding;
Step 2: to add 5ml mass concentration in the aqueous solution obtaining by step 1 be 98% nitric acid and 0.09g fatty alcohol-polyoxyethylene ether and stir, mixture is mixed;
Step 3: add water in the aqueous solution obtaining by step 2, the volume that makes product is 1 liter;
Wherein, product pH value being controlled to step 3 by step 1 is 1.8.
The using method of above-mentioned environment-friendly type passivator comprises treats the step that passivation workpiece carries out the step of passivation and the workpiece after passivation is dried.
Wherein, the time of carrying out passivation is 3 seconds, and the temperature of carrying out passivation is 50 ℃, and the temperature of drying is 80 ℃, is pearl opal through the workpiece of passivation.
Embodiment 3
The present embodiment provides a kind of environment-friendly type passivator, and this environment-friendly type passivator is made up of chromium chloride, Sodium Fluoride, single nickel salt, nitric acid, fatty alcohol-polyoxyethylene ether and water; In every liter of environment-friendly type passivator, contain 10g chromium chloride, 6g Sodium Fluoride, 3g single nickel salt, the nitric acid that 7ml mass concentration is 98%, 0.01g fatty alcohol-polyoxyethylene ether, all the other are water and impurity, the pH value of this environment-friendly type passivator is 2.1.
The preparation method of above-mentioned environment-friendly type passivator comprises and carries out in order following steps:
Step 1: 10g chromium chloride, 6g Sodium Fluoride, 3g single nickel salt and water are mixed to solid in non-metallic container and fully dissolve, in this step, the mixture of chromium chloride, Sodium Fluoride and single nickel salt is 1:1.8 with the water volume ratio adding;
Step 2: to add 7ml mass concentration in the aqueous solution obtaining by step 1 be 98% nitric acid and 0.01g fatty alcohol-polyoxyethylene ether and stir, mixture is mixed;
Step 3: add water in the aqueous solution obtaining by step 2, the volume that makes product is 1 liter;
Wherein, product pH value being controlled to step 3 by step 1 is 2.1.
The using method of above-mentioned environment-friendly type passivator comprises treats the step that passivation workpiece carries out the step of passivation and the workpiece after passivation is dried.
Wherein, the time of carrying out passivation is 10 seconds, and the temperature of carrying out passivation is 25 ℃, and the temperature of drying is 75 ℃, is pearl opal through the workpiece of passivation.
Embodiment 4
The present embodiment provides a kind of environment-friendly type passivator, and this environment-friendly type passivator is made up of chromium chloride, Neutral ammonium fluoride, single nickel salt, nitric acid, fatty alcohol-polyoxyethylene ether and water; In every liter of environment-friendly type passivator, contain 28g chromium chloride, 8g Neutral ammonium fluoride, 6g single nickel salt, the nitric acid that 9ml mass concentration is 98%, 0.1g fatty alcohol-polyoxyethylene ether, all the other are water and impurity, the pH value of this environment-friendly type passivator is 2.2.
The preparation method of above-mentioned environment-friendly type passivator comprises and carries out in order following steps:
Step 1: 28g chromium chloride, 8g Neutral ammonium fluoride, 6g single nickel salt and water are mixed to solid in non-metallic container and fully dissolve, in this step, the mixture of chromium chloride, Neutral ammonium fluoride and single nickel salt is 1:2 with the water volume ratio adding;
Step 2: to add 9ml mass concentration in the aqueous solution obtaining by step 1 be 98% nitric acid and 0.1g fatty alcohol-polyoxyethylene ether and stir, mixture is mixed;
Step 3: add water in the aqueous solution obtaining by step 2, the volume that makes product is 1 liter;
Wherein, product pH value being controlled to step 3 by step 1 is 2.2.
The using method of above-mentioned environment-friendly type passivator comprises treats the step that passivation workpiece carries out the step of passivation and the workpiece after passivation is dried.
Wherein, the time of carrying out passivation is 50 seconds, and the temperature of carrying out passivation is 5 ℃, and the temperature of drying is 60 ℃, is light colour through the workpiece of passivation.
Embodiment 5
The present embodiment provides a kind of environment-friendly type passivator, and this environment-friendly type passivator is made up of chromium chloride, Sodium Fluoride, magnesium sulfate, nitric acid, fatty alcohol-polyoxyethylene ether and water; In every liter of environment-friendly type passivator, contain 18g chromium chloride, 7g Sodium Fluoride, 4g magnesium sulfate, the nitric acid that 6ml mass concentration is 98%, 0.03g fatty alcohol-polyoxyethylene ether, all the other are water and impurity, the pH value of this environment-friendly type passivator is 1.9.
The preparation method of above-mentioned environment-friendly type passivator comprises and carries out in order following steps:
Step 1: 18g chromium chloride, 7g Sodium Fluoride, 4g magnesium sulfate and water are mixed to solid in non-metallic container and fully dissolve, in this step, the mixture of chromium chloride, Sodium Fluoride and magnesium sulfate is 1:2.2 with the water volume ratio adding;
Step 2: to add 6ml mass concentration in the aqueous solution obtaining by step 1 be 98% nitric acid and 0.03g fatty alcohol-polyoxyethylene ether and stir, mixture is mixed;
Step 3: add water in the aqueous solution obtaining by step 2, the volume that makes product is 1 liter;
Wherein, product pH value being controlled to step 3 by step 1 is 1.9.
The using method of above-mentioned environment-friendly type passivator comprises treats the step that passivation workpiece carries out the step of passivation and the workpiece after passivation is dried.
Wherein, the time of carrying out passivation is 30 seconds, and the temperature of carrying out passivation is 40 ℃, and the temperature of drying is 65 ℃, is light colour through the workpiece of passivation.
Embodiment 6
The present embodiment provides a kind of environment-friendly type passivator, and this environment-friendly type passivator is made up of chromium chloride, Neutral ammonium fluoride, magnesium sulfate, nitric acid, fatty alcohol-polyoxyethylene ether and water; In every liter of environment-friendly type passivator, contain 22g chromium chloride, 10g Neutral ammonium fluoride, 5g magnesium sulfate, the nitric acid that 8ml mass concentration is 98%, 0.05g fatty alcohol-polyoxyethylene ether, all the other are water and impurity, the pH value of this environment-friendly type passivator is 2.1.
The preparation method of above-mentioned environment-friendly type passivator comprises and carries out in order following steps:
Step 1: 22g chromium chloride, 10g Neutral ammonium fluoride, 5g magnesium sulfate and water are mixed to solid in non-metallic container and fully dissolve, in this step, the mixture of chromium chloride, Neutral ammonium fluoride and magnesium sulfate is 1:2.5 with the water volume ratio adding;
Step 2: to add 8ml mass concentration in the aqueous solution obtaining by step 1 be 98% nitric acid and 0.05g fatty alcohol-polyoxyethylene ether and stir, mixture is mixed;
Step 3: add water in the aqueous solution obtaining by step 2, the volume that makes product is 1 liter;
Wherein, product pH value being controlled to step 3 by step 1 is 2.1.
The using method of above-mentioned environment-friendly type passivator comprises treats the step that passivation workpiece carries out the step of passivation and the workpiece after passivation is dried.
Wherein, the time of carrying out passivation is 45 seconds, and the temperature of carrying out passivation is 15 ℃, and the temperature of drying is 55 ℃, is light colour through the workpiece of passivation.
Characteristics Detection
In the environment-friendly type passivator of above-described embodiment, chromium chloride is used for generating zinc chrome oxide compound, is main membrane-forming agent; Fluorochemical is complex coordination agent, plays hyperchromic, stable effect; Vitriol is film forming accelerating, plays katalysis; Nitric acid is oxygenant, also plays the effect of blast and guarantee pH value; Fatty alcohol-polyoxyethylene ether is dye leveller, for making even film layer.When preparation, water used can be selected tap water, preferably selects deionized water.
From the environment-friendly type passivator of embodiment 1 to embodiment 6, each portion that takes out, as sample, is followed successively by environment-friendly type passivator 1 to environment-friendly type passivator 6.Environment-friendly type passivator 1 to environment-friendly type passivator 6 is carried out to SGS(Soci é t é G é n é rale de Surveillance, general notary) detect, detected result shows: environment-friendly type passivator 1 to environment-friendly type passivator 6 does not all contain poisonous sexavalent chrome.As can be seen here, environment-friendly type passivator 1 to environment-friendly type passivator 6 meets, and has even exceeded the RoHS(Restriction of Hazardous Substances of European Union) environmental protection standard.
Get 2 parts of existing chromyl passivator, be designated as passivator 7 and passivator 8.Use environment-friendly type passivator 1 to environment-friendly type passivator 6, passivator 7 and passivator 8 respectively metal works of the same race to be carried out to passivation, drying operation, obtain respectively sample 1 to sample 8.Sample 1 to sample 8 is carried out to salt water immersion test (GB9794) to compare their passive film erosion resistance, and experimental result is in table 1.
Table 1
The erosion resistance of the passive film that the passive film erosion resistance that as can be seen from Table 1, above-mentioned environment-friendly type passivator forms forms with existing passivator is suitable.
Therefore the present invention has following beneficial effect:
1. environment-friendly type passivating agent composition provided by the invention is simple, materials are few, cost is low; Can be by the control of the time of carrying out passivation being reached to the color (pearl opal or light colour) needing, potion gets both; Because component is simple, so can save production cost, simplify manufacturing procedure, saving equipment, increases work efficiency;
2. in the passive film obtaining by this environment-friendly type of use passivator, without chromyl nuisance, from the production technique of passivator, eliminated harmful chromic pollution completely;
3. this environment-friendly type passivator long quality-guarantee period; The waste water that the production technique of this environment-friendly type passivator produces is not containing sexavalent chrome, chromic content is little, waste water treatment process is simple, compared with the production technique of existing passivator, there is feature simple to operate, environmental protection low-carbon (LC) (less energy-consumption), eliminate the history of poisonous hexavalent chromium serious environment pollution completely, even not to processing and also can reach discharging standards containing trivalent chromium waste water.
For the processing containing trivalent chromium waste water, in the time that the pH value of waste water is adjusted to 6-8, can produce Cr (OH) 3 precipitations, can eliminate after filtering poisonous trivalent chromic ion.
Obviously, described embodiment is only the present invention's part embodiment, rather than whole embodiment.Based on the embodiment in the present invention, those of ordinary skills, not making the every other embodiment obtaining under creative work prerequisite, belong to the scope of protection of the invention.
Claims (10)
1. the double-colored zinc-plated trivalent chromium passivator of environment-friendly type potion, is characterized in that: be made up of chromium chloride, fluorochemical, vitriol, nitric acid, fatty alcohol-polyoxyethylene ether and water; In every liter of double-colored zinc-plated trivalent chromium passivator of environment-friendly type potion, contain 5～30g chromium chloride, 6～10g fluorochemical, 3～6g vitriol, the nitric acid that 5～10ml mass concentration is 98%, 0.01～0.1g fatty alcohol-polyoxyethylene ether, all the other are water and impurity.
2. the double-colored zinc-plated trivalent chromium passivator of environment-friendly type potion according to claim 1, is characterized in that: the pH value of the double-colored zinc-plated trivalent chromium passivator of this environment-friendly type potion is 1.8～2.3.
3. the double-colored zinc-plated trivalent chromium passivator of environment-friendly type potion according to claim 1 and 2, is characterized in that: described vitriol is rose vitriol, single nickel salt and/or magnesium sulfate.
4. the double-colored zinc-plated trivalent chromium passivator of environment-friendly type potion according to claim 1 and 2, is characterized in that: described fluorochemical is Sodium Fluoride and/or Neutral ammonium fluoride.
5. the double-colored zinc-plated trivalent chromium passivator of environment-friendly type potion according to claim 3, is characterized in that: described fluorochemical is Sodium Fluoride and/or Neutral ammonium fluoride.
6. a preparation method for the double-colored zinc-plated trivalent chromium passivator of environment-friendly type potion as described in any one in claim 1 to 5, is characterized in that: carry out in order following steps:
Step 1: by chromium chloride, fluorochemical, vitriol and water mix and blend in non-metallic container;
Step 2: add nitric acid and fatty alcohol-polyoxyethylene ether and stir in the aqueous solution obtaining by step 1;
Step 3: to adding water in the aqueous solution obtaining by step 2 and obtaining product;
Wherein, make to contain 5～30g chromium chloride in every liter of double-colored zinc-plated trivalent chromium passivator of environment-friendly type potion by step 1 to step 3,6～10g fluorochemical, 3～6g vitriol, 5～10ml mass concentration is 98% nitric acid, 0.01～0.1g fatty alcohol-polyoxyethylene ether, and product pH value is adjusted into 1.8～2.3.
7. a using method for the double-colored zinc-plated trivalent chromium passivator of environment-friendly type potion as described in any one in claim 1 to 5, is characterized in that: comprise and treat the step that passivation workpiece carries out the step of passivation and the workpiece after passivation is dried.
8. the using method of the double-colored zinc-plated trivalent chromium passivator of environment-friendly type potion according to claim 7, is characterized in that: the time of carrying out passivation is 3 seconds to 20 seconds.
9. the using method of the double-colored zinc-plated trivalent chromium passivator of environment-friendly type potion according to claim 7, is characterized in that: the time of carrying out passivation is 30 seconds to 50 seconds.
10. the using method of the double-colored zinc-plated trivalent chromium passivator of environment-friendly type potion according to claim 8 or claim 9, is characterized in that: the temperature of carrying out passivation is 5～50 ℃, and the temperature of drying is 50～80 ℃.
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| CN115074186A (en) * | 2022-07-04 | 2022-09-20 | 中化环境修复(上海)有限公司 | Composition for treating hexavalent chromium pollutants, application and method |
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| CN109487255A (en) * | 2018-11-30 | 2019-03-19 | 佛山市海明威生态科技股份有限公司 | A kind of preparation of environment-friendly type galvanized sheet Chrome-free true qualities passivation product |
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