CN109266042B - Preparation method of pure silver crystal pearlescent pigment - Google Patents
Preparation method of pure silver crystal pearlescent pigment Download PDFInfo
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Abstract
The invention provides a preparation method of a pure silver crystal pearlescent pigment, and relates to the technical field of pigments. The method takes glass flakes as a base material, and sequentially carries out pretreatment, sensitization treatment, activation treatment and surface plating on the base material, wherein the pretreatment of the base material is carried out according to the following steps: step S101: taking 5-7 g of sodium carbonate, adding 16-23 ml of absolute ethyl alcohol, adding distilled water to dilute to 2L, putting 120g of a base material with the particle size of 40-200 mu m in the sodium carbonate, stirring for 30-40 min, and washing with distilled water to be neutral; step S102: and (4) adding 2-4 ml of hydrochloric acid into 4-6 g of ammonium fluoride, adding distilled water to dilute to 1.5L, placing the base material treated in the step S101 into the mixture, stirring for 30-40 min, and washing the mixture to be neutral by using the distilled water. The pure silver crystal pearlescent pigment prepared by the preparation method provided by the invention is easy to control in quality stability, and has excellent weather resistance and high temperature resistance.
Description
Technical Field
The invention relates to the technical field of pigments, in particular to a preparation method of a pure silver crystal pearlescent pigment.
Background
The pearlescent pigment has the glittering effect of metallic pigment and can generate the soft color of natural pearl, and the glittering effect is passively luminous, namely the glittering effect can be displayed under the condition of light. The main types of pearlescent pigments are: natural fish scale pearlescent pigment, bismuth oxychloride crystalline pearlescent pigment and mica coated pearlescent pigment. The pearlescent pigments, which are currently produced most and most widely used in the world, are core natural mica flakes (mica ranging in size from 4m to 120m and approximately 0.5m thick), coated with one or more layers of titanium or other metal oxides by a special chemical process. However, natural mica, as a substrate material of pearlescent pigment, has the defects that although mica sheets can obtain smaller thickness and larger diameter-thickness ratio (generally required to be more than 50), the mica sheets usually have wider thickness distribution range (0.2-1 μm), which easily affects the stability of coating films, uniform-hue pearlescent pigments are not easy to prepare, when the mica sheets are coated with metal oxides, light is scattered due to layer steps and edge gradient thickness formed by peeling mica, the pearlescent effect is reduced, and in addition, the natural mica also contains colored impurity ions such as iron ions, and the impurity ions are required to be removed by adopting a pretreatment process.
Patent publication No. CN101517011A discloses a synthetic mica-based pearlescent pigment containing ferrite, which is prepared by using synthetic mica as a substrate and subjecting the calcined ferrite coating to surface treatment to stabilize the reflectance and chromaticity of the pearlescent pigment. However, the method is only suitable for synthesizing mica, and two coupling agents of epoxy silane and amino silane are required to be added in the post-treatment process, thereby increasing the production cost of the product.
Patent document No. CN103502364A discloses a method for producing silver (Ag) plating pigments. The method for producing silver-plated pigment according to the present invention comprises: a step of forming a tin compound pretreatment layer on the surface of the substrate; and a step of forming a silver plated layer on a lower portion of the tin compound pre-treatment layer by a reflow and electroless plating process using a diluted silver nitrate solution, ammonia water, a citric acid solution, and a diluted potassium hydroxide solution. The silver pigment prepared by the invention has higher performance in brightness, glossiness and chroma than the coating pigment produced by the traditional electroless plating method, but has poorer weather resistance and high temperature resistance, and the preparation method has complicated steps and is difficult to control.
Disclosure of Invention
In view of the above, the technical problem to be solved by the present invention is to provide a method for preparing a pure silver crystal pearlescent pigment, wherein the obtained pure silver crystal pearlescent pigment has the advantages of easy quality stability control, and excellent weather resistance and high temperature resistance.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
the preparation method of the pure silver crystal pearlescent pigment comprises the following steps of sequentially carrying out pretreatment, sensitization treatment, activation treatment and surface plating on a base material by using glass flakes as the base material:
step S101: taking 5-7 g of sodium carbonate, adding 16-23 ml of absolute ethyl alcohol, adding distilled water to dilute to 2L, putting 120g of a base material with the particle size of 40-200 mu m in the sodium carbonate, stirring for 30-40 min, and washing with distilled water to be neutral;
step S102: and (4) adding 2-4 ml of hydrochloric acid into 4-6 g of ammonium fluoride, adding distilled water to dilute to 1.5L, placing the base material treated in the step S101 into the mixture, stirring for 30-40 min, and washing the mixture to be neutral by using the distilled water.
Preferably, the temperature of the stirring in step S101 is 25 ℃.
Preferably, the sensitization treatment is specifically: taking 1-3 g of stannous chloride, adding 15-25 ml of hydrochloric acid, diluting with soft water to 1L, putting the base material treated in the step S102 in the diluted solution, adjusting the pH value to 2.0, stirring for 1-1.2 h, and washing with distilled water to be neutral.
Preferably, the stirring temperature in the sensitization treatment is 25 ℃.
Preferably, the activation treatment is specifically: 1-1.4 g of silver nitrate is taken, distilled water is added to dilute the silver nitrate to 1L, then diluted ammonia water with the mass volume ratio g/ml of 4.8% -5.2% is dripped to generate tawny precipitate, the dropwise addition is continued until the precipitate just disappears, the sensitized base material is placed in the solution, the stirring is carried out for 1-1.2 h, and the solution is washed by distilled water and dried.
Preferably, the stirring temperature in the activation treatment is 25 ℃.
Preferably, the surface plating is in particular: and (3) placing the activated substrate in a silver ammonia solution, controlling the temperature at 4-9 ℃, stirring at a low speed, then adding a glucose solution at a constant speed until the substrate is coated with silver, washing and drying.
Preferably, the preparation method of the silver ammonia solution comprises the following steps: and (3) adding distilled water into 8.2-8.6 g of silver nitrate to dilute to 2L, and then dropwise adding dilute ammonia water with the mass-volume ratio g/ml of 4.8-5.2% to generate a tawny precipitate.
Preferably, the preparation method of the glucose solution comprises the following steps: taking 12-13 g of glucose, adding distilled water to dissolve and dilute to 1.2L.
Preferably, the drying temperature in the surface plating is 100-110 ℃.
Compared with the prior art, the invention has the following beneficial effects:
the glass base material is prepared by pretreating the glass flakes, so that impurities contained in the glass flakes can be effectively removed, the surface smoothness and the glossiness of the glass base material are improved, and the film coating quality of the glass base material is improved. The method comprises the following steps of firstly cleaning the glass flakes by using an alkaline solution, wherein the alkaline solution is prepared by adding ethanol into a certain amount of sodium carbonate and then diluting the sodium carbonate by using distilled water; secondly, the glass flakes are coarsened by adopting an acid solution, the acid solution is obtained by diluting a certain amount of ammonium fluoride and hydrochloric acid with distilled water, and through the treatment, the surface impurities of the glass flakes are fully removed, and meanwhile, the surfaces of the glass flakes form proper surface morphology, so that the smooth proceeding of the subsequent treatment process is facilitated, and the guarantee is provided for improving the stability and the high temperature resistance of the silver pigment.
The method comprises the steps of carrying out sensitization treatment and activation treatment on a pretreated glass flake substrate in sequence, wherein the sensitization treatment adopts a mixed solution of stannous chloride and hydrochloric acid with a certain proportion, so that a tin compound pretreatment layer is formed on the surface of the substrate, and on one hand, expensive metal compounds such as PdCl are not used2On the other hand, the mixed solution of stannous chloride and hydrochloric acid with a specific ratio is beneficial to forming a stannic compound pretreatment layer with a proper thickness, improves the adhesive property of the silver coating and ensures that the stability and the weather resistance of the silver coating are better; the activation treatment adopts silver nitrate solution to activate the base material, thereby forming a silver coating with proper thickness on the surface of the base material and improving the efficiency and quality of surface plating. The surface of the base material is plated with silver after the pretreatment, the sensitization and the activation, in the plating process, the proper stirring speed and the reaction temperature need to be controlled, the stirring speed is proper and slow, specifically, the stirring speed can be set to be not higher than 100r/min (not more than 100 r/min), the stirring speed is too high, the uniform and stable silver coating is not easy to form, the reaction temperature cannot be higher than 10 ℃, and the silver coating cannot be normally formed when the reaction temperature is higher than the temperature; the glucose solution is preferably added at a constant speed, and the adding speed is preferably 10-40 ml/min, so that a more stable silver coating is formed by controlling a proper reaction speed.
According to the invention, through strict control on the treatment process, the processes can be effectively linked and cooperatively matched, so that the silver pearlescent pigment with good stability, weather resistance and high temperature resistance is produced, and the quality of the silver pearlescent pigment is improved.
Detailed Description
In order to better understand the present invention, the following examples are further provided to clearly illustrate the contents of the present invention, but the contents of the present invention are not limited to the following examples. In the following description, numerous specific details are set forth in order to provide a more thorough understanding of the present invention. It will be apparent, however, to one skilled in the art, that the present invention may be practiced without one or more of these specific details.
Example 1
A preparation method of pure silver crystal pearlescent pigment takes glass flakes as a base material, and sequentially carries out pretreatment, sensitization treatment, activation treatment and surface plating on the base material, and specifically comprises the following steps:
1) pretreating a base material:
step S101: taking 6g of sodium carbonate, adding 20ml of absolute ethyl alcohol, adding distilled water to dilute to 2L, placing 120g of a 40-micron base material in the solution, stirring for 30min at 25 ℃, and washing with distilled water to be neutral;
step S102: taking 5g of ammonium fluoride, adding 3ml of hydrochloric acid, adding distilled water to dilute to 1.5L, placing the base material treated in the step S101 in the solution, stirring for 30min at 25 ℃, and washing the solution to be neutral by using distilled water;
2) sensitization treatment: taking 2g of stannous chloride, adding 20ml of hydrochloric acid, diluting the stannous chloride with soft water to 1L, placing the base material treated in the step S102 in the diluted base material, adjusting the pH value to 2.0, stirring the base material at 25 ℃ for 1h, and washing the base material to be neutral by distilled water;
3) activation treatment: taking 1.2g of silver nitrate, adding distilled water to dilute the silver nitrate to 1L, then dropwise adding dilute ammonia water with the mass-volume ratio g/ml of 5% to generate a tawny precipitate, continuously dropwise adding the precipitate until the precipitate just disappears, placing the sensitized substrate in the solution, stirring the solution at 25 ℃ for 1 hour, washing the solution with distilled water, and drying the solution;
4) surface plating: placing the activated substrate in a silver ammonia solution, controlling the temperature at 5.8 ℃, stirring at a slow speed, then adding a glucose solution at a constant speed until the substrate is coated with silver, washing, and drying at 105 ℃;
the preparation method of the silver-ammonia solution comprises the following steps: adding distilled water into 8.4g of silver nitrate to dilute the silver nitrate to 2L, and then dropwise adding dilute ammonia water with the mass volume ratio of g/ml being 5% to generate a tawny precipitate; the preparation method of the glucose solution comprises the following steps: taking 12.6g of glucose, adding distilled water to dissolve and dilute the glucose to 1.2L;
the rotation speed of the slow stirring is 30r/min, and the speed of the uniform adding is 30 ml/min.
Example 2
A preparation method of pure silver crystal pearlescent pigment takes glass flakes as a base material, and sequentially carries out pretreatment, sensitization treatment, activation treatment and surface plating on the base material, and specifically comprises the following steps:
1) pretreating a base material:
step S101: taking 5g of sodium carbonate, adding 16ml of absolute ethyl alcohol, adding distilled water to dilute to 2L, placing 120g of a base material with the particle size of 50 micrometers in the sodium carbonate, stirring for 30min at 25 ℃, and washing with distilled water to be neutral;
step S102: taking 4g of ammonium fluoride, adding 2ml of hydrochloric acid, adding distilled water to dilute to 1.5L, placing the base material treated in the step S101 in the solution, stirring for 32min at 25 ℃, and washing the solution to be neutral by using distilled water;
2) sensitization treatment: taking 1g of stannous chloride, adding 15ml of hydrochloric acid, diluting the stannous chloride with soft water to 1L, putting the base material treated in the step S102 in the diluted base material, adjusting the pH value to 2.0, stirring the base material at 25 ℃ for 1h, and washing the base material to be neutral by distilled water;
3) activation treatment: diluting 1g of silver nitrate with distilled water to 1L, then dropwise adding dilute ammonia water with the mass-volume ratio g/ml of 4.8% to generate a tawny precipitate, continuously dropwise adding the precipitate until the precipitate just disappears, placing the sensitized substrate in the solution, stirring the solution at 25 ℃ for 1 hour, washing the solution with distilled water, and drying the solution;
4) surface plating: placing the activated substrate in a silver ammonia solution, controlling the temperature at 4 ℃, stirring slowly, then adding a glucose solution at a constant speed until the substrate is coated with silver, washing, and drying at 110 ℃;
the preparation method of the silver-ammonia solution comprises the following steps: diluting 8.2g of silver nitrate with distilled water to 2L, and then dropwise adding dilute ammonia water with the mass-volume ratio g/ml of 4.8% to generate a yellow brown precipitate; the preparation method of the glucose solution comprises the following steps: taking 12g of glucose, adding distilled water to dissolve and dilute the glucose to 1.2L;
the rotation speed of slow stirring is 50r/min, and the speed of constant adding is 25 ml/min.
Example 3
A preparation method of pure silver crystal pearlescent pigment takes glass flakes as a base material, and sequentially carries out pretreatment, sensitization treatment, activation treatment and surface plating on the base material, and specifically comprises the following steps:
1) pretreating a base material:
step S101: taking 7g of sodium carbonate, adding 23ml of absolute ethyl alcohol, adding distilled water to dilute to 2L, putting 120g of a substrate with the size of 80 mu m in the solution, stirring for 40min at 25 ℃, and washing with distilled water to be neutral;
step S102: taking 6g of ammonium fluoride, adding 4ml of hydrochloric acid, adding distilled water to dilute to 1.5L, placing the base material treated in the step S101 in the solution, stirring for 35min at 25 ℃, and washing the solution to be neutral by using distilled water;
2) sensitization treatment: taking 3g of stannous chloride, adding 25ml of hydrochloric acid, diluting the mixture to 1L with soft water, placing the base material treated in the step S102 in the mixture, adjusting the pH value to 2.0, stirring the mixture at 25 ℃ for 1.2h, and washing the mixture to be neutral by distilled water;
3) activation treatment: taking 1.4g of silver nitrate, adding distilled water to dilute the silver nitrate to 1L, then dropwise adding dilute ammonia water with the mass-volume ratio g/ml of 5.2% to generate a tawny precipitate, continuously dropwise adding the precipitate until the precipitate just disappears, placing the sensitized substrate in the substrate, stirring the substrate for 1.2 hours at 25 ℃, washing the substrate with distilled water, and drying the substrate;
4) surface plating: placing the activated substrate in a silver ammonia solution, controlling the temperature at 9 ℃, stirring slowly, then adding a glucose solution at a constant speed until the substrate is coated with silver, washing, and drying at 105 ℃;
the preparation method of the silver-ammonia solution comprises the following steps: diluting 8.6g of silver nitrate with distilled water to 2L, and then dropwise adding dilute ammonia water with the mass volume ratio g/ml of 5.2% to generate a yellow brown precipitate; the preparation method of the glucose solution comprises the following steps: taking 13g of glucose, adding distilled water to dissolve and dilute the glucose to 1.2L;
the rotation speed of the slow stirring is 20r/min, and the speed of the uniform adding is 40 ml/min.
Example 4
A preparation method of pure silver crystal pearlescent pigment takes glass flakes as a base material, and sequentially carries out pretreatment, sensitization treatment, activation treatment and surface plating on the base material, and specifically comprises the following steps:
1) pretreating a base material:
step S101: taking 5.5g of sodium carbonate, adding 17ml of absolute ethyl alcohol, adding distilled water to dilute to 2L, placing 120g of 120-micron base material in the solution, stirring for 35min at 25 ℃, and washing with distilled water to be neutral;
step S102: taking 4.3g of ammonium fluoride, adding 2.5ml of hydrochloric acid, adding distilled water to dilute to 1.5L, placing the base material treated in the step S101 in the base material, stirring for 40min at 25 ℃, and washing the base material to be neutral by using distilled water;
2) sensitization treatment: taking 1.5g of stannous chloride, adding 16ml of hydrochloric acid, diluting the stannous chloride with soft water to 1L, putting the base material treated in the step S102 in the diluted base material, adjusting the pH value to 2.0, stirring the base material at 25 ℃ for 1.2h, and washing the base material to be neutral by distilled water;
3) activation treatment: taking 1.1g of silver nitrate, adding distilled water to dilute the silver nitrate to 1L, then dropwise adding dilute ammonia water with the mass-volume ratio g/ml of 4.9% to generate a tawny precipitate, continuously dropwise adding the precipitate until the precipitate just disappears, placing the sensitized substrate in the substrate, stirring the substrate for 1 hour at 25 ℃, washing the substrate with distilled water, and drying the substrate;
4) surface plating: placing the activated substrate in a silver ammonia solution, controlling the temperature at 5 ℃, stirring slowly, then adding a glucose solution at a constant speed until the substrate is coated with silver, washing, and drying at 105 ℃;
the preparation method of the silver-ammonia solution comprises the following steps: diluting 8.3g of silver nitrate with distilled water to 2L, and then dropwise adding dilute ammonia water with the mass-volume ratio g/ml of 4.9% to generate a yellow brown precipitate; the preparation method of the glucose solution comprises the following steps: taking 12.3g of glucose, adding distilled water to dissolve and dilute the glucose to 1.2L;
the rotation speed of the slow stirring is 42r/min, and the speed of the uniform adding is 20 ml/min.
Example 5
A preparation method of pure silver crystal pearlescent pigment takes glass flakes as a base material, and sequentially carries out pretreatment, sensitization treatment, activation treatment and surface plating on the base material, and specifically comprises the following steps:
1) pretreating a base material:
step S101: taking 6.5g of sodium carbonate, adding 21ml of absolute ethyl alcohol, adding distilled water to dilute to 2L, placing 120g of 150-micron base material in the solution, stirring for 30min at 25 ℃, and washing with distilled water to be neutral;
step S102: taking 5.5g of ammonium fluoride, adding 3.5ml of hydrochloric acid, adding distilled water to dilute to 1.5L, placing the base material treated in the step S101 in the base material, stirring for 35min at 25 ℃, and washing the base material to be neutral by using distilled water;
2) sensitization treatment: taking 2.5g of stannous chloride, adding 23ml of hydrochloric acid, diluting the stannous chloride to 1L with soft water, placing the base material treated in the step S102 in the diluted base material, adjusting the pH value to 2.0, stirring the base material at 25 ℃ for 1.2h, and washing the base material to be neutral by distilled water;
3) activation treatment: adding 8.5g of silver nitrate into distilled water to dilute the silver nitrate to 1L, then dropwise adding dilute ammonia water with the mass-volume ratio of g/ml being 5.1% to generate a tawny precipitate, continuously dropwise adding the dilute ammonia water until the precipitate just disappears, placing the sensitized substrate in the solution, stirring the solution at 25 ℃ for 1 hour, washing the solution with distilled water, and drying the solution;
4) surface plating: placing the activated substrate in a silver ammonia solution, controlling the temperature at 7.5 ℃, stirring at a slow speed, then adding a glucose solution at a constant speed until the substrate is coated with silver, washing, and drying at 110 ℃;
the preparation method of the silver-ammonia solution comprises the following steps: diluting 8.4g of silver nitrate with distilled water to 2L, and then dropwise adding dilute ammonia water with the mass volume ratio g/ml of 5.1% to generate a yellow brown precipitate; the preparation method of the glucose solution comprises the following steps: taking 12.5g of glucose, adding distilled water to dissolve and dilute the glucose to 1.2L;
the rotation speed of the slow stirring is 70r/min, and the speed of the uniform adding is 10 ml/min.
Example 6
A preparation method of pure silver crystal pearlescent pigment takes glass flakes as a base material, and sequentially carries out pretreatment, sensitization treatment, activation treatment and surface plating on the base material, and specifically comprises the following steps:
1) pretreating a base material:
step S101: taking 6.2g of sodium carbonate, adding 20ml of absolute ethyl alcohol, adding distilled water to dilute to 2L, placing 120g of 200-micron base material in the solution, stirring for 30min at 25 ℃, and washing with distilled water to be neutral;
step S102: taking 5.2g of ammonium fluoride, adding 3ml of hydrochloric acid, adding distilled water to dilute to 1.5L, placing the base material treated in the step S101 in the base material, stirring for 35min at 25 ℃, and washing the base material to be neutral by using distilled water;
2) sensitization treatment: taking 2.3g of stannous chloride, adding 20ml of hydrochloric acid, diluting the stannous chloride to 1L with soft water, putting the base material treated in the step S102 in the diluted base material, adjusting the pH value to 2.0, stirring the base material at 25 ℃ for 1h, and washing the base material to be neutral by distilled water;
3) activation treatment: taking 1.3g of silver nitrate, adding distilled water to dilute the silver nitrate to 1L, then dropwise adding dilute ammonia water with the mass-volume ratio g/ml of 5% to generate a tawny precipitate, continuously dropwise adding the precipitate until the precipitate just disappears, placing the sensitized substrate in the solution, stirring the solution at 25 ℃ for 1 hour, washing the solution with distilled water, and drying the solution;
4) surface plating: placing the activated substrate in a silver ammonia solution, controlling the temperature at 6 ℃, stirring at a low speed, then adding a glucose solution at a constant speed until the substrate is coated with silver, washing, and drying at 105 ℃;
the preparation method of the silver-ammonia solution comprises the following steps: adding distilled water into 8.3g of silver nitrate to dilute the silver nitrate to 2L, and then dropwise adding dilute ammonia water with the mass volume ratio of g/ml being 5% to generate a tawny precipitate; the preparation method of the glucose solution comprises the following steps: taking 12.5g of glucose, adding distilled water to dissolve and dilute the glucose to 1.2L;
the rotation speed of the slow stirring is 35r/min, and the speed of the uniform adding is 32 ml/min.
Comparative example 1
This comparative example describes the preparation of a pure silver crystal pearlescent pigment, which is essentially the same as in example 1, except that the substrate is pretreated as follows:
100g of sodium carbonate is taken, distilled water is added to dilute the sodium carbonate to 2L, 120g of a 40 mu m base material is placed in the sodium carbonate, the mixture is stirred for 30 hours at 25 ℃, and the mixture is washed to be neutral by the distilled water.
Comparative example 2
This comparative example describes the preparation of a pure silver crystal pearlescent pigment, which is essentially the same as in example 1, except that the substrate is pretreated as follows:
diluting 45g hydrofluoric acid with distilled water to 1.5L, placing 40 μm substrate therein, stirring at 25 deg.C for 40min, and washing with distilled water to neutral.
Comparative example 3
This comparative example describes the preparation of a pure silver crystal pearlescent pigment, which is essentially the same as in example 1, except that the substrate is pretreated as follows:
step S101: taking 100g of sodium carbonate, adding distilled water to dilute the sodium carbonate to 2L, placing 120g of a 40-micron base material in the sodium carbonate, stirring the mixture for 30 hours at 25 ℃, and washing the mixture to be neutral by using the distilled water;
step S102: 5g of ammonium fluoride is taken, 3ml of hydrochloric acid is added, distilled water is added for dilution to 1.5L, the substrate treated in the step S101 is placed in the solution, the solution is stirred for 30min at 25 ℃, and the solution is washed to be neutral by distilled water.
Comparative example 4
The comparative example describes a process for preparing a pure silver crystal pearlescent pigment, which is substantially the same as example 1, except that:
the activation treatment step is omitted, and the sensitized substrate is directly subjected to surface plating.
Evaluation of Effect
1. The pretreated glass flakes of example 1, comparative example 1 to comparative example 3 were subjected to subsequent treatments such as filtration, washing, drying, and the like, and finally calcined at 550 ℃ for 2 hours, and the whiteness of the obtained glass flakes was measured by a whiteness meter, as shown in the following table:
as can be seen from table 1, the bead brightness of the pearlescent pigment is finally affected by different degrees of impurity removal and erosion on the surface of the glass flake by different pretreatment methods, wherein the pretreatment effect of embodiment 1 of the present invention is the best, and the surface impurities of the glass flake can be well removed, so that the bead brightness of the pearlescent pigment is improved. The effect of comparative example 3 is inferior, but is superior to that of comparative examples 1 and 2, which shows that the pretreatment effect is better by combining the two modes of cleaning with the alkaline solution and coarsening with the acidic solution, and the final effect of the pretreatment is influenced by the concentration of the alkaline solution, the cleaning temperature and the property of the acidic solution. The pretreatment method adopted by the invention has mild conditions (both at room temperature of 25 ℃), obviously lower concentration of the alkali solution and the acid solution, less material input cost, reduced corrosion to equipment and obviously improved pretreatment effect.
2. The products obtained in example 1 of the present invention and comparative examples 1 to 4 were subjected to a weather resistance test, respectively
The weather resistance test adopts a xenon lamp laboratory accelerated aging test, products obtained in the example 1 and the comparative examples 1-4 are made into weather resistance test sample plates, the weather resistance test sample plates are operated for 2000 hours according to the test conditions in the table 1, the evaluation interval period is 500 hours, and whether the silver pearlescent pigment has the phenomena of light loss, chalking, discoloration and yellowing or not is visually observed.
TABLE 1 xenon lab accelerated test procedure parameters
As a result: the pearlescent pigment obtained in the embodiment 1 of the invention has the advantages of no pulverization, no discoloration, no yellowing and obvious weather resistance; comparative examples 1 to 4 have discoloration, yellowing and/or chalking phenomena of different degrees, and the weather resistance is reduced compared with that of example 1.
In order to further confirm that the sample under the process condition has remarkable weather resistance, weather resistance comparison experiments are carried out on the products obtained in the example 1 and the comparative examples 1-4. Under the same conditions, the products obtained in example 1 and comparative examples 1 to 4 were made into weather resistance test specimens, which were put into an accelerated aging xenon lamp box to undergo accelerated aging tests, and the results are shown in Table 2 (O-no powdering; -slight powdering;. X-powdering).
TABLE 2 weather resistance comparative test results
The results show that the pretreatment method of the glass flake substrate is proper, and the sensitization and the activation treatment are adopted in sequence, so that the weather resistance of the pearlescent pigment is obviously enhanced.
3. The products obtained in the example 1 of the invention and the comparative examples 1 to 4 were respectively subjected to a high temperature resistance test
The high temperature resistance test method comprises the following steps: calcining the products obtained in the example 1 and the comparative examples 1-4 at 800 ℃ for 20min, 40min, 60min and 80min in sequence, observing the products through a scanning electron microscope image, and recording the time points of obvious cracks of the products.
The result shows that the surface of the product of the invention has obvious cracks in 80min under the condition of high temperature of 800 ℃, while the surface of the product obtained in comparative examples 1-4 has obvious cracks in 40min, 60min and 20 min.
In combination with the tests, the preparation method of the pure silver crystal pearlescent pigment is an improvement of the existing preparation method, compared with the existing preparation method, the reaction condition is milder, the production cost is lower, the weather resistance and the high temperature resistance of the obtained product are more remarkable, and the quality stability is higher.
Finally, the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting, and other modifications or equivalent substitutions made by the technical solutions of the present invention by those of ordinary skill in the art should be covered within the scope of the claims of the present invention as long as they do not depart from the spirit and scope of the technical solutions of the present invention.
Claims (7)
1. The preparation method of the pure silver crystal pearlescent pigment takes glass flakes as a base material and is characterized in that the base material is sequentially subjected to pretreatment, sensitization treatment, activation treatment and surface plating, and the preparation method specifically comprises the following steps:
1) pretreating a base material:
step S101: taking 5-7 g of sodium carbonate, adding 16-23 ml of absolute ethyl alcohol, adding distilled water to dilute to 2L, putting 120g of a base material with the particle size of 40-200 mu m in the sodium carbonate, stirring for 30-40 min, and washing with distilled water to be neutral;
step S102: taking 4-6 g of ammonium fluoride, adding 2-4 ml of hydrochloric acid, adding distilled water to dilute to 1.5L, placing the base material treated in the step S101 in the base material, stirring for 30-40 min, and washing the base material to be neutral by using the distilled water;
2) sensitization treatment:
taking 1-3 g of stannous chloride, adding 15-25 ml of hydrochloric acid, diluting with soft water to 1L, putting the base material treated in the step S102 in the diluted soft water, adjusting the pH value to 2.0, stirring for 1-1.2 h, and washing with distilled water to be neutral;
3) activation treatment:
1-1.4 g of silver nitrate is taken, distilled water is added to dilute the silver nitrate to 1L, then dilute ammonia water with the mass volume ratio g/ml of 4.8% -5.2% is dripped to generate tawny precipitate, the dropwise addition is continued until the precipitate just disappears, the sensitized base material is placed in the solution, the stirring is carried out for 1-1.2 h, and the solution is washed by distilled water and dried;
4) surface plating:
and (3) placing the activated substrate in a silver ammonia solution, controlling the temperature at 4-9 ℃, stirring at a low speed, then adding a glucose solution at a constant speed until the substrate is coated with silver, washing and drying.
2. The method of preparing a pure silver crystal pearlescent pigment according to claim 1, wherein: the stirring temperature in step S101 is 25 ℃.
3. The method of preparing a pure silver crystal pearlescent pigment according to claim 2, characterized in that: the stirring temperature in the sensitization treatment was 25 ℃.
4. The method of preparing a pure silver crystal pearlescent pigment according to claim 3, characterized in that: the stirring temperature in the activation treatment was 25 ℃.
5. The method of preparing a pure silver crystal pearlescent pigment according to claim 4, characterized in that: the preparation method of the silver ammonia solution comprises the following steps: and (3) adding distilled water into 8.2-8.6 g of silver nitrate to dilute to 2L, and then dropwise adding dilute ammonia water with the mass-volume ratio of 4.8-5.2 g/ml to generate a tawny precipitate.
6. The method of preparing a pure silver crystal pearlescent pigment according to claim 5, wherein: the preparation method of the glucose solution comprises the following steps: taking 12-13 g of glucose, adding distilled water to dissolve and dilute to 1.2L.
7. The method of preparing a pure silver crystal pearlescent pigment according to claim 6, characterized in that: the drying temperature in the surface plating is 100-110 ℃.
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