阅读说明：本技术 一种钻石珑珠光颜料的制备方法 (Preparation method of diamond long pearlescent pigment ) 是由 付中华 于 2019-11-30 设计创作，主要内容包括：本发明公开了一种钻石珑珠光颜料的制备方法,包括以下步骤：称取基材15-20kg,加入去离子水至140-160L,调pH至1.4-1.7,升温至58-61℃,得到悬浮液,之后进行如下两层包裹；第一层：在上述悬浮液中同时加入四氯化锡溶液9-12.6L和氯化钠溶液1.5-2.7L,所述四氯化锡溶液的浓度为0.12-0.15mol/L,所述氯化钠溶液的浓度为0.08-0.14mol/L,搅拌20min,升温至75℃,调pH至1.8-2.1；第二层：包括以下步骤：在第一层悬浮液中加入四氯化钛溶液溶液,加至银白、干涉金、干涉红、干涉紫、干涉蓝或干涉绿时停止,过滤、洗涤、烘干、煅烧,得到钻石珑珠光颜料,本发明制备成本低廉,制备产物反射率高。(The invention discloses a preparation method of diamond long pearlescent pigment, which comprises the following steps: weighing 15-20kg of base material, adding deionized water to 140-160L, adjusting the pH value to 1.4-1.7, heating to 58-61 ℃ to obtain a suspension, and then wrapping the suspension by the following two layers; a first layer: adding 9-12.6L of stannic chloride solution and 1.5-2.7L of sodium chloride solution into the suspension at the same time, wherein the concentration of the stannic chloride solution is 0.12-0.15mol/L, the concentration of the sodium chloride solution is 0.08-0.14mol/L, stirring for 20min, heating to 75 ℃, and adjusting the pH to 1.8-2.1; a second layer: the method comprises the following steps: and adding a titanium tetrachloride solution into the first layer of suspension, stopping adding until silver white, interference gold, interference red, interference purple, interference blue or interference green, filtering, washing, drying and calcining to obtain the diamond long pearlescent pigment.)

1. A preparation method of diamond long pearlescent pigment is characterized by comprising the following steps:

weighing 15-20kg of base material, adding deionized water to 140-160L, adjusting the pH value to 1.4-1.7, heating to 58-61 ℃ to obtain a suspension, and then wrapping the suspension by the following two layers;

a first layer: adding 9-12.6L of stannic chloride solution and 1.5-2.7L of sodium chloride solution into the suspension at the same time, wherein the concentration of the stannic chloride solution is 0.12-0.15mol/L, the concentration of the sodium chloride solution is 0.08-0.14mol/L, stirring for 20min, heating to 75 ℃, and adjusting the pH to 1.8-2.1;

A second layer: the method comprises the following steps: and adding a titanium tetrachloride solution into the first layer of suspension, stopping adding until silver white, interference gold, interference red, interference purple, interference blue or interference green, filtering, washing, drying and calcining to obtain the diamond long pearlescent pigment.

2. The method as claimed in claim 1, wherein the substrate is glass flake.

3. The method according to claim 1, wherein said diamond pearlescent pigment has a particle size of 40-400 μm.

4. The method according to claim 1, wherein the tin tetrachloride solution has a flow rate of 60mL/min to 70mL/min, and the sodium chloride solution has a concentration of 10 mL/min to 15 mL/min.

5. The method as claimed in claim 1, wherein the calcination temperature is 550-600 ℃.

6. The method of claim 1, wherein the titanium tetrachloride has a concentration of 0.9 to 1.1mol/L and a flow rate of 45 to 50 ml/min.

7. The method for preparing diamond long pearlescent pigment according to claim 1, wherein the diamond long pearlescent pigment comprises the following components in percentage by mass: 67-95% of base material, 3-31% of titanium dioxide, 0.7-0.9% of stannic oxide and 0.1-0.3% of sodium chloride.

8. The method according to claim 1, wherein the pH is lowered by hydrochloric acid solution, and the pH is raised by sodium hydroxide solution.

Technical Field

The invention belongs to the technical field of pigments, and particularly relates to a preparation method of diamond long pearlescent pigment.

Background

Pearlescent pigments are used as special effect pigments, and are increasingly applied in many industrial fields due to unique and elegant gloss and soft or glittering appearance effects caused by different colors and particle sizes, wherein diamond pearlescent pigments have glittering luster like diamonds, are insoluble in water and harmless to human bodies, can be contacted with skin and food, and are widely applied to special fields such as cosmetics and food packaging.

The Chinese patent application with publication number CN102876090A discloses a preparation method of pearlescent pigment for enhancing interference effect, which at least comprises the following steps: forming at least one crystal form transformation promoter layer on the surface of the substrate or the metal oxide coating layer thereof, wherein the crystal form transformation promoter is SnO2 or hydrated SnO 2; the weight percentage of the dehydrated SnO2 and the substrate in the finished product is 10-20%, the coating rate is 20-70%, when the calcining temperature is higher than 700 ℃, the metallic oxide pigment is calcined at high temperature, most or all of the crystal structure of the coated oxide is converted, and the coated oxides of various different crystal forms generate different refractive indexes, so that the pearlescent pigment with the interference enhancement effect is prepared, the invention adds a crystal form conversion promoter SnO2 layer in the coating process to enhance the interference effect, the prepared pearlescent pigment has the effect of changing color along with the angle, the brightness and the chromaticity are greatly improved, the process is easier to operate, but due to the more content of Sn in the crystal form conversion promoter, although the phase transition temperature of the metallic oxide pigment such as TiO2 can be obviously reduced, the thickness of the TiO2 after phase transition is small, the coverage rate is low, and the overall light reflectivity is low, the color is more vivid but does not give a brilliant diamond-like texture.

Chinese patent with publication number CN104231675B discloses a preparation method of titanium series crystal effect pigment, which comprises the following steps: preparing suspension and preparing a precursor; preparing the series of precursors; and (3) calcining: washing and drying the obtained precursor, and calcining at 775-785 ℃ to obtain titanium series crystal effect pigments; before precursor preparation, suspension is prepared, acid is adjusted, temperature is raised, solution concentration, pH value and temperature are strictly controlled within a certain range, especially before reaction, temperature is well controlled, and reaction speed and pigment accumulation effect can be improved to a certain extent; when the pH is adjusted to 1.5 and the temperature is raised to 62-67 ℃, the effect is particularly prominent; the particle size of the synthetic mica is 10-100 meshes, the required technical effect can be achieved, but the phase change promoter only contains tin dioxide, the phase change time of titanium dioxide is long, and the cost is high.

Disclosure of Invention

In view of the above, the present invention aims to provide a method for preparing diamond long pearlescent pigment, which has low preparation cost and high reflectivity of the prepared product, aiming at the defects of the prior art.

In order to achieve the purpose, the invention adopts the following technical scheme:

A preparation method of diamond long pearlescent pigment comprises the following steps:

weighing 15-20kg of base material, adding deionized water to 140-160L, adjusting the pH value to 1.4-1.7, heating to 58-61 ℃ to obtain a suspension, and then wrapping the suspension by the following two layers;

a first layer: adding 9-12.6L of stannic chloride solution and 1.5-2.7L of sodium chloride solution into the suspension at the same time, wherein the concentration of the stannic chloride solution is 0.12-0.15mol/L, the concentration of the sodium chloride solution is 0.08-0.14mol/L, stirring for 20min, heating to 75 ℃, and adjusting the pH to 1.8-2.1;

a second layer: the method comprises the following steps: and adding a titanium tetrachloride solution into the first layer of suspension, stopping adding until silver white, interference gold, interference red, interference purple, interference blue or interference green, filtering, washing, drying and calcining to obtain the diamond long pearlescent pigment.

Further, the base material is glass flake.

Furthermore, the particle size of the diamond long pearlescent pigment is 40-400 μm.

Further, the flow rate of the stannic chloride solution is 60mL/min-70mL/min, and the concentration of the sodium chloride solution is 10-15 mL/min.

Further, the calcination temperature is 550-600 ℃.

Furthermore, the concentration of the titanium tetrachloride is 0.9-1.1mol/L, and the flow rate is 45-50 ml/min.

Further, the diamond long pearlescent pigment comprises the following components in percentage by mass: 67-95% of base material, 3-31% of titanium dioxide, 0.7-0.9% of stannic oxide and 0.1-0.3% of sodium chloride.

Furthermore, hydrochloric acid solution is adopted for adjusting the pH value to be low, and sodium hydroxide solution is adopted for adjusting the pH value to be high.

The titanium dioxide can be gradually changed to rutile type under the condition of high-temperature firing, but the change temperature is high, the change time is long, the energy consumption is huge, in order to save cost, zinc chloride is usually added in the current production process, the zinc chloride is changed into zinc dioxide in the high-temperature firing process, the zinc dioxide and tin dioxide are jointly used as phase change promoters, because the zinc ion is divalent positive ion, the titanium ion in the titanium dioxide is tetravalent ion, after various zinc ions are introduced, in order to keep charge balance, oxygen anion vacancy can be generated, the migration rate of the oxygen ion with larger radius in the solid phase reaction can be accelerated, the rapid crystal form change is very favorable for realizing, the phase change temperature can be reduced, the phase change time is reduced, the sodium ion in the sodium chloride is monovalent and monovalent, the chemical valence difference with the titanium ion is larger, the oxygen anion is easy to move too fast, the crystal nucleus structure is disturbed, the crystal transformation of titanium dioxide is affected, so that the addition of sodium chloride as a phase transition promoter is not easily conceivable to those skilled in the art.

The invention has the beneficial effects that:

1. the diamond long pearlescent pigment prepared by the invention adopts the glass flakes, has excellent corrosion resistance and good permeability resistance, is beneficial to uniform adhesion of tin tetrachloride, sodium chloride and titanium chloride, and has uniform color and luster.

2. The content of titanium dioxide in the product is high, the thickness of the rutile titanium dioxide after calcination is large, the covering rate is high, the integral light reflection rate of the product is high, and the glossiness is better.

3. The sodium chloride and the tin dioxide are jointly used as phase change accelerators, so that the dosage of the tin dioxide is greatly reduced while the crystal forming effect is not influenced, the required calcining time is shortened, the calcining temperature is reduced, and the cost is saved; and the sodium chloride and the stannic oxide are jointly used as the phase change accelerant, so that the sintering of the titanium dioxide can be prevented, and the color development quality of the product is ensured.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.