A dry-process compounded green pigment and its production process
By using a dry compounding process with specific raw materials and equipment, the problems of long processing time and poor dispersibility in the production of green pigments have been solved, achieving efficient and low-cost pigment preparation and improving the dispersibility and weather resistance of pigments.
Patent Information
- Application Number
- CN202310677159.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-06-08
- Publication Date
- 2026-01-30
- Estimated Expiration
- 2043-06-08
AI Technical Summary
In existing green pigment production processes, wet processes are time-consuming and costly, while dry processes produce pigments with large particle size, poor dispersibility and weather resistance, which affect the coloring effect.
A dry compounding process is adopted, using calcium carbonate, talc, iron oxide yellow, phthalocyanine blue and additives (wetting agent, dispersant and emulsifier) as raw materials. After premixing in a biaxial cone mixer, the mixture is kneaded in a ball mill, and the temperature and pressure are controlled. The mixture is then further pulverized to obtain a pigment with a particle size of less than 800 mesh.
It improves the dispersibility, hydrophilicity, and weather resistance of pigments, enhances tinting strength and color, and reduces production costs.
Abstract
Description
TECHNICAL FIELD
[0001] The present application belongs to the field of pigments and its production technology, and particularly relates to a dry-compounded green pigment and a production process thereof. BACKGROUND
[0002] Pigment refers to a substance capable of dyeing an object, and can be soluble pigment and insoluble pigment, inorganic pigment and organic pigment. Inorganic pigment is generally mineral substance, and organic pigment is generally obtained from plants and marine animals, such as alizarin blue, gamboge and purple extracted from shellfish.
[0003] Green pigment is commonly used for coloring cement base court, resin-based sports ground and water-permeable road. The existing green pigments are mostly produced by wet process and dry process. The wet process is to disperse raw material powder in solvent such as ethanol, and to obtain the pigment by repeated rinsing, filtering and drying, which takes a long time and consumes a large amount of solvent, resulting in high production cost. The dry process is to mechanically mix raw material powder by high-speed mixer, but the pigment prepared by mixing has large particle size, and has poor dispersibility and weather resistance in actual use, which affects the coloring effect. SUMMARY
[0004] The present application provides a dry-compounded green pigment and a production process thereof, and aims to solve the above technical problems.
[0005] The present application is implemented as follows. A dry-compounded green pigment is prepared by dry-compounding, and comprises the following raw materials in percentage by weight: body material 40-50%, iron oxide yellow 45-51%, phthalocyanine blue 4-6%, and auxiliary agent 1-3%.
[0006] Further, the body material comprises calcium carbonate and talcum powder.
[0007] Further, the weight ratio of calcium carbonate to talcum powder in the body material is 2:1.
[0008] Further, the auxiliary agent comprises wetting agent, dispersant and emulsifier.
[0009] Further, the weight ratio of wetting agent, dispersant and emulsifier is 1:1:1.
[0010] Further, the wetting agent is one of fatty alcohol polyoxyethylene ether, coconut oil acid diethanol amide, octylphenol polyoxyethylene ether, fatty acid polyoxyethylene ester and alkylphenol polyoxyethylene ester, the dispersant is trimethylolpropane, and the emulsifier is dodecylphenol polyoxyethylene ether or nonylphenol polyoxyethylene ether.
[0011] Further, the raw materials include, by weight percentage, body material 45%, iron oxide yellow 48%, phthalocyanine blue 5%, and auxiliary agent 2%.
[0012] Further, the raw materials further include, by weight percentage, iron oxide red 0.5-0.8%.
[0013] Further, the raw materials include, by weight percentage, body material 45%, iron oxide yellow 47.3%, phthalocyanine blue 4.9%, iron oxide red 0.8%, and auxiliary agent 2%.
[0014] The application further provides a production process of the dry compounded green pigment, comprising the following steps:
[0015] Each raw material is weighed by weight percentage;
[0016] Each raw material except the auxiliary agent is put into a double-shaft conical mixer and mixed for 3-5 min to obtain a premix;
[0017] The premix is put into a ball mill and kneaded for 5-7 h, with the temperature controlled at 55-60 DEG C and the pressure controlled below 1.5 atm to obtain a raw mixed powder;
[0018] The auxiliary agent is added to the raw mixed powder and the mixture is continuously kneaded in the ball mill for 2-3 h, with the temperature controlled at 55-60 DEG C and the pressure controlled below 1.5 atm to obtain a cooked mixed powder;
[0019] The cooked mixed powder is sieved by a vibrating screen and then put into a pulverizer to be pulverized to obtain the dry compounded green pigment.
[0020] Advantages
[0021] In the dry compounded green pigment provided by the application, the body material in the pigment includes talcum powder, which can effectively increase the flowability of other raw materials in the stirring and mixing and ball milling process, so that the raw materials are mixed more fully. The wetting agent, dispersing agent and emulsifier in the auxiliary agent can coat the membranes of particles of each raw material in the ball milling process, improve the dispersibility between inorganic raw materials and organic raw materials, and thus improve the weather resistance, color and coloring power of the pigment. In the production process, the two-step mixing procedure of premixing by the double-shaft conical mixer and ball milling kneading increases the uniformity of the mixture of each raw material, and the modification with the auxiliary agent can solve the dispersibility problem between inorganic raw materials and organic raw materials, and further reduce the particle size of the green pigment. The particle size of the finished product is above 800 mesh, and the finished product has good hydrophilicity, dispersibility, weather resistance, color and coloring power. DETAILED DESCRIPTION
[0022] The raw materials of the dry compounded green pigment provided by the application include body material, iron oxide yellow, phthalocyanine blue and auxiliary agent. The body material includes calcium carbonate and talcum powder, the calcium carbonate is base material, and the talcum powder is used to improve the fluidity of the system in the ball milling process and improve the mixing effect of the raw materials. The auxiliary agent includes wetting agent, dispersant and emulsifier, the wetting agent is one of fatty alcohol polyoxyethylene ether, coconut oil acid diethanol amide, octyl phenol polyoxyethylene ether, fatty acid polyoxyethylene ester and alkyl phenol polyoxyethylene ester, the dispersant is trimethylolpropane, the wetting agent and the dispersant are coated on the surface of the particles of the calcium carbonate, the talcum powder, the iron oxide yellow and the phthalocyanine blue, which can improve the mechanical mixing degree between the raw materials, make the raw material mixing more uniform and avoid agglomeration. The emulsifier is dodecyl phenol polyoxyethylene ether or nonyl phenol polyoxyethylene ether, which can improve the dispersion effect between the inorganic raw materials calcium carbonate, talcum powder and iron oxide yellow and the organic raw material phthalocyanine blue, so that they are kneaded into multiple whole bodies with smaller particle size in the ball milling process, which is beneficial to improve the color uniformity. The wetting agent, the dispersant and the emulsifier in the auxiliary agent can improve the hydrophilicity, dispersibility and weather resistance of the pigment, and then improve the color, brightness and tinting strength.
[0023] In addition, in order to make the color of the green pigment deeper, a small amount of iron oxide red can be added to the raw materials to increase the green phase effect.
[0024] The application also provides a production process of the dry compounded green pigment, which includes weighing each raw material according to the weight percentage, mixing each raw material except the auxiliary agent in a double-shaft conical mixer to obtain premix, kneading the premix in a ball mill to obtain mixed raw powder, adding the auxiliary agent to the mixed raw powder and continuing to knead in the ball mill to obtain mixed mature powder, screening the mixed mature powder through a vibrating screen and then crushing the mixed mature powder in a crusher to obtain the dry compounded green pigment.
[0025] Each powder raw material is premixed in the double-shaft conical mixer, the self-rotation rate of the double-shaft conical mixer is 26-30 r / min, and the revolution rate is 2.5 r / min. The particle size of the mixed raw material is basically the same as that of the initial raw material. Generally, the particle size of the initial raw material is 315-325 mesh. It can be predicted that the smaller the particle size of the powder raw material, the higher the density of the mutual doping of each raw material, and the closer the fit between the raw material particles. The overall performance of the finished pigment is better, the pigment is not easy to stratify, and the dispersion and tinting strength can be improved when coloring. Therefore, after premixing, the premix is further processed by the ball mill, the particle size of the mixed raw material is reduced to more than 800 mesh, and the auxiliary agent is added during the processing. In this way, the particle size of the raw material particles can be reduced, and the auxiliary agent can be uniformly coated on the surface of the raw material particles, thereby improving the hydrophilicity, weather resistance and color of the pigment.
[0026] The ball milling process controls the temperature at 55-60 DEG C and the pressure is lower than 1.5 atmospheres, if the temperature or pressure is too high, the ball mill stops, the exhaust port is opened to release the gas, and the temperature or pressure is reduced.
[0027] In addition, the production process of the dry compounded green pigment of the present application further comprises the step of variable speed ball milling kneading during the process of putting the premix into the ball mill for kneading for 5-7 hours and adding the auxiliary agent into the mixed raw powder for continuing kneading for 2-3 hours in the ball mill. Taking the example of ball milling for 7 hours before adding the auxiliary agent and ball milling for 3 hours after adding the auxiliary agent, the speed is controlled at 10-15 r / min in the first 0.5 hours to make the premix fully filled into the grinding medium; the speed is controlled at 15-20 r / min in the next 0.5-2 hours to reduce the particle size of the mixed raw material; the speed is controlled at 20-23 r / min in the next 2-4 hours to further reduce the particle size of the mixed raw material; the speed is controlled at 25-26 r / min in the next 4-7 hours to reduce the particle size of the mixed raw material again, and then the machine stops, the auxiliary agent is added, the speed is controlled at 10 r / min in the first 0.5 hours to make the auxiliary agent filled into the grinding medium, and the speed is controlled at 26-28 r / min in the next 0.5-3 hours to make the mixed raw powder fully mixed with the auxiliary agent.
[0028] The mixed finished powder is ground to obtain the dry compounded green pigment, if there are multiple ball mills for production, the dry compounded green pigments produced by the multiple ball mills need to be mixed and ground again to make the color of the same batch of products uniform.
[0029] In order to make the purpose, technical scheme and advantages of the present application more clear, the present application is further described in detail by the following examples. It should be understood that the specific examples described herein are only used to explain the present application, and are not used to limit the present application.
[0030] Example 1
[0031] The example of the present application provides a dry compounded green pigment, which comprises the following raw materials:
[0032] 300 kg of calcium carbonate, 150 kg of talcum powder, 480 kg of yellow iron oxide, 50 kg of phthalocyanine blue and 20 kg of auxiliary agent, the auxiliary agent is composed of fatty alcohol polyoxyethylene ether, trimethylolpropane and dodecyl phenol polyoxyethylene ether in a weight ratio of 1:1:1, and the particle size of the calcium carbonate, talcum powder, yellow iron oxide and phthalocyanine blue is 325 mesh.
[0033] The production process of the dry compounded green pigment comprises the following steps:
[0034] Take calcium carbonate, talcum powder, iron oxide yellow, phthalocyanine blue and auxiliary agent respectively, put calcium carbonate, talcum powder, iron oxide yellow and phthalocyanine blue into double-shaft conical mixer and mix for 5 minutes to obtain premix, put the premix into a ball mill and knead for 7 hours, during which the speed is controlled at 10 r / min for the first 0.5 hours, 15 r / min for 0.5-2 hours, 20 r / min for 2-4 hours, 25 r / min for 4-7 hours, the temperature is controlled at 55-60 DEG C, and the pressure is lower than 1.5 atmospheres, stop after reaching the time, obtain the raw powder, add auxiliary agent to the raw powder and continue to knead in the ball mill for 3 hours, during which the speed is controlled at 10 r / min for the first 0.5 hours and 26 r / min for 0.5-3 hours, the temperature is controlled at 55-60 DEG C, and the pressure is lower than 1.5 atmospheres, stop after reaching the time, obtain the cooked powder, screen the cooked powder through a vibrating screen and put it into a pulverizer to be crushed, obtain the dry compounded green pigment with particle size greater than 800 mesh.
[0035] Example 2
[0036] The embodiment of the present application provides a dry compounded green pigment, which comprises the following raw materials:
[0037] 270 kg of calcium carbonate, 130 kg of talcum powder, 510 kg of iron oxide yellow, 60 kg of phthalocyanine blue and 30 kg of auxiliary agent, the auxiliary agent is composed of coconut oil acid diethanol amide, trimethylolpropane and nonylphenol polyoxyethylene ether in a weight ratio of 1:1:1, and the particle size of calcium carbonate, talcum powder, iron oxide yellow and phthalocyanine blue is 325 mesh.
[0038] The production process of the dry compounded green pigment comprises the following steps:
[0039] Take calcium carbonate, talcum powder, iron oxide yellow, phthalocyanine blue and auxiliary agent respectively, put calcium carbonate, talcum powder, iron oxide yellow and phthalocyanine blue into double-shaft conical mixer and mix for 5 minutes to obtain premix, put the premix into a ball mill and knead for 7 hours, during which the speed is controlled at 10 r / min for the first 0.5 hours, 15 r / min for 0.5-2 hours, 20 r / min for 2-4 hours, 25 r / min for 4-7 hours, the temperature is controlled at 55-60 DEG C, and the pressure is lower than 1.5 atmospheres, stop after reaching the time, obtain the raw powder, add auxiliary agent to the raw powder and continue to knead in the ball mill for 3 hours, during which the speed is controlled at 10 r / min for the first 0.5 hours and 26 r / min for 0.5-3 hours, the temperature is controlled at 55-60 DEG C, and the pressure is lower than 1.5 atmospheres, stop after reaching the time, obtain the cooked powder, screen the cooked powder through a vibrating screen and put it into a pulverizer to be crushed, obtain the dry compounded green pigment with particle size greater than 800 mesh.
[0040] Example 3
[0041] The embodiment of the present application provides a dry compounded green pigment, which comprises the following raw materials:
[0042] calcium carbonate 340 kg, talcum powder 160 kg, iron oxide yellow 450 kg, phthalocyanine blue 40 kg, and an additive 10 kg, wherein the additive is composed of octylphenol polyoxyethylene ether, trimethylolpropane and dodecylphenol polyoxyethylene ether in a weight ratio of 1:1:1, and the particle size of the calcium carbonate, talcum powder, iron oxide yellow and phthalocyanine blue is 325 mesh.
[0043] The production process of the dry compounded green pigment comprises the following steps:
[0044] The calcium carbonate, talcum powder, iron oxide yellow, phthalocyanine blue and additive are weighed respectively, the calcium carbonate, talcum powder, iron oxide yellow and phthalocyanine blue are put into a double-shaft conical mixer and mixed for 5 min to obtain a premix, the premix is put into a ball mill and kneaded for 5 h, during which the rotating speed is controlled to be 13 r / min in the first 0.5 h, the rotating speed is controlled to be 18 r / min in the period of 0.5-1 h, the rotating speed is controlled to be 23 r / min in the period of 1-3 h, the rotating speed is controlled to be 26 r / min in the period of 3-5 h, the temperature is controlled to be 55-60 DEG C, the pressure is controlled to be lower than 1.5 atmospheres, and the machine is stopped after the time is reached to obtain a raw mixed powder, the additive is added to the raw mixed powder and the mixture is continuously kneaded in the ball mill for 3 h, during which the rotating speed is controlled to be 10 r / min in the first 0.5 h, the rotating speed is controlled to be 28 r / min in the period of 0.5-3 h, the temperature is controlled to be 55-60 DEG C, the pressure is controlled to be lower than 1.5 atmospheres, and the machine is stopped after the time is reached to obtain a cooked mixed powder, the cooked mixed powder is screened through a vibrating screen and then put into a pulverizer to be crushed to obtain the dry compounded green pigment with a particle size greater than 800 mesh.
[0045] Example 4
[0046] The embodiment of the present application provides a dry compounded green pigment, which comprises the following raw materials:
[0047] calcium carbonate 300 kg, talcum powder 150 kg, iron oxide yellow 473 kg, phthalocyanine blue 49 kg, iron oxide red 8 kg, and an additive 20 kg, wherein the additive is composed of fatty acid polyoxyethylene ester, trimethylolpropane and nonylphenol polyoxyethylene ether in a weight ratio of 1:1:1, and the particle size of the calcium carbonate, talcum powder, iron oxide yellow, phthalocyanine blue and iron oxide red is 325 mesh.
[0048] The production process of the dry compounded green pigment comprises the following steps:
[0049] Take calcium carbonate, talcum powder, yellow iron oxide, phthalocyanine blue, red iron oxide and additives respectively, put calcium carbonate, talcum powder, yellow iron oxide, phthalocyanine blue and red iron oxide into a double-shaft conical mixer and mix for 5 minutes to obtain premix, put the premix into a ball mill and knead for 7 hours, during which the speed is controlled at 10 r / min for the first 0.5 hours, 15 r / min for 0.5-2 hours, 20 r / min for 2-4 hours, and 25 r / min for 4-7 hours, the temperature is controlled at 55-60 DEG C, and the pressure is less than 1.5 atmospheres, stop after the time is reached to obtain raw mixed powder, add additives to the raw mixed powder and continue to knead in the ball mill for 3 hours, during which the speed is controlled at 10 r / min for the first 0.5 hours and 26 r / min for 0.5-3 hours, the temperature is controlled at 55-60 DEG C, and the pressure is less than 1.5 atmospheres, stop after the time is reached to obtain cooked mixed powder, screen the cooked mixed powder through a vibrating screen and then put it into a pulverizer to be pulverized to obtain dry compounded green pigment with particle size greater than 800 mesh.
[0050] Example 5
[0051] The embodiment of the present application provides a kind of dry compounded green pigment, including the following raw materials:
[0052] Calcium carbonate 326 kg, talcum powder 163 kg, yellow iron oxide 455 kg, phthalocyanine blue 41 kg, red iron oxide 5 kg, and additives 10 kg, the additives are composed of alkyl phenol polyoxyethylene ester, trimethylolpropane and dodecyl phenol polyoxyethylene ether according to weight ratio 1:1:1, and the particle size of calcium carbonate, talcum powder, yellow iron oxide, phthalocyanine blue and red iron oxide is 325 mesh.
[0053] The production process of the dry compounded green pigment includes the following steps:
[0054] Take calcium carbonate, talcum powder, yellow iron oxide, phthalocyanine blue, red iron oxide and additives respectively, put calcium carbonate, talcum powder, yellow iron oxide, phthalocyanine blue and red iron oxide into a double-shaft conical mixer and mix for 5 minutes to obtain premix, put the premix into a ball mill and knead for 7 hours, during which the speed is controlled at 10 r / min for the first 0.5 hours, 15 r / min for 0.5-2 hours, 20 r / min for 2-4 hours, and 25 r / min for 4-7 hours, the temperature is controlled at 55-60 DEG C, and the pressure is less than 1.5 atmospheres, stop after the time is reached to obtain raw mixed powder, add additives to the raw mixed powder and continue to knead in the ball mill for 3 hours, during which the speed is controlled at 10 r / min for the first 0.5 hours and 26 r / min for 0.5-3 hours, the temperature is controlled at 55-60 DEG C, and the pressure is less than 1.5 atmospheres, stop after the time is reached to obtain cooked mixed powder, screen the cooked mixed powder through a vibrating screen and then put it into a pulverizer to be pulverized to obtain dry compounded green pigment with particle size greater than 800 mesh.
[0055] Example 6
[0056] The embodiment of the present application provides a dry compounded green pigment, which comprises the following raw materials:
[0057] calcium carbonate 316 kg, talcum powder 158 kg, iron oxide yellow 463 kg, phthalocyanine blue 42 kg, iron oxide red 6 kg, and an additive 15 kg, wherein the additive is composed of fatty alcohol polyoxyethylene ether, trimethylolpropane and nonylphenol polyoxyethylene ether in a weight ratio of 1:1:1, and the particle size of the calcium carbonate, talcum powder, iron oxide yellow, phthalocyanine blue and iron oxide red is 325 mesh.
[0058] The production process of the dry compounded green pigment comprises the following steps:
[0059] The calcium carbonate, talcum powder, iron oxide yellow, phthalocyanine blue, iron oxide red and additive are weighed respectively, the calcium carbonate, talcum powder, iron oxide yellow, phthalocyanine blue and iron oxide red are put into a double-shaft conical mixer and mixed for 5 min to obtain a premix, the premix is put into a ball mill and kneaded for 6 h, during which the rotating speed is controlled to be 15 r / min in the first 0.5 h, the rotating speed is controlled to be 19 r / min in the period of 0.5-2 h, the rotating speed is controlled to be 23 r / min in the period of 2-4 h, the rotating speed is controlled to be 26 r / min in the period of 4-6 h, the temperature is controlled to be 55-60 DEG C, the pressure is controlled to be lower than 1.5 atmospheres, and the machine is stopped after the time is reached to obtain a raw mixed powder, the additive is added into the raw mixed powder and the mixture is continuously kneaded in the ball mill for 3 h, the rotating speed is controlled to be 10 r / min in the first 0.5 h, the rotating speed is controlled to be 28 r / min in the period of 0.5-3 h, the temperature is controlled to be 55-60 DEG C, the pressure is controlled to be lower than 1.5 atmospheres, and the machine is stopped after the time is reached to obtain a cooked mixed powder, the cooked mixed powder is screened through a vibrating screen and then put into a pulverizer to be pulverized to obtain the dry compounded green pigment with a particle size greater than 800 mesh.
[0060] Through tests, the dry compounded green pigments prepared in Examples 1-6 can all rapidly settle in clear water and the upper water body is clear after settling, which shows good hydrophilicity; the dry compounded green pigments prepared in Examples 1-6 are respectively put into a stirring machine and mixed with cement and sand, and the system is uniform in color and high in color concentration after mixing, which shows good dispersibility, color and tinting strength; the cement boards containing the dry compounded green pigments prepared in Examples 1-6 are placed in an outdoor environment for 6 months, and no obvious color change is observed, and the color is bright, which shows good weather resistance.
[0061] The above only describes the preferred embodiments of the present application and is not used to limit the present application, and any modification, equivalent replacement and improvement made within the spirit and principle of the present application shall be included in the protection scope of the present application.
Claims
1. A dry compounded green pigment, characterized in that, By weight percentage, including the following raw materials: body material 45%, iron oxide yellow 47.3%, phthalocyanine blue 4.9%, iron oxide red 0.8%, auxiliary 2%, the body material includes calcium carbonate and talcum powder, the weight ratio of calcium carbonate to talcum powder in the body material is 2:1, the auxiliary is composed of fatty acid polyoxyethylene ester, trimethylolpropane and nonylphenol polyoxyethylene ether in a weight ratio of 1:1:1, the particle size of calcium carbonate, talcum powder, iron oxide yellow, phthalocyanine blue and iron oxide red is 325 mesh; The production process of the dry compounded green pigment comprises the following steps: Respectively, calcium carbonate, talcum powder, iron oxide yellow, phthalocyanine blue, iron oxide red and auxiliary are weighed, calcium carbonate, talcum powder, iron oxide yellow, phthalocyanine blue and iron oxide red are put into a double-shaft conical mixer and mixed for 5 min to obtain a premix; The premix is put into a ball mill and kneaded for 7 h, during which the rotating speed is controlled at 10 r / min for the first 0.5 h, 15 r / min for 0.5-2 h, 20 r / min for 2-4 h and 25 r / min for 4-7 h, the temperature is controlled at 55-60 DEG C, the pressure is lower than 1.5 atm, and the machine is stopped after the time is reached to obtain a raw mixed powder; The auxiliary is added to the raw mixed powder and kneaded in the ball mill for another 3 h, during which the rotating speed is controlled at 10 r / min for the first 0.5 h and 26 r / min for 0.5-3 h, the temperature is controlled at 55-60 DEG C, the pressure is lower than 1.5 atm, and the machine is stopped after the time is reached to obtain a cooked mixed powder; The cooked mixed powder is screened through a vibrating screen and then put into a pulverizer to be pulverized to obtain the dry compounded green pigment.
Citation Information
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