CN114231284A - Preparation method of active heavy calcium carbonate applied to rare earth self-luminous material - Google Patents

Preparation method of active heavy calcium carbonate applied to rare earth self-luminous material Download PDF

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CN114231284A
CN114231284A CN202111599403.9A CN202111599403A CN114231284A CN 114231284 A CN114231284 A CN 114231284A CN 202111599403 A CN202111599403 A CN 202111599403A CN 114231284 A CN114231284 A CN 114231284A
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calcium carbonate
heavy calcium
rare earth
stirring
portions
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温增勇
李森福
李达
李蔡华
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Guangdong Xianglong Technology Co ltd
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Guangdong Xianglong Technology Co ltd
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    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/77Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
    • C09K11/7783Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals one of which being europium
    • C09K11/7792Aluminates

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  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
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  • Organic Chemistry (AREA)
  • Luminescent Compositions (AREA)

Abstract

The invention discloses a preparation method of active heavy calcium carbonate applied to a rare earth self-luminous material. In the present invention, Sr is weighed2ZnSi2O7500 to 700 portions of Eu2+20 to 30 portions of Dy3+20 to 30 portions of SrAl2O490 to 100 portions of BaREF520 to 30 portions of Dy3+10 to-20 parts of Eu3+10 to-20 portions of Gd2O310 to-20 portions of Ti4+30 to 50 portions; taking out the modified heavy calcium carbonate block after drying, crushing for 3min at high speed by a crusher to obtain active heavy calcium carbonate dry powder, and then grinding the heavy calcium carbonate powder to the diameter of 2 mu m by a grinder; mixing the raw materials according to the proportion, and then putting the mixture into a planetary ball mill for grinding to fully mix the raw materials; the prepared active heavy calcium carbonate powder can emit red light in a low-temperature environment, emit blue and white light after thermochromic, endow a novel function of a noctilucent material, and widen the application of the noctilucent material in the fields of temperature-sensitive sensing and the like, therebyThe persistent luminescence of the rare earth self-luminescent material and the durability of the material are improved.

Description

Preparation method of active heavy calcium carbonate applied to rare earth self-luminous material
Technical Field
The invention belongs to the technical field of heavy calcium carbonate, and particularly relates to a preparation method of active heavy calcium carbonate applied to a rare earth self-luminous material.
Background
Ground calcium carbonate, called triple superphosphate for short, is ground from natural carbonate minerals such as calcite, marble and limestone. The inorganic filler is a common powdery inorganic filler and has the advantages of high chemical purity, high inertia, difficult chemical reaction, good thermal stability, no decomposition at the temperature of below 400 ℃, high whiteness, low oil absorption rate, low refractive index, soft quality, dryness, no crystal water, low hardness, low abrasion value, no toxicity, no odor, good dispersibility and the like. In the development of rare earth functional materials, rare earth luminescent materials are particularly attractive. Rare earth has spectral properties incomparable with common elements due to the special electronic layer structure, and the rare earth luminescence almost covers the whole solid luminescence range, so long as the luminescence is mentioned, the rare earth can hardly be distinguished. Atoms of rare earth elements have unfilled electronic configuration shielded by the outside, so that the rare earth elements have abundant electronic energy levels and long-life excited states, energy level transition channels are as many as 20 or more than ten thousand, and the rare earth elements can generate various radiation absorption and emission to form wide light-emitting and laser materials.
However, the common rare earth self-luminous heavy calcium carbonate material has lower luminous time, so that the practicability of the rare earth self-luminous heavy calcium carbonate material in the using process is lower.
Disclosure of Invention
The invention aims to: in order to solve the problems, the preparation method of the active heavy calcium carbonate applied to the rare earth self-luminous material is provided.
The technical scheme adopted by the invention is as follows: the preparation method of the active heavy calcium carbonate applied to the rare earth self-luminous material comprises the following steps:
s1, preparing the rare earth self-luminous material: weighing Sr2ZnSi2O7500 to 700 portions of Eu2+20 to 30 portions of Dy3+20 to 30 portions of SrAl2O490 to 100 portions of BaREF520 to 30 portions of Dy3+10 to-20 parts of Eu3+10 to-20 portions of Gd2O310 to-20 portions of Ti4+30 to 50 portions; mixing the raw materials according to the proportion, and then putting the mixture into a planetary ball mill for grinding to fully mix the raw materials;
s2, pouring the uniformly mixed powder into a crucible, and then putting the crucible into a high-temperature tube furnace according to the set experimental conditions; after sintering is finished, taking the calcined sample out of the crucible after natural cooling to obtain the rare earth luminescent material;
s3, weighing 900 to 1000 parts of calcium carbonate dry powder with the granularity of 43 to 47 mu m into a stirring reaction kettle, and adding purified water to prepare slurry with the solid mass fraction of 75 percent;
s4, weighing 9-27 parts of stearic acid, adding the stearic acid into the slurry prepared in the step S3, and fully stirring and mixing the stearic acid and the slurry to obtain initial modified slurry;
s5, taking out the initial modified slurry in the step S4, adding the initial modified slurry into a stirring dispersion machine for stirring;
s6, stopping stirring after the stirring in the step S5 is finished, taking out the slurry, and drying the slurry in a drying box at 180 ℃;
s7, in the step S6, after drying, taking out the modified heavy calcium carbonate blocks, crushing the modified heavy calcium carbonate blocks for 3min at a high speed by a crusher to obtain active heavy calcium carbonate dry powder, and then grinding the heavy calcium carbonate powder to the diameter of 2 mu m by a grinder;
s8, mixing the heavy calcium carbonate dry powder prepared in the step S6 and the rare earth luminescent material prepared in the step S2, placing the mixture in a dry stirring and mixing box, and stirring the mixture;
and S9, after stirring, packaging and storing the obtained powder material to obtain the active heavy calcium carbonate applied to the rare earth self-luminous material, thereby finishing the whole preparation process.
In a preferred embodiment, in step S1, the time for the planetary ball mill to grind is controlled to be 50min, and the grinding speed is controlled to be 1500 r/min.
In a preferred embodiment, in step S2, the sintering temperature in the high-temperature tube furnace is controlled to 1800 degrees celsius, and the sintering time is controlled to 4 hours.
In a preferred embodiment, in the step S3, the stirring time of the stirring reaction kettle is 50min, and the stirring speed is 800 r/min.
In a preferred embodiment, in the step S4, the slurry has an initial viscosity of 147mPa · S at 42 ℃ and a viscosity of 228mPa · S after standing for 20 min.
In a preferred embodiment, in step S5, the stirring speed is 1100r/min, and the stirring time is 120 min.
In a preferred embodiment, in step S6, the drying temperature in the drying oven is controlled to be 180 ℃ and the drying time is 90 min.
In a preferred embodiment, in step S8, the stirring speed is 600r/min, and the stirring time is 240 min.
In summary, due to the adoption of the technical scheme, the invention has the beneficial effects that:
1. the prepared active heavy calcium carbonate powder can emit red light in a low-temperature environment, and emit blue and white light after thermochromic, so that a new function of the noctilucent material is endowed, and the application of the noctilucent material in the fields of temperature-sensitive sensing and the like is widened, and the lasting luminescence of the rare earth self-luminescent material and the durability of the material are improved.
2. In the present invention, the particle size of the ground calcium carbonate particles is reduced from 45 μm to 2 μm. With the gradual increase of the addition amount of stearic acid, the activation degree of the heavy calcium carbonate is increased, and the oil absorption value is reduced. When the addition of stearic acid is increased to 2 mass percent, the activation degree of the heavy calcium carbonate exceeds 98 percent, so that the grinding and modification integrated process is favorable for reducing the production cost of the heavy calcium carbonate and increasing the competitiveness of the product.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments. 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.
The first embodiment is as follows:
the preparation method of the active heavy calcium carbonate applied to the rare earth self-luminous material comprises the following steps:
s1, preparing the rare earth self-luminous material: weighing Sr2ZnSi2O7500 parts of Eu2+20 parts of Dy3+20 parts of SrAl2O490 portions of BaREF520 parts of Dy3+10 parts of Eu3+10 parts of Gd2O310 parts of Ti4+30 parts of (1); mixing the raw materials according to the proportion, and then putting the mixture into a planetary ball mill for grinding to fully mix the raw materials; in the step S1, the grinding time of the planetary ball mill is controlled to be 50min, and the grinding speed is 1500 r/min;
s2, pouring the uniformly mixed powder into a crucible, and then putting the crucible into a high-temperature tube furnace according to the set experimental conditions; after sintering is finished, taking the calcined sample out of the crucible after natural cooling to obtain the rare earth luminescent material; in step S2, the sintering temperature in the high-temperature tube furnace is controlled at 1800 ℃ and the sintering time is controlled at 4 hours;
s3, weighing 900 parts of calcium carbonate dry powder with the granularity of 43-47 mu m into a stirring reaction kettle, and adding purified water to prepare slurry with the solid mass fraction of 75%; in step S3, stirring with a stirring reaction kettle for 50min at a stirring speed of 800 r/min;
s4, weighing 9 parts of stearic acid, adding the stearic acid into the slurry prepared in the step S3, and fully stirring and mixing the stearic acid and the slurry to obtain initial modified slurry; in step S4, the initial viscosity of the slurry at 42 ℃ is 147mPa & S, and the viscosity is 228mPa & S after standing for 20 min;
s5, taking out the initial modified slurry in the step S4, adding the initial modified slurry into a stirring dispersion machine for stirring; in step S5, the stirring speed is 1100r/min, and the stirring time is 120 min;
s6, stopping stirring after the stirring in the step S5 is finished, taking out the slurry, and drying the slurry in a drying box at 180 ℃; in step S6, the drying temperature in the drying oven is controlled to be 180 ℃, and the drying time is 90 min;
s7, in the step S6, after the drying is finished, the modified heavy calcium carbonate blocks are taken out and are ground for 3min at a high speed by a grinder to obtain active heavy calcium carbonate dry powder; then ground the heavy calcium carbonate powder to a diameter of 2 μm using a grinder;
s8, mixing the heavy calcium carbonate dry powder prepared in the step S6 and the rare earth luminescent material prepared in the step S2, placing the mixture in a dry stirring and mixing box, and stirring the mixture; in step S8, the stirring speed is 600r/min, and the stirring time is 240 min;
s9, after stirring, packaging and storing the obtained powder material to obtain the active ground calcium carbonate applied to the rare earth self-luminous material, thereby finishing the whole preparation process, wherein the prepared active ground calcium carbonate powder can emit red light in a low-temperature environment, emit blue and white light after temperature-sensitive discoloration, endow a new function of the noctilucent material, widen the application of the noctilucent material in the fields of temperature-sensitive sensing and the like, thereby improving the lasting luminescence of the rare earth self-luminous material and the durability of the material, and reducing the particle size of the ground calcium carbonate particles from 45 mu m to 2 mu m. With the gradual increase of the addition amount of stearic acid, the activation degree of the heavy calcium carbonate is increased, and the oil absorption value is reduced. When the addition of stearic acid is increased to 2 mass percent, the activation degree of the heavy calcium carbonate exceeds 98 percent, so that the grinding and modification integrated process is favorable for reducing the production cost of the heavy calcium carbonate and increasing the competitiveness of the product.
Example two:
the preparation method of the active heavy calcium carbonate applied to the rare earth self-luminous material comprises the following steps:
s1, preparing the rare earth self-luminous material: weighing Sr2ZnSi2O7700 parts of Eu2+30 parts of Dy3+30 parts of SrAl2O4100 portions of BaREF530 parts of Dy3+20 parts of Eu3+20 parts of Gd2O320 parts of Ti4+50 parts of a mixture; mixing the raw materials according to the proportion, and then putting the mixture into a planetary ball mill for grinding to fully mix the raw materials; in the step S1, the grinding time of the planetary ball mill is controlled to be 50min, and the grinding speed is 1500 r/min;
s2, pouring the uniformly mixed powder into a crucible, and then putting the crucible into a high-temperature tube furnace according to the set experimental conditions; after sintering is finished, taking the calcined sample out of the crucible after natural cooling to obtain the rare earth luminescent material; in step S2, the sintering temperature in the high-temperature tube furnace is controlled at 1800 ℃ and the sintering time is controlled at 4 hours;
s3, weighing 000 parts of calcium carbonate dry powder with the granularity of 43-47 mu m into a stirring reaction kettle, and adding purified water to prepare slurry with the solid mass fraction of 75%; in step S3, stirring with a stirring reaction kettle for 50min at a stirring speed of 800 r/min;
s4, weighing 27 parts of stearic acid, adding the stearic acid into the slurry prepared in the step S3, and fully stirring and mixing the stearic acid and the slurry to obtain initial modified slurry; in step S4, the initial viscosity of the slurry at 42 ℃ is 147mPa & S, and the viscosity is 228mPa & S after standing for 20 min;
s5, taking out the initial modified slurry in the step S4, adding the initial modified slurry into a stirring dispersion machine for stirring; in step S5, the stirring speed is 1100r/min, and the stirring time is 120 min;
s6, stopping stirring after the stirring in the step S5 is finished, taking out the slurry, and drying the slurry in a drying box at 180 ℃; in step S6, the drying temperature in the drying oven is controlled to be 180 ℃, and the drying time is 90 min;
s7, in the step S6, after the drying is finished, the modified heavy calcium carbonate blocks are taken out and are ground for 3min at a high speed by a grinder to obtain active heavy calcium carbonate dry powder; then ground the heavy calcium carbonate powder to a diameter of 2 μm using a grinder;
s8, mixing the heavy calcium carbonate dry powder prepared in the step S6 and the rare earth luminescent material prepared in the step S2, placing the mixture in a dry stirring and mixing box, and stirring the mixture; in step S8, the stirring speed is 600r/min, and the stirring time is 240 min;
s9, after stirring, packaging and storing the obtained powder material to obtain the active ground calcium carbonate applied to the rare earth self-luminous material, thereby finishing the whole preparation process, wherein the prepared active ground calcium carbonate powder can emit red light in a low-temperature environment, emit blue and white light after temperature-sensitive discoloration, endow a new function of the noctilucent material, widen the application of the noctilucent material in the fields of temperature-sensitive sensing and the like, thereby improving the lasting luminescence of the rare earth self-luminous material and the durability of the material, and reducing the particle size of the ground calcium carbonate particles from 45 mu m to 2 mu m. With the gradual increase of the addition amount of stearic acid, the activation degree of the heavy calcium carbonate is increased, and the oil absorption value is reduced. When the addition of stearic acid is increased to 2 mass percent, the activation degree of the heavy calcium carbonate exceeds 98 percent, so that the grinding and modification integrated process is favorable for reducing the production cost of the heavy calcium carbonate and increasing the competitiveness of the product.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.

Claims (8)

1. A preparation method of active heavy calcium carbonate applied to a rare earth self-luminous material is characterized by comprising the following steps: the preparation method of the active heavy calcium carbonate applied to the rare earth self-luminous material comprises the following steps:
s1, preparing the rare earth self-luminous material: weighing Sr2ZnSi2O7500 to 700 portions of Eu2+20 to 30 portions of Dy3+20 to 30 portions of SrAl2O490 to 100 portions of BaREF520 to 30 portions of Dy3+10 to-20 parts of Eu3+10 to-20 portions of Gd2O310 to-20 portions of Ti4+30 to 50 portions; mixing the raw materials according to the proportion, and then putting the mixture into a planetary ball mill for grinding to fully mix the raw materials;
s2, pouring the uniformly mixed powder into a crucible, and then putting the crucible into a high-temperature tube furnace according to the set experimental conditions; after sintering is finished, taking the calcined sample out of the crucible after natural cooling to obtain the rare earth luminescent material;
s3, weighing 900 to 1000 parts of calcium carbonate dry powder with the granularity of 43 to 47 mu m into a stirring reaction kettle, and adding purified water to prepare slurry with the solid mass fraction of 75 percent;
s4, weighing 9-27 parts of stearic acid, adding the stearic acid into the slurry prepared in the step S3, and fully stirring and mixing the stearic acid and the slurry to obtain initial modified slurry;
s5, taking out the initial modified slurry in the step S4, adding the initial modified slurry into a stirring dispersion machine for stirring;
s6, stopping stirring after the stirring in the step S5 is finished, taking out the slurry, and drying the slurry in a drying box at 180 ℃;
s7, in the step S6, after drying, taking out the modified heavy calcium carbonate blocks, crushing the modified heavy calcium carbonate blocks for 3min at a high speed by a crusher to obtain active heavy calcium carbonate dry powder, and then grinding the heavy calcium carbonate powder to the diameter of 2 mu m by a grinder;
s8, mixing the heavy calcium carbonate dry powder prepared in the step S6 and the rare earth luminescent material prepared in the step S2, placing the mixture in a dry stirring and mixing box, and stirring the mixture;
and S9, after stirring, packaging and storing the obtained powder material to obtain the active heavy calcium carbonate applied to the rare earth self-luminous material, thereby finishing the whole preparation process.
2. The method for preparing activated heavy calcium carbonate applied to the rare earth self-luminous material according to claim 1, wherein the method comprises the following steps: in the step S1, the grinding time of the planetary ball mill is controlled to be 50min, and the grinding speed is 1500 r/min.
3. The method for preparing activated heavy calcium carbonate applied to the rare earth self-luminous material according to claim 1, wherein the method comprises the following steps: in the step S2, the sintering temperature in the high-temperature tube furnace is controlled to 1800 ℃, and the sintering time is controlled to 4 hours.
4. The method for preparing activated heavy calcium carbonate applied to the rare earth self-luminous material according to claim 1, wherein the method comprises the following steps: in the step S3, the stirring time of the stirring reaction kettle is 50min, and the stirring speed is 800 r/min.
5. The method for preparing activated heavy calcium carbonate applied to the rare earth self-luminous material according to claim 1, wherein the method comprises the following steps: in the step S4, the initial viscosity of the slurry at 42 ℃ is 147mPa & S, and the viscosity after standing for 20min is 228mPa & S.
6. The method for preparing activated heavy calcium carbonate applied to the rare earth self-luminous material according to claim 1, wherein the method comprises the following steps: in the step S5, the stirring speed is 1100r/min, and the stirring time is 120 min.
7. The method for preparing activated heavy calcium carbonate applied to the rare earth self-luminous material according to claim 1, wherein the method comprises the following steps: in the step S6, the drying temperature in the drying oven is controlled to 180 ℃ and the drying time is 90 min.
8. The method for preparing activated heavy calcium carbonate applied to the rare earth self-luminous material according to claim 1, wherein the method comprises the following steps: in the step S8, the stirring speed is 600r/min, and the stirring time is 240 min.
CN202111599403.9A 2021-12-24 2021-12-24 Preparation method of active heavy calcium carbonate applied to rare earth self-luminous material Pending CN114231284A (en)

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Application publication date: 20220325