CN112871002A - Uniform mixing method of multi-component powder raw materials - Google Patents
Uniform mixing method of multi-component powder raw materials Download PDFInfo
- Publication number
- CN112871002A CN112871002A CN202110035931.5A CN202110035931A CN112871002A CN 112871002 A CN112871002 A CN 112871002A CN 202110035931 A CN202110035931 A CN 202110035931A CN 112871002 A CN112871002 A CN 112871002A
- Authority
- CN
- China
- Prior art keywords
- raw materials
- powder
- grinding
- ball milling
- balls
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
- B01F23/60—Mixing solids with solids
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F33/00—Other mixers; Mixing plants; Combinations of mixers
- B01F33/25—Mixers with loose mixing elements, e.g. loose balls in a receptacle
- B01F33/251—Mixers with loose mixing elements, e.g. loose balls in a receptacle using balls as loose mixing element
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F33/00—Other mixers; Mixing plants; Combinations of mixers
- B01F33/80—Mixing plants; Combinations of mixers
- B01F33/805—Mixing plants; Combinations of mixers for granular material
- B01F33/8052—Mixing plants; Combinations of mixers for granular material involving other than mixing operations, e.g. milling, sieving or drying
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F33/00—Other mixers; Mixing plants; Combinations of mixers
- B01F33/80—Mixing plants; Combinations of mixers
- B01F33/83—Mixing plants specially adapted for mixing in combination with disintegrating operations
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F33/00—Other mixers; Mixing plants; Combinations of mixers
- B01F33/80—Mixing plants; Combinations of mixers
- B01F33/836—Mixing plants; Combinations of mixers combining mixing with other treatments
- B01F33/8361—Mixing plants; Combinations of mixers combining mixing with other treatments with disintegrating
- B01F33/83613—Mixing plants; Combinations of mixers combining mixing with other treatments with disintegrating by grinding or milling
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
- B01F35/20—Measuring; Control or regulation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
- B01F35/20—Measuring; Control or regulation
- B01F35/21—Measuring
- B01F35/213—Measuring of the properties of the mixtures, e.g. temperature, density or colour
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
- B01F35/20—Measuring; Control or regulation
- B01F35/22—Control or regulation
Abstract
The invention discloses a uniform mixing method of multi-component powder raw materials, which comprises the following steps: adding liquid which does not influence the chemical property of the powder as a liquid grinding medium into the powder, and adding grinding balls as a solid grinding medium, so that when the powder is subjected to ball milling, premixing and standing for layering, the depth of the upper surface clear liquid is not higher than 4 mm; ball milling and mixing. Compared with the prior art, the technical scheme of the invention has the advantages that a proper amount of liquid grinding medium and solid grinding medium is added, the fluidity state of the grinding slurry is controlled, the effect of improving the uniformity of the raw material for multi-component powder raw materials is realized generally, the research and development cost of developing the uniform mixing process for the specificity of the multi-component powder raw materials is reduced, and the universality is better.
Description
Technical Field
The invention belongs to the field of material preparation, and particularly relates to a uniform mixing method of multi-component powder raw materials.
Background
The powder raw material treatment is an important stage in the material preparation process, the pretreatment of the powder raw material is involved in the preparation of materials such as glass, ceramics, crystals and the like, and the stage is very important to the uniformity and the composition stability of the material preparation.
At present, no standard detection method is available for the uniformity of the powder raw materials, and the production efficiency is low because the performance of the finished product material prepared by sintering can be identified only, the mixing process is continuously improved by means of experience and search, and the mixing time is prolonged. Moreover, for powder raw materials with different particle sizes, specific gravities and proportions, a mixing process needs to be searched again, and the process research and development cost is extremely high.
At present, a uniform mixing method of multi-component powder raw materials with high universality is needed, and the uniform mixing method has a good uniform mixing effect on most multi-component powder raw materials, so that the process research and development cost is reduced.
Disclosure of Invention
Aiming at the defects or improvement requirements of the prior art, the invention provides a uniform mixing method of multi-component powder raw materials, which aims to improve the grinding effect of universality by simultaneously adding a proper amount of liquid grinding medium and solid grinding medium and controlling the fluidity state of grinding slurry, thereby solving the technical problems that the type, the proportion and the matched ball milling parameters of the added grinding medium are required to be developed specifically when the multi-component powder raw materials are uniformly mixed in the prior art, and the research and development cost of the uniform mixing process is high.
In order to achieve the above object, according to one aspect of the present invention, there is provided a method for uniformly mixing multicomponent powdery raw materials, comprising the steps of:
adding liquid which does not influence the chemical property of the powder as a liquid grinding medium into the powder, and adding grinding balls as a solid grinding medium, so that when the powder is placed and layered after ball milling and premixing, the powder is in a slurry state, and the depth of the upper surface clear liquid is not higher than 4 mm; ball milling and mixing.
Preferably, in the method for uniformly mixing the multi-component powder raw materials, the liquid grinding medium is pure water, absolute ethyl alcohol or an ethanol water solution, and the mass ratio of the liquid grinding medium to the powder is 0.1-1.2, preferably 0.2-0.8.
Preferably, in the method for uniformly mixing the multi-component powder raw materials, the ball milling premixing rotating speed is 120-180 r/min, and the ball milling premixing time is 30-60 min; and standing for layering, preferably standing for more than 30 min.
Preferably, in the method for uniformly mixing the multi-component powder raw materials, the grinding balls are made of corundum, zirconia and agate.
Preferably, in the method for uniformly mixing the multi-component powder raw materials, the diameter of the grinding ball is 1-6 mm; preferably, the grinding balls are divided into two types of balls with different sizes or three types of balls with different sizes, wherein the diameter range of the large balls is 4-6 mm, the diameter range of the medium balls is 3-4 mm, and the diameter range of the small balls is 1-3 mm.
Preferably, in the method for uniformly mixing the multi-component powder raw materials, the weight parts of the large balls, the small balls and the medium balls are 2-4 parts, 0-5 parts and 3 parts respectively.
Preferably, in the method for uniformly mixing the multi-component powder raw materials, the ball milling is uniformly mixed by adopting a ball milling tank of corundum, zirconia, agate, nylon, polyurethane or polytetrafluoroethylene, and the roughness Ra of the inner wall of the ball milling tank is less than 0.8. The mass ratio of the grinding balls to the powder is 0.5-3, preferably 1-2.
Preferably, in the method for uniformly mixing the multi-component powder raw materials, the rotating speed of the ball mill is controlled to be below the high-speed rotating speed without slurry flying at the top, and the lowest rotating speed is that the rising height of slurry is not lower than the depth 2/3 of the tank body when the slurry rotates; preferably 100 to 300r/min, more preferably 150 to 250 r/min.
Preferably, in the method for uniformly mixing the multi-component powder raw materials, the ball milling and uniform mixing time is 8-24 hours, and preferably 10-20 hours.
Preferably, the method for uniformly mixing the multi-component powder raw materials further comprises a uniformity detection step, and one or a combination of the following methods is adopted:
particle size analysis method:
randomly drawing more than 10 samples from the mixed samples for sampling detection, analyzing median particle diameter D50 by using a particle size analyzer, calculating the ratio of standard deviation to average value, and considering that the mixing is uniform when the ratio of the standard deviation to the average value is less than a preset threshold value, or else, considering that the mixing is non-uniform; the threshold value is preferably 5%, and more preferably 2%.
Image analysis method:
performing differential imaging on the mixed sample to ensure that the images of different powder components have contrast difference characteristics, such as different colors or different gray scales; taking a plurality of imaging areas, counting the image pixel proportion of specific contrast, calculating according to percentage, determining that the image is uniform if the image accords with normal distribution and the ratio of standard deviation to average value is less than a preset threshold value, or determining that the image is non-uniform if the image is not uniform; the threshold value is preferably 5%, and more preferably 2%.
Quantitative analysis method of regional elements:
taking at least 10 sampling units, testing the element content of the component of each unit sample, counting that the specific element content accords with normal distribution, and the ratio of the standard deviation to the average value is less than a preset threshold value, considering the element content to be uniform, or considering the element content to be non-uniform; the threshold value is preferably 5%, and more preferably 2%.
Generally, compared with the prior art, the technical scheme of the invention has the advantages that a proper amount of liquid grinding medium and solid grinding medium is added, the fluidity state of the grinding slurry is controlled, the effect of improving the uniformity of the raw material for multi-component powder raw materials is generally achieved, the research and development cost of developing the uniform mixing process for the specificity of the multi-component powder raw materials is reduced, and the universality is better.
The preferred scheme cooperates with the proportioning and other grinding processes of the quantitative control grinding ball, the liquid medium and the powder raw materials, and has the dual functions of powder crushing and mixing aiming at the powder raw materials with different particle sizes, specific gravities and proportioning, and can achieve better uniform mixing and rapid detection effects.
Drawings
FIG. 1 is a picture of the powder of example 2 after adding 0.3m of liquid ball milling medium and mixing;
FIG. 2 is a photograph of the powder of example 2 after adding 0.7m of liquid ball-milling medium and mixing.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
The invention provides a uniform mixing method of multi-component powder raw materials, which comprises the following steps:
liquid which does not influence the chemical property of the powder is added into the powder to serve as a liquid grinding medium, and grinding balls are added to serve as a solid grinding medium, so that when the powder is placed and layered after ball milling and premixing, the powder is in a slurry state, and the depth of the upper surface clear liquid is not higher than 4 mm.
The ball milling premixing rotating speed is 120-180 r/min, and the ball milling premixing time is 30-60 min;
standing for layering, preferably standing for more than 30 min;
the liquid grinding medium is pure water, absolute ethyl alcohol or an ethanol water solution, and the mass ratio of the pure water, the absolute ethyl alcohol or the ethanol water solution to the powder is 0.1-1.2, preferably 0.2-0.8. If the grinding medium content exceeds the preset value, the grinding medium is added too much, and the grinding medium needs to be dried by an oven to a proper amount; if the depth of the surface clear liquid is not more than 4mm, the mixture is in a slurry state with good fluidity, and no granular powder is exposed, the grinding medium and the powder are in proper proportion, and the sample can be continuously mixed.
The grinding balls are made of corundum, zirconia and agate. The diameter of the grinding balls is 1-6 mm, the grinding balls are divided into two types of balls with different sizes or three types of balls with different sizes, and the three types of balls with different sizes are preferably selected; wherein the diameter range of the large ball is 4-6 mm, the diameter range of the medium ball is 3-4 mm, and the diameter range of the small ball is 1-3 mm; the weight parts of the big balls, the middle balls and the small balls are respectively 2-4 parts, 0-5 parts and 3 parts;
ball milling and mixing, wherein a ball milling tank is corundum, zirconia, agate, nylon, polyurethane or polytetrafluoroethylene ball milling tank, and the roughness Ra of the inner wall is less than 0.8. The mass ratio of the grinding balls to the powder is 0.5-3, preferably 1-2; the method specifically comprises the following steps:
grinding the ground slurry by using a ball mill to obtain powder, controlling the rotating speed of the ball mill to be below the high-speed rotating speed of no slurry flying at the top, wherein the lowest rotating speed is that the rising height of the slurry is not lower than the depth 2/3 of the tank body when the slurry rotates; preferably 100 to 300r/min, more preferably 150 to 250 r/min; the sample mixing time is 8-24 hours, preferably 10-20 hours;
and (3) directly drying the mixed materials together with a ball milling tank at the drying temperature of 50-100 ℃ for different time according to the types and the contents of the raw materials and the grinding medium until the raw materials are dry and can naturally fall off, pouring the raw materials and the grinding balls into a sample separation sieve as much as possible, and after sieving, preferably transferring the raw materials into a vessel for pre-sintering to perform pre-sintering.
The ball milling and even mixing process parameters including the addition amount of the liquid grinding medium and the specification and proportion of the solid grinding medium are confirmed by using raw materials with different colors and a large number of experiments; and (4) after the final raw materials are sieved, a particle size analyzer and microscope image analysis are used for detecting the uniformity of the raw materials and the uniform mixing effect.
Preferably, the method further comprises a uniformity detection step, and one or a combination of the following methods is adopted:
particle size analysis method:
randomly drawing more than 10 samples from the mixed samples for sampling detection, analyzing median particle diameter D50 by using a particle size analyzer, calculating the ratio of standard deviation to average value, and considering that the mixing is uniform when the ratio of the standard deviation to the average value is less than a preset threshold value, or else, considering that the mixing is non-uniform; the threshold is preferably 5%, and more preferably 2%; the powder of each component has respective particle size distribution before ball milling, and the particle size tends to be uniform after ball milling, so the uniform degree of the particle size can be measured by utilizing the ratio of the standard deviation of the particle size to the average particle size, and the uniformity of the uniform mixing effect can be judged.
Image analysis method:
performing differential imaging on the mixed sample to ensure that the images of different powder components have contrast difference characteristics, such as different colors or different gray scales; taking a plurality of imaging areas, counting the pixel proportion of a specific contrast image, calculating according to percentage, determining that the image is uniform if the image accords with normal distribution and the ratio of standard deviation to average value is less than a preset threshold value, or determining that the image is non-uniform if the image is not uniform; the threshold is preferably 5%, and more preferably 2%; different powder colors or particle sizes are different, a microscope or a high-definition camera is used for shooting pictures, the distribution state of a unit sample is analyzed according to the powder differences, and the uniformity of the uniform mixing effect can be judged through the internal dispersion uniformity of the sample and the dispersion consistency among different samples.
Quantitative analysis method of regional elements:
taking at least 10 sampling units, testing the element content of the component of each unit sample, counting that the specific element content accords with normal distribution, and the ratio of the standard deviation to the average value is less than a preset threshold value, considering the element content to be uniform, or considering the element content to be non-uniform; the threshold value is preferably 5%, and more preferably 2%. And (3) testing the content of the component elements in the minimum unit of each unit sample by adopting a regional element quantitative analysis method, calculating a standard deviation according to the method, and determining whether the component elements are uniform or not, wherein if the content of the volatile elements is consistent with the design, the volatile elements are not volatilized.
The method for uniformly mixing the multi-component raw materials is not only suitable for the initial raw materials, but also suitable for the method for uniformly mixing the multi-component raw materials, which is provided by the invention, for the pre-sintered powder raw materials, as powder particles grow and locally generate agglomeration, so that the powder is more uniformly dispersed.
The selection of grinding media and the exploration of ball milling parameters are important characteristics for improving the ball milling uniform mixing effect, and the invention discovers through a large amount of experiments that:
when the amount of the liquid grinding media is too much, on one hand, the cost is higher, and on the other hand, the slurry is difficult to uniformly mix due to splashing to the top of the grinding tank; more complicated, the final ball milling effect is not uniform due to the layered sedimentation caused by different particle sizes and densities under the conditions that the liquid grinding medium is too much, the total amount of the solid grinding medium, i.e. the grinding balls, cannot be matched, and the particle size of the solid grinding medium and the particle size of the powder raw material cannot be matched. In order to match various powder materials, the ball milling and uniformly mixing method provided by the invention has good uniformly mixing effect on various powder raw materials by using a set of grinding balls with different diameters, powder gradation and a proper amount of liquid grinding medium. Under the mutual cooperation of the liquid grinding medium and the solid grinding medium, the raw materials and the grinding medium can be ensured to be in a slurry state and not to be distributed non-uniformly due to self difference.
The invention creatively adopts the depth of the surface clear liquid to judge whether the adding amount of the liquid grinding medium is proper or not, the depth of the surface clear liquid is a comprehensive judgment index combining the parameters of the powder raw material, the solid grinding medium and the grinding tank, and can directly and accurately judge the ball milling state of the raw material, thereby generally improving the ball milling uniform mixing, and the optimal ball milling state is the surface clear liquid after standing, and the depth of the surface clear liquid is not more than 4 mm.
According to the preferable scheme, after the material mixing is finished, the uniformity of the mixed material can be rapidly and quantitatively detected by a method of particle size analysis, image analysis or element analysis, and the production efficiency is improved.
In the preferred scheme, under the matching condition of a solid grinding medium and a liquid grinding medium, slurry is easy to splash and the uniformity is influenced when the rotating speed of the ball mill is too high, and the slurry cannot be fully ground and mixed when the rotating speed is too low. Through a large number of experiments, ball milling rotating speed conditions are groped by taking the mixed materials for 30-60 min and no flying slurry on the upper part of a grinding tank as standards.
The following are examples:
example 1
0.2Na2O-0.2CaO-0.6SiO2Pretreatment of multicomponent glass powder
Preparation of 0.2Na is required2O-0.2CaO-0.6SiO2Glass, accurately weighed in proportion with Na2CO3、CaO、SiO2The three kinds of powder are taken as the total weight of raw materials, namely m grams;
the following grinding media were added to the zirconia ball mill jar:
solid grinding media: grinding ball 1.5m gram, the grinding ball material is zirconia, includes wherein: a large ball with the diameter of 6mm, a medium ball with the diameter of 4mm and a small ball with the diameter of 2mm, wherein the weight part ratio is 3:4: 3;
liquid grinding medium: gradually adding absolute ethyl alcohol to the weight of 0.1m, 0.2m, 0.4m and 0.6m g for experiment;
the total volume is about the grinding pot volume 1/2. Ball milling and mixing for 1h at the rotating speed of 150r/min, taking out the ball milling tank, standing for 40min, and observing the slurry state and the clear liquid depth of the grinding medium and powder mixture, which are shown in the following table. After the optimal usage amount of the liquid grinding medium is determined, the rotating speed is increased to 200r/min, the top of the grinding tank is ensured not to have a slurry flying phenomenon, and the materials are continuously mixed for 10 hours.
Taking out the grinding tank, putting the grinding tank into a baking oven at 100 ℃, baking for about 5 hours, completely drying the powder, sieving the powder by a 20-mesh sieve, and fully vibrating to completely separate the powder from the grinding balls.
And (3) uniformity detection: the mixed samples are randomly sampled and detected, the particle size distribution after ball milling is analyzed by a particle size analyzer, more than 10 samples are tested by D10, D50 and D90, the ratio of the standard deviation of the particle size to the average particle size is calculated by using the median particle size D50, the detection result is shown in the following table 1, and the optimal embodiment is that when the weight of absolute ethyl alcohol is added to be 0.4m g, the particle size distribution data after ball milling is shown in the following table 2.
TABLE 1 Effect of Anhydrous ethanol addition on powder slurry State
Table 2D 50 particle size testing
Example 2
Bismuth sodium titanate Bi0.5Na0.5TiO3Pretreatment of ceramic powder
Need to prepare Bi0.5Na0.5TiO3Ceramic powder is proportionally and accurately weighed by Na2CO3、Bi2O3、TiO2The three kinds of powder are taken as the total weight of raw materials, namely m grams;
adding the following ball milling media into a polytetrafluoroethylene grinding tank:
liquid ball milling medium: gradually adding absolute ethyl alcohol to the weight of 0.3m, 0.5m, 0.7m, 0.9m and 1.1m to carry out experiments;
solid grinding media: grinding ball 1.2m gram, the grinding ball material is agate, wherein includes: a large ball with the diameter of 5mm and a small ball with the diameter of 2mm, wherein the weight part ratio is 2: 3;
the total volume is about the grinding pot volume 1/2. And (3) ball-milling and mixing materials for 40min at the rotating speed of 150r/min, taking out the ball-milling tank, standing for 40min, observing the slurry state and the clear liquid depth of the mixture of the grinding medium and the powder, and considering the following table 3, the addition of 0.5m, 0.7m and 0.9m of ethanol is proper, but considering the volatilization of the ethanol in the ball-milling process, the addition of 0.7m of ethanol is preferred. After the optimal usage amount of the liquid grinding medium is determined, the rotating speed is increased to 220r/min, the top of the grinding tank is ensured not to have a slurry flying phenomenon, and the materials are continuously mixed for 15 hours.
Taking out the grinding tank, putting the grinding tank into an oven at 80 ℃, baking for about 8 hours, completely drying the powder, sieving the powder by a 20-mesh sieve, and fully vibrating to completely separate the powder from the grinding balls.
And (3) uniformity detection:
uniformity detection is carried out by adopting a particle size analysis method (the steps are the same as those in the embodiment 1) and an image analysis method;
the results of particle size analysis are shown in Table 3.
Evaluating by adopting an image analysis method, specifically: the method comprises the steps of taking pictures of different powder components with different colors, particle sizes or other morphological differences by using a microscope or a high-definition camera, and analyzing the distribution states of at least 10 different selected areas according to the powder differences, wherein the distribution states comprise the internal dispersion uniformity of the selected areas and the dispersion consistency among the different selected areas. Bi2O3Powder is yellow green, other powder is white, test Bi2O3And calculating the ratio of the image pixel ratio of the powder in different selected areas to the average ratio of the standard deviation of the ratio. The high resolution photograph of the resulting mixture after adding 0.3m of liquid ball milling media according to this example is shown in FIG. 1; a high resolution photograph of the resulting mixture after mixing with 0.7m of liquid ball milling media according to this example is shown in FIG. 2, and the results of the image analysis and measurement after mixing are shown in Table 4 and the particle size measurement results are shown in Table 5.
TABLE 3 Effect of Anhydrous ethanol addition on powder slurry State
TABLE 4 results of image analysis
Table 5D 50 particle size testing
It will be understood by those skilled in the art that the foregoing is only a preferred embodiment of the present invention, and is not intended to limit the invention, and that any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (10)
1. The uniform mixing method of the multi-component powder raw materials is characterized by comprising the following steps:
adding liquid which does not influence the chemical property of the powder as a liquid grinding medium into the powder, and adding grinding balls as a solid grinding medium, so that when the powder is subjected to ball milling, premixing and standing for layering, the depth of the upper surface clear liquid is not higher than 4 mm; ball milling and mixing.
2. The method for uniformly mixing multicomponent powder raw materials according to claim 1, wherein the liquid grinding medium is pure water, absolute ethyl alcohol, or an aqueous solution of ethyl alcohol, and the mass ratio of the liquid grinding medium to the powder is 0.1 to 1.2, preferably 0.2 to 0.8.
3. The method for uniformly mixing multi-component powder raw materials according to claim 1, wherein the ball milling premixing rotating speed is 120-180 r/min, and the ball milling premixing time is 30-60 min; and standing for layering, preferably standing for more than 30 min.
4. The method for uniformly mixing multicomponent powder raw materials according to claim 1, wherein the grinding balls are made of corundum, zirconia or agate.
5. The method for uniformly mixing multicomponent powder raw materials according to claim 1, wherein the grinding balls have a diameter of 1 to 6 mm; preferably, the grinding balls are divided into two types of balls with different sizes or three types of balls with different sizes, wherein the diameter range of the large balls is 4-6 mm, the diameter range of the medium balls is 3-4 mm, and the diameter range of the small balls is 1-3 mm.
6. The method for uniformly mixing multicomponent powder raw materials according to claim 4, wherein the weight parts of the large, medium and small spheres are 2 to 4 parts, 0 to 5 parts and 3 parts, respectively.
7. The method for homogeneously mixing multicomponent powder raw materials according to claim 1, wherein the ball milling and homogeneously mixing is carried out in a ball milling tank of corundum, zirconia, agate, nylon, polyurethane or polytetrafluoroethylene, and the roughness Ra of the inner wall is less than 0.8. The mass ratio of the grinding balls to the powder is 0.5-3, preferably 1-2.
8. The method of homogenizing a multicomponent powder raw material according to claim 1, wherein the rotational speed of the ball mill is controlled to be not higher than a high rotational speed at which no slurry flies from the top, and the lowest rotational speed is a rotational speed at which the slurry rises to a height not lower than a tank depth 2/3; preferably 100 to 300r/min, more preferably 150 to 250 r/min.
9. The method for uniformly mixing multicomponent powder raw materials according to claim 1, wherein the ball milling and uniformly mixing time is 8 to 24 hours, preferably 10 to 20 hours.
10. The method for homogeneously mixing multicomponent powdery raw materials according to claim 1, further comprising a step of detecting the homogeneity by one or a combination of the following methods:
particle size analysis method:
randomly drawing more than 10 samples from the mixed samples for sampling detection, analyzing median particle diameter D50 by using a particle size analyzer, calculating the ratio of standard deviation to average value, and considering that the mixing is uniform when the ratio of the standard deviation to the average value is less than a preset threshold value, or else, considering that the mixing is non-uniform; the threshold is preferably 5%, and more preferably 2%;
image analysis method:
performing differential imaging on the mixed sample to ensure that the images of different powder components have contrast difference characteristics, such as different colors or different gray scales; taking a plurality of imaging areas and counting the image pixel proportion of specific contrast, if the image pixel proportion accords with normal distribution and the ratio of the standard deviation to the average value is smaller than a preset threshold value, considering the image pixel proportion as uniform, and if the image pixel proportion is not uniform, considering the image pixel proportion as non-uniform; the threshold is preferably 5%, and more preferably 2%;
quantitative analysis method of regional elements:
taking at least 10 sampling units, testing the element content of the component of each unit sample, counting that the specific element content accords with normal distribution, and the ratio of the standard deviation to the average value is less than a preset threshold value, considering the element content to be uniform, or considering the element content to be non-uniform; the threshold value is preferably 5%, and more preferably 2%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110035931.5A CN112871002A (en) | 2021-01-12 | 2021-01-12 | Uniform mixing method of multi-component powder raw materials |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110035931.5A CN112871002A (en) | 2021-01-12 | 2021-01-12 | Uniform mixing method of multi-component powder raw materials |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112871002A true CN112871002A (en) | 2021-06-01 |
Family
ID=76044100
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110035931.5A Pending CN112871002A (en) | 2021-01-12 | 2021-01-12 | Uniform mixing method of multi-component powder raw materials |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112871002A (en) |
Citations (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS54159771A (en) * | 1978-06-07 | 1979-12-17 | Kubota Ltd | Wet type automatic crusher |
| AU5746796A (en) * | 1995-06-20 | 1997-01-22 | Minnesota Mining And Manufacturing Company | Alpha alumina-based abrasive grain containing silica and iron oxide |
| GR3025143T3 (en) * | 1993-06-29 | 1998-02-27 | Pfizer | Apparatus for mixing and detecting on-line homogeneity. |
| CN101279213A (en) * | 2008-01-17 | 2008-10-08 | 京东方科技集团股份有限公司 | Device for circularly grinding and dispersing and method thereof |
| CN101279369A (en) * | 2008-05-15 | 2008-10-08 | 金川集团有限公司 | Method for preparing sheet silver powder with high dispersibility |
| CN101318817A (en) * | 2008-06-25 | 2008-12-10 | 重庆科技学院 | Process for manufacturing barium zirconium titanate ceramic |
| CN101550015A (en) * | 2009-04-23 | 2009-10-07 | 桂林工学院 | Method of preparing perovskite niobate titanate nanometer powders |
| CN101798227A (en) * | 2010-03-24 | 2010-08-11 | 桂林理工大学 | Solid phase synthetic method of niobate-titanate nano-powder |
| CN102176519A (en) * | 2011-03-02 | 2011-09-07 | 湖南美特新材料科技有限公司 | Method for preparing submicron-level lithium carbonate, lithium carbonate powder and application of lithium carbonate powder |
| CN103272677A (en) * | 2013-05-22 | 2013-09-04 | 袁伟 | Method for preparing nano particles and application thereof |
| CN103626492A (en) * | 2013-12-18 | 2014-03-12 | 江西赛瓷材料有限公司 | Scandia-stabilized zirconia powder for solid oxide fuel battery |
| CN104311013A (en) * | 2014-10-10 | 2015-01-28 | 北京理工大学 | Ceramic powder material SmTaO4 and preparation method thereof |
| CN104475213A (en) * | 2014-11-10 | 2015-04-01 | 张藜泷 | Method for preparing ultra-fine Hetian jade powder |
| CN105548280A (en) * | 2015-12-30 | 2016-05-04 | 东旭科技集团有限公司 | Method for determining uniformity of mixed batch for alkali-free glass and method for preparing mixed batch |
| CN107793149A (en) * | 2017-11-01 | 2018-03-13 | 西南大学 | A kind of preparation method of ZTA nano composite powders |
| CN107805074A (en) * | 2017-11-13 | 2018-03-16 | 戴承萍 | A kind of processing method of electronic ceramics casting slurry |
| CN110201594A (en) * | 2019-06-27 | 2019-09-06 | 杜婧宇 | A kind of preparation method and preparation system of high fluidity and stability water-coal-slurry |
| CN111233472A (en) * | 2020-02-19 | 2020-06-05 | 内蒙古科技大学 | Application of multifunctional silver niobate ceramic in electrocaloric effect refrigeration technology |
| CN111992318A (en) * | 2020-08-05 | 2020-11-27 | 饶从相 | Mixing process for traditional Chinese medicine powder |
-
2021
- 2021-01-12 CN CN202110035931.5A patent/CN112871002A/en active Pending
Patent Citations (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS54159771A (en) * | 1978-06-07 | 1979-12-17 | Kubota Ltd | Wet type automatic crusher |
| GR3025143T3 (en) * | 1993-06-29 | 1998-02-27 | Pfizer | Apparatus for mixing and detecting on-line homogeneity. |
| AU5746796A (en) * | 1995-06-20 | 1997-01-22 | Minnesota Mining And Manufacturing Company | Alpha alumina-based abrasive grain containing silica and iron oxide |
| CN101279213A (en) * | 2008-01-17 | 2008-10-08 | 京东方科技集团股份有限公司 | Device for circularly grinding and dispersing and method thereof |
| CN101279369A (en) * | 2008-05-15 | 2008-10-08 | 金川集团有限公司 | Method for preparing sheet silver powder with high dispersibility |
| CN101318817A (en) * | 2008-06-25 | 2008-12-10 | 重庆科技学院 | Process for manufacturing barium zirconium titanate ceramic |
| CN101550015A (en) * | 2009-04-23 | 2009-10-07 | 桂林工学院 | Method of preparing perovskite niobate titanate nanometer powders |
| CN101798227A (en) * | 2010-03-24 | 2010-08-11 | 桂林理工大学 | Solid phase synthetic method of niobate-titanate nano-powder |
| CN102176519A (en) * | 2011-03-02 | 2011-09-07 | 湖南美特新材料科技有限公司 | Method for preparing submicron-level lithium carbonate, lithium carbonate powder and application of lithium carbonate powder |
| CN103272677A (en) * | 2013-05-22 | 2013-09-04 | 袁伟 | Method for preparing nano particles and application thereof |
| CN103626492A (en) * | 2013-12-18 | 2014-03-12 | 江西赛瓷材料有限公司 | Scandia-stabilized zirconia powder for solid oxide fuel battery |
| CN104311013A (en) * | 2014-10-10 | 2015-01-28 | 北京理工大学 | Ceramic powder material SmTaO4 and preparation method thereof |
| CN104475213A (en) * | 2014-11-10 | 2015-04-01 | 张藜泷 | Method for preparing ultra-fine Hetian jade powder |
| CN105548280A (en) * | 2015-12-30 | 2016-05-04 | 东旭科技集团有限公司 | Method for determining uniformity of mixed batch for alkali-free glass and method for preparing mixed batch |
| CN107793149A (en) * | 2017-11-01 | 2018-03-13 | 西南大学 | A kind of preparation method of ZTA nano composite powders |
| CN107805074A (en) * | 2017-11-13 | 2018-03-16 | 戴承萍 | A kind of processing method of electronic ceramics casting slurry |
| CN110201594A (en) * | 2019-06-27 | 2019-09-06 | 杜婧宇 | A kind of preparation method and preparation system of high fluidity and stability water-coal-slurry |
| CN111233472A (en) * | 2020-02-19 | 2020-06-05 | 内蒙古科技大学 | Application of multifunctional silver niobate ceramic in electrocaloric effect refrigeration technology |
| CN111992318A (en) * | 2020-08-05 | 2020-11-27 | 饶从相 | Mixing process for traditional Chinese medicine powder |
Non-Patent Citations (3)
| Title |
|---|
| 张书达等: "金 刚 石微粉和抛光液的制造工艺检测技术及应用 （ 下 ）", 《超硬材料工程》 * |
| 甘学贤等: "研磨设备和工艺参数对氧化锆粉体粒度的影响", 《耐火材料》 * |
| 肖劲等: "片状超细 α-Ａｌ2 Ｏ3 的 制备研究", 《矿冶工程》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102854080B (en) | Method for measuring iron content in steel slag | |
| HU226972B1 (en) | Method for measuring degree and homogeneity of alumina calcination | |
| CN108593428A (en) | A kind of discrete material Particle Breakage test device and test method | |
| JP5199782B2 (en) | Quality evaluation method of fly ash | |
| Germani et al. | Automated scanning electron microscopy for atmospheric particle analysis | |
| CN111323282A (en) | Preparation method of paint powder standard sample containing 17 migratable elements limited in toy field | |
| CN107132162A (en) | A kind of particle diameter of alkaline earth metal carbonate powder and the assay method of particle diameter distribution | |
| CN112871002A (en) | Uniform mixing method of multi-component powder raw materials | |
| Bhuiyan et al. | Quantitative image analysis of bubble cavities in iron ore green pellets | |
| CN101329280A (en) | Fast testing method of hydrogen peroxide residue in milk-like liquid and testing reagent kit thereof | |
| EP0752110B1 (en) | Method and appliance for controlling the grinding of mineral raw materials | |
| CN110208454A (en) | A method of improving the cement dose measuring accuracy for being used for stabilized macadam base | |
| CN114912725A (en) | Application of quality control method based on physical attributes in detection of Suhuang cough relieving capsule intermediate | |
| WO2022100516A1 (en) | Cell suspension sample imaging method and system, and kit | |
| Peksa et al. | Histometric and biochemical properties of the thyroid gland in sheep with high iodine supplementation | |
| Zegzulka et al. | Flow characterization methods of glidants | |
| RU2267117C1 (en) | Method of determining time of mixing loose materials | |
| Hörenz et al. | 889–A Study on the Analysis of Particle Size Distribution for Bimodal Model Nanoparticles by Electron Microscopy | |
| CN104597071B (en) | Assay method of the carbon-sulfur crucible with respect to softening temperature | |
| CN115144323B (en) | Method for detecting content of non-metallic inclusions in metal powder for additive manufacturing | |
| CN114502266B (en) | Powder mixing system and powder mixing method | |
| Herber et al. | A collaborative study using solid sampling graphite furnace atomic absorption spectrometry | |
| CN212254951U (en) | Dispersing ability detection system of dispersing agent and detection device thereof | |
| JP2813952B2 (en) | Colored magnetic powder for magnetic particle flaw detection test and method for producing the same | |
| CN117782906A (en) | Particle size determination method of pharmaceutical auxiliary material magnesium stearate |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |