CN113388341B - Solid binder and preparation method and application thereof - Google Patents

Solid binder and preparation method and application thereof Download PDF

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Publication number
CN113388341B
CN113388341B CN202110671578.XA CN202110671578A CN113388341B CN 113388341 B CN113388341 B CN 113388341B CN 202110671578 A CN202110671578 A CN 202110671578A CN 113388341 B CN113388341 B CN 113388341B
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binder
powder
tablets
raw materials
materials
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CN113388341A (en
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刘梦雪
黄士伟
肖慧丽
李保军
王莹
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Anhui Jinggong Testing And Testing Center Co ltd
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Anhui Jinggong Testing And Testing Center Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J101/00—Adhesives based on cellulose, modified cellulose, or cellulose derivatives
    • C09J101/08—Cellulose derivatives
    • C09J101/26—Cellulose ethers
    • C09J101/28—Alkyl ethers
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02—Non-macromolecular additives
    • C09J11/06—Non-macromolecular additives organic
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/08—Macromolecular additives
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q

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  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
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Abstract

The invention provides a solid binder and a preparation method and application thereof, wherein raw materials comprise binder, dispersing agent, lubricant, tackifier, and the solid binder is synergistic with the raw materials in the prior art, has good lubricity and powder fluidity, excellent dispersibility, good cohesiveness, can meet the tabletting requirements of cement and various raw materials, and has the advantages of high yield, low cost, easy obtainment of raw materials and low cost. In addition, the solid binder is prepared into tablets, and the tablets are coated with an outer layer, so that the tablets are moisture-proof, easy to transport and capable of being stored in a large amount.

Description

Solid binder and preparation method and application thereof
Technical Field
The invention belongs to the field of building material detection. In particular to a solid binder, a preparation method and application thereof.
Background
The powder tabletting method is a preferred sample preparation method for tabletting detection in the cement industry due to the advantages of high analysis speed, wide detection range, high accuracy, simple operation and the like, but also has the defects of poor powder flowability, large tablet weight difference, easiness in cracking caused by powder tabletting and the like, so that the application of the process is limited to a certain extent.
Along with the change of mixed materials in the cement industry and the improvement of market demands, the requirement on the adhesive is higher and higher. The raw materials in the cement industry are rich, the cohesiveness and the dispersibility of different materials are different, and the tabletting adhesives need to be compatible with the dispersibility, cohesiveness, lubricity and powder flowability of the materials. The liquid binder is not easy to be completely dispersed in the powder, the bonding effect is limited, and the liquid can be evaporated in the grinding process, so that the quality of the sample is changed, and the test results such as fluorescence are affected, so that the solid binder is preferentially considered in the cement industry at present.
The solid binder used in the cement industry at present depends on import, foreign binder research is more, and the imported binder is high in cost and the product updating speed is slower, so that the updating speed of the cement raw materials in China cannot be considered. Particularly, for some raw materials with high silicon and high iron, the binder in China and abroad can not ensure that the material is pressed into tablets with higher tablet ratio at present.
Disclosure of Invention
The invention aims to provide a solid binder and a preparation method thereof, wherein the solid binder has good dispersibility, can meet the tabletting requirements of cement and various raw materials, and has high yield, low-cost and easily obtained raw materials and low cost.
It is a further object of the present invention to provide the use of a solid binder for powder tabletting, in particular for cement, clinker, raw meal, limestone, sandstone, clay, slag, iron ore, coal fines, silica fume, easy tabletting and to bring the fluorescence test to within the error limits.
The specific technical scheme of the invention is as follows:
the solid binder comprises the following raw materials in parts by weight:
40-60 parts of binder, 30-40 parts of dispersing agent, 1-5 parts of lubricant and 8-15 parts of tackifier.
The binder is selected from one or more of methylcellulose, microcrystalline cellulose or starch.
The viscosity of the methyl cellulose is selected from one of 400 mPas, 1500 mPas or 40000 mPas;
the grain diameter of the microcrystalline cellulose is 20-50 mu m;
the starch is of reagent grade;
the dispersing agent is selected from lactose or galactose;
the lactose is selected from at least one of alpha-lactose monohydrate or anhydrous lactose;
the lubricant is selected from paraffin wax;
the tackifier is selected from polyvinylpyrrolidone, and its average molecular weight is selected from one of 10000 (K13-18), 24000 (K23-27) and 58000 (K29-32).
The binder also comprises an outer coating, and the outer coating coats the solid binder;
the mass of the outer coating is 2-4% of the mass of the binder.
The outer coating is purchased from Beijing Yingmao pharmaceutical Co Ltd as gastric-soluble film coating premix, model ASJ2106014.
The preparation method of the solid binder specifically comprises the following steps:
and (3) stirring and mixing the formula amount of binder, dispersant, lubricant and tackifier.
Preferably, the preparation method comprises the following steps: under the condition of 20-40r/min of rotating speed, firstly mixing the formula amount of binder, the dispersing agent and the binder, firstly stirring clockwise for 10-12min, stopping 1-5min, then stirring anticlockwise for 10-12min, stopping 1-5min, repeating the above operation for 1.5-1.8h, then adding the formula amount of lubricant, firstly stirring clockwise for 10-12min, stopping 1-5min, then stirring anticlockwise for 10-12min, stopping 1-5min, and repeating the above operation for 0.5-0.6 h.
Placing the prepared solid binder in a tablet press to prepare tablets; the tablet has a thickness of 0.4-0.6cm and a diameter of 0.8-1.5cm.
The preparation method also comprises the following steps: coating the surface of the tablet with an outer coating by a coating machine;
the temperature is set to 40 ℃ by a coating machine, and the tablet can be uniformly coated after the operation time is 1-1.2 h.
The solid binder provided by the invention is applied to powder tabletting, and is especially suitable for tabletting and molding of clinker, cement, raw materials, limestone, sandstone, clay, iron ore, slag, silica fume and coal dust in a cement intelligent factory for fluorescence detection.
In the invention, the dispersant acts as: the molecular structure of the selected dispersing agent is a polyhydroxy structure (for example, one molecule of alpha-lactose monohydrate contains eight hydroxyl groups), the dispersing agent can be adsorbed on the surface of a material during grinding, the hydroxyl groups reduce the potential energy of the surface of the powder of the material during grinding, prevent the powder from agglomerating, enhance the fluidity of the powder, ensure that the formed tabletting tablet is uniform, have better repeatability of a fluorescence test result (the repeatability deviation recorded in the embodiment is smaller), and avoid the powder from pasting and grinding.
The adhesive acts as: the selected binder is a high molecular substance which has stronger viscosity and deformability, and when the powder is ground, the long chain structure of the high molecular substance can well adsorb the powder after the molecules are contacted with the powder, and when the powder is pressed, the whole powder can have better compressibility.
In addition, the synergistic effect of the dispersing agent and the binder can ensure that the powder has better fluidity during grinding, and can be uniformly dispersed; the molding has good compressibility when being pressed, and the molding are relatively balanced. The powder has better cohesiveness than the imported binder, strong dispersity, and can be used for molding more difficult-to-mold materials, the fluorescence test error is smaller than that of the imported binder, and the particle size of the powder after grinding is smaller than that of the powder after using the imported binder. The dispersing agent is mainly because the dispersing agent selected by the invention contains abundant hydroxyl groups, the adhesive contains a plurality of methoxy groups, when the powder is ground, the powder is in a dynamic state, long chains of the adhesive are opened, the dispersing agent cannot be adsorbed by the adhesive in a large amount, and the dispersing agent is still adsorbed on the powder of the material by virtue of the action of the hydroxyl groups, so that the fluidity and the dispersibility of the powder are enhanced. When the powder is molded, under the condition of being pressed, the adhesive can form a hydrogen bond with hydroxyl on the dispersing agent, so that the powder is closely connected with excellent compressibility, and the powder cannot rebound to generate cracking after the stress is over.
Compared with the prior art, the solid binder provided by the invention has the advantages that the raw materials are the binder, the dispersing agent, the lubricant and the tackifier which are mutually synergistic, the lubricity and the powder flowability are good, the dispersibility is excellent, the cohesiveness is good, the tabletting requirements of cement and various raw materials can be met, the tablet forming rate is high, the raw materials are low in cost and easy to obtain, and the cost is low. In addition, the solid binder is prepared into tablets, and the tablets are coated with an outer layer, so that the tablets are moisture-proof, easy to transport and capable of being stored in a large amount.
Drawings
FIG. 1 is a particle size distribution of a green charge after addition of an inlet binder;
FIG. 2 is a particle size distribution of a feedstock after addition of the binder of the present invention;
FIG. 3 is a microscopic image of silica fume and sandstone molded with two binders;
FIG. 4 is a photograph of a millstone after grinding blank raw meal and adding two binders in a laboratory;
FIG. 5 is a photograph of the millstone after intelligent factory testing;
FIG. 6 maximum deviation of fluorescence after addition of different materials to the binder of the present invention.
Figure 7 is a molded picture of two binders with different materials added.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions in the embodiments of the present invention will be clearly and completely described in the following in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The test materials, reagents and the like used in the examples described below are commercially available unless otherwise specified.
Those of skill in the art, without any particular mention of the techniques or conditions, may follow the techniques or conditions described in the literature in this field or follow the product specifications.
The invention provides a solid binder which comprises the following raw materials in parts by weight:
40-60 parts of binder, 30-40 parts of dispersing agent, 1-5 parts of lubricant and 8-15 parts of tackifier.
The binder is selected from one or more of methylcellulose, microcrystalline cellulose or starch.
The viscosity of the methyl cellulose is selected from one of 400 mPas, 1500 mPas or 40000 mPas;
the grain diameter of the microcrystalline cellulose is 20-50 mu m;
the starch is of reagent grade;
the dispersing agent is selected from lactose and galactose;
the lactose is selected from at least one of alpha-lactose monohydrate and anhydrous lactose;
the lubricant is selected from paraffin wax;
the tackifier is selected from polyvinylpyrrolidone, and its average molecular weight is selected from one of 10000 (K13-18), 24000 (K23-27) and 58000 (K29-32).
The binder also comprises an outer coating, and the outer coating coats the solid binder;
the mass of the outer coating is 2-4% of the mass of the binder.
The outer coating is purchased from Beijing Yingmao pharmaceutical Co Ltd as gastric-soluble film coating premix, model ASJ2106014.
The preparation method of the solid binder specifically comprises the following steps:
mixing the adhesive, the dispersing agent, the lubricant and the tackifier according to the formula amount.
Preferably, the preparation method comprises the following steps: under the condition of 20-40r/min of rotating speed, firstly mixing the formula amount of binder, the dispersing agent and the binder, firstly stirring clockwise for 10-12min, stopping 1-5min, then stirring anticlockwise for 10-12min, stopping 1-5min, repeating the above operation for 1.5-1.8h, then adding the formula amount of lubricant, firstly stirring clockwise for 10-12min, stopping 1-5min, then stirring anticlockwise for 10-12min, stopping 1-5min, and repeating the above operation for 0.5-0.6 h.
Placing the prepared solid binder in a tablet press to prepare tablets; the tablet has a thickness of 0.4-0.6cm and a diameter of 0.8-1.5cm.
Coating the surface of the tablet with an outer coating layer by a coating machine: the temperature of the coating machine is set to 40 ℃, and the tablet can be uniformly coated after the operation time is 1-1.2 hours.
The solid binder is applied to powder tabletting, and is particularly suitable for tabletting and forming clinker, cement, raw materials, limestone, sandstone, iron ore, slag, silica fume, coal dust and clay in a cement intelligent factory for fluorescence detection.
Example 1
The solid binder comprises binder powder and an outer coating, wherein the binder powder comprises the following raw materials in parts by weight:
35 parts of methylcellulose (viscosity 40000 mPa.s), 5 parts of starch, 5 parts of microcrystalline cellulose (particle size 20 mu m), 30 parts of alpha-lactose monohydrate, 7 parts of galactose, 3 parts of paraffin wax and 10 parts of polyvinylpyrrolidone (molecular weight 58000).
And (3) coating an outer layer: accounting for 2 percent of the mass of the binder powder. The outer coating is provided by Beijing Yingmao pharmaceutical Co.
The preparation method of the solid binder comprises the following steps: mixing the formula amount of binder, the dispersing agent and the binder under the condition of the rotating speed of 30r/min, firstly stirring clockwise for 10min, stopping for 2min, then stirring anticlockwise for 10min, stopping for 2min, repeating the above operation for 1.8h in the whole process, then adding the formula amount of lubricant, firstly stirring clockwise for 10min, stopping for 2min, then stirring anticlockwise for 10min, stopping for 2min, repeating the above operation for 0.5h, and finally obtaining the adhesive.
Placing the prepared solid binder in a tablet press to prepare tablets; the tablet size was 0.4cm in thickness and 1.5cm in diameter.
Coating the surface of the tablet with an outer coating by a coating machine; the temperature is set to 40 ℃ by a coating machine, the tablets can be uniformly coated in the running time of 1.2 hours, the average weight of the coated tablets is 0.3g, and the difference between each tablet is +/-0.01 g.
Intelligent factory test: the main material was uniformly volumetric by adding a dosing cup (18 cc dosing cup, fixed volume) according to the smith inlet device with the adhesive, the number of adhesive patches being set in advance on the system mainframe. Number of binder sheets (overall mass ratio 2-4%): 3 pieces of clinker, 2 pieces of cement, 3 pieces of raw materials, 1 piece of limestone, 3 pieces of sandstone, 3 pieces of iron ore, 3 pieces of slag and 3 pieces of clay.
The binder prepared in example 1 of the present invention and the auxiliary agent purchased from smith, denmark (auxiliary agent provided by the smith inlet device) were used as the imported binder, and the two binders were compared with each other for the tabletting conditions of the different materials as the main materials, the fluorescence test results, and the particle distribution conditions. In the detection process, when the binder and the imported binder are subjected to the same main material experiment, the main materials are the same, the experimental conditions and parameters are the same, and the binders are only different in selection. The fluorescent test conditions are satisfied: the repeatability measured by the pressed powder formed by adding the binder into the same batch of materials after grinding meets the requirement of the fluorescence analysis repeatability limit of GB/T176.
The detection process is as follows: the system host sets the number of the added adhesive in advance, grinding time and rotating speed; the system host sets the number of the added adhesive, grinding time and rotating speed in advance. The adhesive is placed into an adhesive placing port of the intelligent system, and the placing device can control the number and time of the adhesive to be added; the raw materials are automatically sampled, the samples enter a quantitative cup, and redundant samples are pre-ground and cleaned to a grinding disc. The binder and the main raw materials enter a vibration mill of a milling system for milling. The ground material enters an automatic tablet press of the system for molding. And (5) making the slices enter a negative pressure detector, continuously performing fluorescence detection on the qualified slices, and placing unqualified slices in an unqualified product placing area.
Under the same conditions, the binder of the present invention and the inlet binder are in the form of sheets as shown in Table 1 below; v represents that the condition is satisfied, x represents that it is not satisfied; the satisfaction of the sheeting condition means: the formed tablets pass the split test: specifically, the negative pressure of the pressed sheet after adsorption molding is more than or equal to 78mbar (the Smith device is set to 78 mbar).
Table 1 shows a comparison of the sheeting of the binders of the present invention with the inlet binders in an intelligent factory comparison test
Laboratory test: clinker, cement, raw materials, limestone, sandstone, clay, iron ore, coal dust and silica fume are purchased from a white horse cement plant, 30g of the raw materials are uniformly and respectively weighed, and 3 sheets of the binder are uniformly and respectively added (the binder accounts for 3%).
The grinding conditions for laboratory test of the flaking condition are: grinding with a vibration mill (SM-1 vibration mill, inc. of North Aster instrument, dendong) for 60s, tabletting conditions: the ground tablets were formed by tabletting at 30MPa using a tablet press (BP-1 powder press, inc. of North Aster instrument Co., ltd.). The inlet binder was the same as the main material used in the binder test of the present invention, and the experimental conditions were the same as parameters, except for the choice of binder.
The test results are shown in table 2, and v indicates that the condition is satisfied, and x indicates that the condition is not satisfied. The specific standard is as follows: visually observing whether a split situation exists or not, and determining the situation of tiny cracks and flaking of the edge of the tablet by using a polarized light microscope pair, wherein the situations of cracks and flaking are not satisfied by the tablet;
table 2 laboratory test sheeting of different materials
Fig. 3 is a microscopic picture of the laboratory silica fume and sandstone after two binders are added respectively, in fig. 3 a is a picture of the laboratory silica fume after an inlet binder is added, and b is a picture of the sandstone after an inlet binder is added; fig. 3 c is a picture of silica fume with the binder of the present invention added thereto, and d is a picture of sandstone with the binder of the present invention added thereto. In fig. 3, a and c show the middle region of silica fume, and in fig. 3, b and d show the edge region of the sandstone tablet. From the figure, the pressed sheet formed by adding the imported binder into the silica fume has obvious cracks, the edge area of the sandstone is uneven and has some cracks. In contrast, silica fume and sandstone surfaces using the binders of the present invention were smooth and no cracks were found. The above shows that the invention has excellent cohesiveness and wider applicability to cement related materials.
Sticking and grinding conditions: neither the invention nor the inlet binder is sticky to the mill.
Fig. 4 is a photograph of a laboratory mill after grinding blank raw material and adding the binder of example 1, the inlet binder, respectively, and it can be seen from the photograph that the mill surface is stained with a clear raw material without the binder, and this is effectively suppressed after the inlet binder or the binder of the present invention is added.
Fig. 5 is a graph of a millstone after the vibration mill of the intelligent quality control system is disassembled after the intelligent factory test of raw materials, cement, limestone, sandstone, clay, clinker, and iron ore are added with the binder of the present invention, and as can be seen, there is no paste grinding phenomenon using the binder of the present invention.
X-ray fluorescence detection result and error:
the repeatability limit is the requirement of the method according to GB/T176 cement chemistry analysis method, and the following is the fluorescence result of the test after 10 sheets of samples of different materials are molded after the binder of the embodiment 1 is added into a laboratory, so that the requirement of the repeatability limit of GB/T176 is met.
The fluorescent test conditions are satisfied: the maximum deviation of fluorescence data measured by the pressed sheet formed by powder after the same batch of materials are added with the binder for grinding meets the requirement of the repeatability limit of the fluorescence analysis of GB/T176.
Table 3 shows the results of fluorescence detection of the formed pieces of the materials after the binder of the invention is added in laboratory tests, and FIG. 6 shows the maximum deviation of the tests of different elements of each material, wherein the deviation is less than the repeatability limit, and meets the GB/T176 fluorescence detection requirement.
TABLE 3 detection of fluorescence of the tablets of different laboratory materials with the addition of the binders according to the invention
Table 4 shows the fluorescence measurements of the different materials tested in the intelligent plant corresponding to Table 1, wherein these 3 materials only had fluorescence data for the addition of the binder of the invention, since iron ore, slag, sandstone with high silicon content could not be formed after the use of the imported binder.
TABLE 4 fluorescence detection results of different materials tested in intelligent factories
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Table 5 shows the repeatability deviations of the fluorescence data of the different materials in Table 4. From Table 5, it is clear that the repeatability deviations of the binders of the present invention are smaller than those of the imported binders, indicating that the binders of the present invention allow for a more uniform distribution of the formed tablets and exhibit better flowability.
TABLE 5 repeatability bias of fluorescence data for different materials in TABLE 4
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The particle distribution results of the materials after the binder is added in the laboratory are shown in Table 6, the material indexes of the powder are the same, the powder grinding conditions and time are the same, the dosage of the added binder is the same, and the difference is only that the binder is selected.
TABLE 6 powder particle distribution X after grinding the invention and the imported binder in laboratory 50 Data
Material Inlet adhesive X 50 /μm The invention X 50 /μm
Raw material 4.01 3.86
Sandstone 4.86 4.74
Silica fume 6.34 6.30
Clinker material 9.57 9.51
Cement and its preparation method 13.66 13.55
Limestone powder 2.39 2.30
FIG. 1 is a particle size distribution of a green charge after addition of an inlet binder; FIG. 2 shows the particle size distribution of a feedstock after addition of the binder of the present invention.
As can be seen from the table, X of the material to which the binder of the present invention is added 50 Smaller than the addition of the inlet binder, and exhibits superior dispersibility.
Example 2
The solid binder comprises binder powder and an outer coating, wherein the binder powder comprises the following raw materials in parts by weight:
binder powder: 53 parts of methylcellulose (viscosity 400 mPa.s), 38 parts of alpha-lactose monohydrate, 1 part of paraffin and 8 parts of polyvinylpyrrolidone (average molecular weight 10000).
And (3) coating an outer layer: accounting for 4 percent of the mass of the binder powder. The outer coating is provided by Beijing Yingmao pharmaceutical Co.
The preparation method of the solid binder comprises the following steps: mixing the formula amount of binder, the dispersing agent and the binder under the condition of the rotating speed of 30r/min, firstly stirring clockwise for 10min, stopping for 2min, then stirring anticlockwise for 10min, stopping for 2min, repeating the above operation for 1.8h in the whole process, then adding the formula amount of lubricant, firstly stirring clockwise for 10min, stopping for 2min, then stirring anticlockwise for 10min, stopping for 2min, repeating the above operation for 0.5h, and finally obtaining the adhesive.
Placing the prepared solid binder in a tablet press to prepare tablets; the tablet size was 0.5cm in thickness and 1.0cm in diameter.
Coating the surface of the tablet with an outer coating by a coating machine; the temperature is set to 40 ℃ by a coating machine, the tablets can be uniformly coated in the running time of 1h, the average weight of the coated tablets is 0.3g, and the difference between each tablet is +/-0.01 g.
Intelligent factory test: the main material was uniformly volumetric by adding a dosing cup (18 cc dosing cup, fixed volume) according to the smith inlet device with the adhesive, the number of adhesive patches being set in advance on the system mainframe. Number of binder sheets (overall mass ratio 2-4%): 3 pieces of raw materials, 3 pieces of clinker, 2 pieces of cement, 3 pieces of sandstone and 1 piece of limestone.
The binder prepared in example 2 of the present invention was compared with the auxiliary agent purchased from denmark smith (auxiliary agent provided by the smith inlet device) as an inlet binder against the tabletting conditions, fluorescence test results, and particle distribution conditions of the different materials of the cement as a main material. In the detection process, when the binder and the imported binder are subjected to the same main material experiment, the main materials are the same, the experimental conditions and parameters are the same, and the binders are only different in selection. The fluorescent test conditions are satisfied: the repeatability measured by the pressed powder formed by adding the binder into the same batch of materials after grinding meets the requirement of the fluorescence analysis repeatability limit of GB/T176.
The detection process is as follows: the system host sets the number of the added adhesive in advance, grinding time and rotating speed; the system host sets the number of the added adhesive, grinding time and rotating speed in advance. The adhesive is placed into an adhesive placing port of the intelligent system, and the placing device can control the number and time of the adhesive to be added; the raw materials are automatically sampled, the samples enter a quantitative cup, and redundant samples are pre-ground and cleaned to a grinding disc. The binder and the main raw materials enter a vibration mill of a milling system for milling. The ground material enters an automatic tablet press of the system for molding. And (5) making the slices enter a negative pressure detector, continuously performing fluorescence detection on the qualified slices, and placing unqualified slices in an unqualified product placing area.
The sheeting conditions were compared as follows:
the inventive binder and inlet binder were sheeted under the same conditions as shown in table 7 below; v represents that the condition is satisfied, x represents that it is not satisfied; the satisfaction of the sheeting condition means: the formed tablets pass the split test: specifically, the negative pressure of the pressed sheet after adsorption molding is more than or equal to 78mbar (the Smith device is set to 78 mbar).
Table 7 sheeting of five materials with different binders at intelligent plants
Material Inlet adhesive Inventive example 2 adhesive
Raw material √ √
Clinker material √ √
Cement and its preparation method √ √
Sandstone √ √
Limestone powder √ √
Fig. 7 shows the case of the intelligent factory tabletting of example 2 for five materials, five columns of 3 tablets each, from left to right, of five materials, raw material, clinker, cement, sandstone and limestone. The five materials are qualified in negative pressure detection, the molding surface is smooth, and no cracking condition exists.
Table 8 shows the fluorescence measurement results of the tablets formed by the inlet binder and the binder of example 2 of the present invention in the intelligent factory for five materials, six tablets were formed for each material, 3 tablets of the inlet binder and 3 tablets of example 2 of the present invention were added.
TABLE 8 fluorescence detection results of different materials tested in intelligent factories
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Table 9 shows the maximum deviation of fluorescence detection for the two binders used for the different materials in Table 8, and it is clear from the table that the maximum deviation of fluorescence detection using the materials of the present invention is smaller than that using the inlet binders, indicating that the tablets formed using the present invention are more uniform.
Table 9 maximum deviation of fluorescence data for different materials in table 8
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Particle size distribution: table 10 shows the particle size X of the above five materials after grinding 50 The data, the material index of grinding is the same, the grinding condition and time are the same, the dosage of the added binder is the same, and the difference is only that the binder is selected. It can be seen that the powder of example 2 of the present invention has a smaller particle size, indicating that it is more sufficiently ground.
TABLE 10 particle size X of the above materials 50 Data
Material Inlet adhesive X 50 /μm Inventive example 2X 50 /μm
Raw material 3.85 3.78
Clinker material 9.60 9.56
Cement and its preparation method 8.00 7.96
Sandstone 4.11 4.02
Limestone powder 2.65 2.41
The absence of a paste-like appearance of the abrasive disc after application of the adhesive of example 2 of the present invention was observed with the naked eye.
Example 3
The solid binder comprises binder powder and an outer coating, wherein the binder powder comprises the following raw materials in parts by weight:
binder powder: 55 parts of methylcellulose (viscosity 1500 mPa.s), 5 parts of microcrystalline cellulose (particle size 40 μm), 30 parts of alpha-lactose monohydrate, 5 parts of paraffin wax and 15 parts of polyvinylpyrrolidone (molecular weight 24000).
And (3) coating an outer layer: accounting for 3 percent of the mass of the binder powder. The outer coating is provided by Beijing Yingmao pharmaceutical Co.
The preparation method of the solid binder comprises the following steps: mixing the formula amount of binder, the dispersing agent and the binder under the condition of the rotating speed of 30r/min, firstly stirring clockwise for 10min, stopping for 2min, then stirring anticlockwise for 10min, stopping for 2min, repeating the above operation for 1.8h in the whole process, then adding the formula amount of lubricant, firstly stirring clockwise for 10min, stopping for 2min, then stirring anticlockwise for 10min, stopping for 2min, repeating the above operation for 0.5h, and finally obtaining the adhesive.
Placing the prepared solid binder in a tablet press to prepare tablets; the tablet size was 0.6cm in thickness and 0.8cm in diameter.
Coating the surface of the tablet with an outer coating by a coating machine; the temperature is set to 40 ℃ by a coating machine, the tablets can be uniformly coated in the running time of 1.2 hours, the average weight of the coated tablets is 0.3g, and the difference between each tablet is +/-0.01 g.
The binder prepared in example 3 of the present invention was compared with the auxiliary agent purchased from denmark smith (auxiliary agent provided by smith inlet equipment) for the above-mentioned tabletting conditions of different materials of cement as main material, fluorescence test results, and particle distribution conditions, respectively. In the detection process, when the binder and the imported binder are subjected to the same main material experiment, the main materials are the same, the experimental conditions and parameters are the same, and the binders are only different in selection. The fluorescent test conditions are satisfied: the repeatability measured by the pressed powder formed by adding the binder into the same batch of materials after grinding meets the requirement of the fluorescence analysis repeatability limit of GB/T176.
The grinding conditions for laboratory test of the flaking condition are: grinding with a vibration mill (SM-1 vibration mill, inc. of North Aster instrument, dendong) for 60s, tabletting conditions: the ground tablets were formed by tabletting at 30MPa using a tablet press (BP-1 powder press, inc. of North Aster instrument Co., ltd.). The inlet binder was the same as the main material used in the binder test of the present invention, and the experimental conditions were the same as parameters, except for the choice of binder.
Sheeting test results:
as shown in table 11, v indicates that the condition is satisfied, and x indicates that the condition is not satisfied. The specific standard is as follows: and observing the condition of no splinter by naked eyes, wherein the condition of splinter is not satisfied in order to satisfy the condition. The results show that inventive example 3 allows more material to be shaped and exhibits better adhesion.
Table 11 laboratory sheeting after the addition of inlet binders and inventive example 3 to different materials
Material Inlet adhesive Inventive example 3 adhesive
Raw material √ √
Clinker material √ √
Cement and its preparation method √ √
Sandstone √ √
Limestone powder √ √
Iron ore × √
Silica fume × √
X-ray fluorescence detection result and error:
fluorescence detection according to GB/T176 method for Cement chemistry analysis, the repeatability limit is the requirement of the method, and the following is the fluorescence result of the test after 3 sheets of samples of different materials are molded by adding an inlet binder and the binder ground in an example 3 in a laboratory, so that the requirement of GB/T176 repeatability limit is met. The fluorescent test conditions are satisfied: the repeatability measured by the pressed powder formed by adding the binder into the same batch of materials after grinding meets the requirement of the fluorescence analysis repeatability limit of GB/T176.
Table 12 shows the results of fluorescence measurements of the tablets of the invention after the addition of the binder to the different materials in laboratory tests (same test conditions), wherein silica fume and iron ore were not formable using the imported binder, all with the addition of the fluorescence data of the invention. Table 13 shows the maximum deviation of the tests of different elements of each material, and the deviation is smaller than the repeatability limit and meets the GB/T176 fluorescence detection requirement.
Table 12 laboratory fluorescence measurements after addition of inlet binders and inventive example 3 to different materials
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TABLE 13 maximum deviation of fluorescence data in TABLE 12
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Particle distribution:table 14 shows the particle size X of the above materials after grinding with different binders 50 The data, the material index of grinding is the same, the grinding condition and time are the same, the dosage of the added binder is the same, and the difference is only that the binder is selected.
Table 14 particle size X of the corresponding materials in Table 12 after grinding with different binders 50 Data
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The results show that the grinding particle size is smaller after the binder of the invention is used, which indicates that the grinding is more sufficient by using the binder of the invention.

Claims (4)

1. The solid binder is characterized by comprising the following raw materials in parts by weight:
40-60 parts of binder, 30-40 parts of dispersing agent, 1-5 parts of lubricant and 8-15 parts of tackifier;
the binder is one or more selected from methylcellulose, microcrystalline cellulose or starch;
the dispersing agent is selected from lactose or galactose;
the lactose is selected from alpha-lactose monohydrate;
the lubricant is selected from paraffin wax;
the tackifier is selected from polyvinylpyrrolidone.
2. The solid binder of claim 1 wherein the binder further comprises an outer coating, the outer coating having a mass of 2-4% of the mass of the binder.
3. A method for preparing the solid binder according to claim 1, wherein the preparation method specifically comprises the following steps:
mixing the adhesive, the dispersing agent, the lubricant and the tackifier according to the formula amount.
4. Use of a solid binder according to claim 1 or 2 for powder tabletting.
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JPH03132326A (en) * 1989-10-19 1991-06-05 Mitsubishi Kasei Corp Manufacture of laminated film or laminated sheet
TW507005B (en) * 1999-05-11 2002-10-21 Merck Patent Gmbh Grinding aids for x-ray fluorescence analysis
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