CN113388341A - 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
CN113388341A
CN113388341A CN202110671578.XA CN202110671578A CN113388341A CN 113388341 A CN113388341 A CN 113388341A CN 202110671578 A CN202110671578 A CN 202110671578A CN 113388341 A CN113388341 A CN 113388341A
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binder
powder
solid binder
solid
tablets
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CN113388341B (en
Inventor
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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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J101/00Adhesives based on cellulose, modified cellulose, or cellulose derivatives
    • C09J101/08Cellulose derivatives
    • C09J101/26Cellulose ethers
    • C09J101/28Alkyl ethers
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02Non-macromolecular additives
    • C09J11/06Non-macromolecular additives organic
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/08Macromolecular additives
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q

Abstract

The invention provides a solid binder and a preparation method and application thereof, wherein raw materials comprise a binder, a dispersing agent, a lubricant and a tackifier, and the raw materials are cooperated with each other, so that the solid binder has good lubricity and powder flowability, excellent dispersibility and good cohesiveness, can meet the tabletting requirements of cement and various raw materials, and has the advantages of high yield, cheap and easily available raw materials and low cost. In addition, the solid binder is prepared into tablets, and the tablets are coated with the solid binder, so that the tablets are moisture-proof, easy to transport and capable of being stored in large quantities.

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 and a preparation method and application thereof.
Background
The powder tabletting method has the advantages of high analysis speed, wide detection range, high accuracy, simple operation and the like, and becomes a preferred sample preparation method for tabletting detection in the cement industry, but has the defects of poor powder flowability, large tablet weight difference, easy cracking of powder tabletting and the like, so that the application of the process is limited to a certain extent.
With the change of mixed materials in the cement industry and the promotion of market demand, the requirement on the binder is higher and higher. The raw materials in the cement industry are rich, the caking property and the dispersibility of different materials are different, and the tabletting binder needs to take the dispersibility, the caking property, the lubricity and the powder flowability of the materials into consideration. The liquid binder is not easy to be completely dispersed in the powder, the binding effect is limited, and the liquid can be evaporated during the grinding process to cause the quality change of a sample so as to influence the results of tests such as fluorescence and the like, so the solid binder is preferably considered in the cement industry at present.
At present, solid binders used in the cement industry mostly depend on import, foreign binders are researched more frequently, and the research is from the earliest compound of hydroxyalkylamine and lignin derivatives to the later triethanolamine and deeper modified compounds, but the imported binders are high in cost and the product updating is slower, and the updating speed of domestic cement raw materials cannot be considered. Particularly for some high-silicon and high-iron raw materials, the prior binding agent in China or abroad can not ensure that the material tabletting has higher tabletting rate.
Disclosure of Invention
The invention aims to provide a solid binder and a preparation method thereof, the solid binder has good dispersibility, can meet the tabletting requirements of cement and various raw materials, and has high yield, cheap and easily obtained raw materials and low cost.
Another object of the present invention is to provide the use of a solid binder for powder tableting, in particular for cement, clinker, raw meal, limestone, sandstone, clay, slag, iron ore, coal dust, silica fume, which is easy to tablet and allows fluorescence testing within error.
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 dispersant, 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 reagent grade;
the dispersant 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;
the tackifier is selected from polyvinylpyrrolidone, and the average molecular weight of the polyvinylpyrrolidone 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 wraps the solid binder;
the mass of the outer coating is 2-4% of that of the binder.
The outer coating is purchased from a gastric-soluble film coating premix of Beijing Engramme pharmaceutical Co., Ltd, model ASJ 2106014.
The preparation method of the solid binder comprises the following specific steps:
and stirring and mixing the binder, the dispersant, the lubricant and the tackifier according to the formula ratio.
Preferably, the preparation method comprises the following steps: under the condition of the rotating speed of 20-40r/min, firstly mixing the adhesive, the dispersant and the tackifying adhesive according to the formula amount, stopping stirring for 1-5min after stirring clockwise for 10-12min, then stirring anticlockwise for 10-12min, stopping stirring for 1-5min, repeating the above operations for 1.5-1.8h totally, then adding the lubricant according to the formula amount, stopping stirring clockwise for 10-12min, then stopping stirring for 1-5min, then stirring anticlockwise for 10-12min, stopping stirring for 1-5min, repeating the above operations for 0.5-0.6h totally, and thus obtaining the adhesive.
Putting the prepared solid binder into a tablet press to prepare tablets; the tablet size is 0.4-0.6cm in thickness and 0.8-1.5cm in diameter.
The preparation method also comprises the following steps: coating the surface of the tablet with an outer coating by a coating machine;
the coating machine is used for setting the temperature at 40 ℃ and the running time at 1-1.2h, and tablets can be uniformly coated.
The invention provides an application of a solid binder, which is used for powder tabletting, and is particularly suitable for tabletting and forming clinker, cement, raw meal, limestone, sandstone, clay, iron ore, slag, silica fume and coal powder in a cement intelligent factory for fluorescence detection.
In the invention, the dispersant functions as follows: the molecular structures of the selected dispersing agents are all polyhydroxy structures (for example, one molecule of alpha-lactose monohydrate contains eight hydroxyl groups), the dispersing agents can be adsorbed on the surface of a material during grinding, and the hydroxyl groups reduce the surface potential energy of the material powder during grinding, prevent the powder from agglomerating, enhance the flowability of the powder, enable the formed tablet to be uniform, enable the repeatability of a fluorescence test result to be better (the repeatability deviation recorded in the embodiment is smaller), and avoid the phenomenon of powder pasting and grinding.
The function of the binder: the selected binder is a high molecular substance which has strong viscosity and deformability, and when the powder is ground, after molecules are contacted with the powder, the long-chain structure of the binder can well adsorb the powder, so that the whole powder has good compressibility when being pressed.
In addition, the synergistic action 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 pressed, and the two are relatively balanced. The powder has better caking property and strong dispersibility than the imported caking agent, and shows that more difficult-to-mold materials can be molded, the fluorescence test error is smaller than that of the imported caking agent, and the particle size of the ground powder is smaller than that of the imported caking agent. The dispersing agent selected by the invention contains abundant hydroxyl, the binder contains a plurality of methoxyl, the powder is in a dynamic state during grinding, the long chain of the binder is opened, the dispersing agent cannot be greatly adsorbed by the binder, and the dispersing agent is still adsorbed on the material powder by virtue of the action of the hydroxyl, so that the flowability and the dispersibility of the powder are enhanced. During molding, under the condition of pressure, the binder can form hydrogen bonds with hydroxyl groups on the dispersing agent, so that the powder is closely associated with excellent compressibility, and the powder cannot rebound to crack after the pressure is applied.
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 lubricating agent and the tackifier which are mutually cooperated, the lubricating property 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 tabletting rate is high, the raw materials are cheap and easy to obtain, and the cost is low. In addition, the solid binder is prepared into tablets, and the tablets are coated with the solid binder, so that the tablets are moisture-proof, easy to transport and capable of being stored in large quantities.
Drawings
FIG. 1 is a graph showing the particle size distribution of green material after the addition of an inlet binder;
FIG. 2 is a particle size distribution of a feedstock after addition of a binder of the present invention;
FIG. 3 is a microscopic picture of silica fume and sandstone after being formed by adding two binders;
FIG. 4 is a photograph of a laboratory mill grinding blank raw material and a millstone after two binders have been added;
FIG. 5 is a picture of a grinding disc after an intelligent factory test;
FIG. 6 shows the maximum deviation of fluorescence of different materials after the addition of the binder according to the invention.
Fig. 7 is a formed picture of two binders with different materials added.
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.
Test materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
The specific techniques or conditions not specified in the examples can be performed according to the techniques or conditions described in the literature in the field or according to the product specification.
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 dispersant, 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 reagent grade;
the dispersant 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;
the tackifier is selected from polyvinylpyrrolidone, and the average molecular weight of the polyvinylpyrrolidone 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 wraps the solid binder;
the mass of the outer coating is 2-4% of that of the binder.
The outer coating is purchased from a gastric-soluble film coating premix of Beijing Engramme pharmaceutical Co., Ltd, model ASJ 2106014.
The preparation method of the solid binder comprises the following specific steps:
and stirring and mixing the binder, the dispersant, the lubricant and the tackifier according to the formula ratio.
Preferably, the preparation method comprises the following steps: under the condition of the rotating speed of 20-40r/min, firstly mixing the adhesive, the dispersant and the tackifying adhesive according to the formula amount, stopping stirring for 1-5min after stirring clockwise for 10-12min, then stirring anticlockwise for 10-12min, stopping stirring for 1-5min, repeating the above operations for 1.5-1.8h totally, then adding the lubricant according to the formula amount, stopping stirring clockwise for 10-12min, then stopping stirring for 1-5min, then stirring anticlockwise for 10-12min, stopping stirring for 1-5min, repeating the above operations for 0.5-0.6h totally, and thus obtaining the adhesive.
Putting the prepared solid binder into a tablet press to prepare tablets; the tablet has a thickness of 0.4-0.6cm and a diameter of 0.8-1.5 cm.
Coating the surface of the tablet with an outer coating by a coating machine: the coating machine is set at 40 deg.C, and the operation time is 1-1.2 hr.
The solid binder is applied to powder tabletting, and is particularly suitable for tabletting and molding clinker, cement, raw meal, limestone, sandstone, iron ore, slag, silica fume, coal powder and clay in a cement intelligent factory for fluorescence detection.
Example 1
The solid binder comprises a binder powder and an outer coating, wherein the binder powder comprises the following raw materials in parts by weight:
35 parts of methyl cellulose (viscosity 40000 mPas), 5 parts of starch, 5 parts of microcrystalline cellulose (particle size of 20 mu m), 30 parts of alpha-lactose monohydrate, 7 parts of galactose, 3 parts of paraffin and 10 parts of polyvinylpyrrolidone (molecular weight 58000).
Coating the outer layer: accounting for 2 percent of the mass of the binder powder. The outer coating is provided by Beijing Engramme pharmaceutical Co.
The preparation method of the solid binder comprises the following steps: under the condition of the rotating speed of 30r/min, firstly mixing the adhesive, the dispersing agent and the tackifying adhesive according to the formula amount, stirring clockwise for 10min, stopping for 2min, then stirring anticlockwise for 10min, stopping for 2min, repeating the above operations, wherein the whole process is 1.8h, then adding the lubricant according to the formula amount, stirring clockwise for 10min, stopping for 2min, then stirring anticlockwise for 10min, stopping for 2min, and repeating the above operations for 0.5 h.
Putting the prepared solid binder into a tablet press to prepare tablets; the tablet size is 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 operation time is 1.2h, the tablets can be uniformly coated, the average weight of the coated tablets is 0.3g, and the difference of each tablet is +/-0.01 g.
Intelligent factory test: the adhesive is added according to the Smith import equipment, the main material is unified in volume by adding the quantitative cup (18cc quantitative cup, fixed volume), and the number of adhesive pieces is set before the system mainframe. The number of the binder pieces (the whole mass accounts for 2-4%): adding 3 pieces of clinker, 2 pieces of cement, 3 pieces of raw material, 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 purchased from smith in denmark (auxiliary provided with the smith import equipment) were used as imported binders, and the two binders were respectively used for tabletting of different materials as main materials, and the fluorescence test results and particle distribution were compared. In the detection process, when the binder and the imported binder are subjected to the same main material experiment, the main materials are selected to be the same, the experiment conditions and parameters are the same, and only the binder is selected to be different. The fluorescent test conditions are satisfied: the repeatability of the pressed sheet formed by powder ground by adding the same batch of material into the binder meets the requirement of the fluorescent analysis repeatability limit of GB/T176.
The detection process is as follows: the system host sets the number of pieces added with the binder, the grinding time and the rotating speed in advance; the system host sets the number of pieces of the added binder, the grinding time and the rotating speed in advance. The adhesive is put into an adhesive placing port of the intelligent system, and the placing device can control the number and time of adding the adhesive; the raw material is automatically sampled, the sample enters the quantitative cup, and the redundant sample is pre-ground and cleaned by the grinding disc. And the adhesive and the main raw material enter a vibration mill of a grinding system for grinding. The milled material is fed into an automatic tabletting machine of the system for forming. And (4) enabling the tablets to enter a negative pressure detection machine, continuously carrying out fluorescence detection on qualified tablets, and placing unqualified tablets into an unqualified product placing area.
The inventive binders and the imported binders were sheeted under the same conditions, as shown in table 1 below; v represents that the condition is satisfied, and x represents that the condition is not satisfied; the condition of meeting the slicing condition is that: the molded tablets passed the splinter test: in particular to a tablet after being absorbed and molded, so that the negative pressure of the tablet is more than or equal to 78mbar (the Smith device is set to be 78 mbar).
Table 1 shows the comparative flaking conditions of the inventive adhesive and the imported adhesive in the intelligent factory comparative test
Figure BDA0003119503990000051
Laboratory tests: clinker, cement, raw meal, limestone, sandstone, clay, iron ore, coal powder and silica fume are purchased from a white horse cement factory, the raw materials are respectively weighed as 30g as main materials, and 3 pieces of binder are added in a unified way (the binder accounts for 3 percent).
The grinding conditions of the tablet forming condition tested by the laboratory are as follows: grinding for 60s with a vibration mill (model SM-1 vibration mill grinder, dandongbei yuan instruments ltd.), tabletting conditions: the ground tablets were tabletted and formed at 30MPa using a tablet press (BP-1 type powder press, dan northeast aster instruments ltd). The inlet binder is the same as the main material used in the binder test of the invention, and the experimental condition parameters are the same, and the difference is only in the selection of the binder.
The test results are shown in table 2, where √ denotes that the condition is satisfied, and ×. denotes that the condition is not satisfied. The specific standard is as follows: observing the situation of existence of the cracks by naked eyes, and determining the situations of fine cracks and the warping of the edge of the tabletting by using a polarizing microscope pair, wherein the situations of existence of the cracks and the warping are that the tabletting does not meet the conditions;
TABLE 2 laboratory testing of different materials for flaking
Figure BDA0003119503990000061
FIG. 3 is a micrograph of laboratory silica fume and sandstone with two binders added respectively, wherein a in FIG. 3 is a picture of silica fume with an imported binder added thereto, and b is a picture of sandstone with an imported binder added thereto; in fig. 3, c is a picture of silica fume added with the binder of the present invention, and d is a picture of sandstone added with the binder of the present invention. In fig. 3, a and c show the silica fume middle region, and b and d show the sandstone tablet edge region in fig. 3. The figure shows that the pressed sheet formed by adding the imported adhesive into the silica fume has obvious cracks, and the sandstone edge area is uneven and has some cracks. In contrast, silica fume and sandstone surfaces using the binder of the present invention were flat and no cracks were found. The invention has the advantages of excellent caking property and wider forming applicability to cement-related materials.
Sticking and grinding conditions: both the present invention and the imported adhesive are not sticky.
Fig. 4 is a picture of a laboratory millstone after grinding blank raw materials in a laboratory and adding the binder and the imported binder of example 1 respectively, and the picture shows that the surface of the millstone is stained with obvious raw materials when the binder is not added, and the situation is effectively restrained after the imported binder or the binder of the invention is added.
Fig. 5 is a grinding disc picture after the vibration mill of the intelligent quality control system is disassembled after the binder of the invention is added into the experimental raw materials, cement, limestone, sandstone, clay, clinker and iron ore of the intelligent factory, and the grinding is finished completely, and the picture shows that the phenomenon of grinding is not generated by using the binder of the invention.
X-ray fluorescence detection results and errors:
the fluorescent detection is carried out according to GB/T176 'cement chemical analysis method', the repeatability limit is the requirement of the method, and the following is a fluorescent result of a test after samples of different materials are added into a laboratory, and the samples are ground by the binder in the embodiment 1 and are molded into 10 pieces, so that the GB/T176 repeatability limit requirement is met.
The fluorescent test conditions are satisfied as follows: the maximum deviation of fluorescence data measured by tabletting of powder formed by adding the binder and grinding the same batch of materials meets the requirement of the fluorescent analysis repeatability limit of GB/T176.
Table 3 shows the results of fluorescence measurements of different materials after addition of the binder of the present invention in laboratory tests, and FIG. 6 shows the maximum deviation of the measurements of different elements of each material, which shows that the deviations are smaller than the repeatability limit and satisfy the GB/T176 fluorescence detection requirements.
TABLE 3 results of fluorescence measurements of patches of laboratory different materials added with binders according to the invention
Figure BDA0003119503990000071
Figure BDA0003119503990000081
Figure BDA0003119503990000091
Table 4 shows the fluorescence measurements of the different materials tested in the intelligent plant corresponding to table 1, wherein the 3 materials only have fluorescence data of the binder of the present invention, because iron ore, slag, and sandstone with high silicon content cannot be formed using the imported binder.
TABLE 4 fluorescence detection results of different materials tested in Intelligent factory
Figure BDA0003119503990000092
Figure BDA0003119503990000101
Figure BDA0003119503990000111
Table 5 shows the repeatability deviation of the fluorescence data for the different materials in table 4. from table 5, it can be seen that the repeatability deviation using the binder of the present invention is less than that of the imported binder, indicating that the binder of the present invention allows the molded tablets to be distributed more uniformly and exhibit better flow properties.
TABLE 5 variation in reproducibility of fluorescence data for different materials in TABLE 4
Figure BDA0003119503990000112
Figure BDA0003119503990000121
Figure BDA0003119503990000131
The particle distribution results of the materials after grinding, which are added with the binder in the laboratory, are shown in table 6, the ground materials have the same index, the grinding conditions and time are the same, the amount of the added binder is the same, and the difference is only in the selection of the binder.
Table 6 powder particle distribution X of the invention after grinding with imported binder in laboratory50Data of
Material Imported binder X50/μm Invention X50/μm
Raw material 4.01 3.86
Sandstone 4.86 4.74
Silica fume 6.34 6.30
Clinker 9.57 9.51
Cement 13.66 13.55
Limestone 2.39 2.30
FIG. 1 is a graph showing the particle size distribution of green material after the addition of an inlet binder; FIG. 2 is a particle size distribution of a feedstock with the addition of a binder of the present invention.
As can be seen from the table, X is the amount of the material to which the binder of the present invention is added50Is smaller than that of the imported adhesive, and shows excellent dispersibility.
Example 2
The solid binder comprises a binder powder and an outer coating, wherein the binder powder comprises the following raw materials in parts by weight:
binder powder: 53 parts of methyl cellulose (viscosity is 400 mPas), 38 parts of alpha-lactose monohydrate, 1 part of paraffin and 8 parts of polyvinylpyrrolidone (average molecular weight is 10000).
Coating the outer layer: accounting for 4 percent of the mass of the binder powder. The outer coating is provided by Beijing Engramme pharmaceutical Co.
The preparation method of the solid binder comprises the following steps: under the condition of the rotating speed of 30r/min, firstly mixing the adhesive, the dispersing agent and the tackifying adhesive according to the formula amount, stirring clockwise for 10min, stopping for 2min, then stirring anticlockwise for 10min, stopping for 2min, repeating the above operations, wherein the whole process is 1.8h, then adding the lubricant according to the formula amount, stirring clockwise for 10min, stopping for 2min, then stirring anticlockwise for 10min, stopping for 2min, and repeating the above operations for 0.5 h.
Putting the prepared solid binder into a tablet press to prepare tablets; the tablet size is 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 operation time is 1h, the tablets can be uniformly coated, the average weight of the coated tablets is 0.3g, and the difference of each tablet is +/-0.01 g.
Intelligent factory test: the adhesive is added according to the Smith import equipment, the main material is unified in volume by adding the quantitative cup (18cc quantitative cup, fixed volume), and the number of adhesive pieces is set before the system mainframe. The number of the binder pieces (the whole mass accounts for 2-4%): adding 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 and the auxiliary purchased from smith in denmark (auxiliary provided with the smith import equipment) as imported binders were compared with the tabletting condition, fluorescence test result and particle distribution condition of different materials of the cement as the 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 selected to be the same, the experiment conditions and parameters are the same, and only the binder is selected to be different. The fluorescent test conditions are satisfied: the repeatability of the pressed sheet formed by powder ground by adding the same batch of material into the binder meets the requirement of the fluorescent analysis repeatability limit of GB/T176.
The detection process is as follows: the system host sets the number of pieces added with the binder, the grinding time and the rotating speed in advance; the system host sets the number of pieces of the added binder, the grinding time and the rotating speed in advance. The adhesive is put into an adhesive placing port of the intelligent system, and the placing device can control the number and time of adding the adhesive; the raw material is automatically sampled, the sample enters the quantitative cup, and the redundant sample is pre-ground and cleaned by the grinding disc. And the adhesive and the main raw material enter a vibration mill of a grinding system for grinding. The milled material is fed into an automatic tabletting machine of the system for forming. And (4) enabling the tablets to enter a negative pressure detection machine, continuously carrying out fluorescence detection on qualified tablets, and placing unqualified tablets into an unqualified product placing area.
The sheeting was compared as follows:
the inventive binder and the imported binder were sheeted under the same conditions, as shown in table 7 below; v represents that the condition is satisfied, and x represents that the condition is not satisfied; the condition of meeting the slicing condition is that: the molded tablets passed the splinter test: in particular to a tablet after being absorbed and molded, so that the negative pressure of the tablet is more than or equal to 78mbar (the Smith device is set to be 78 mbar).
TABLE 7 flaking after adding different binders to the five materials in the Intelligent factory
Material Imported binder Inventive example 2 Binder
Raw material
Clinker
Cement
Sandstone
Limestone
Fig. 7 shows the situation of tabletting five materials in an intelligent factory according to example 2, wherein five rows of the five materials are provided, each row comprises 3 pieces, and the five materials comprise raw materials, clinker, cement, sandstone and limestone from left to right. The five materials are qualified through negative pressure detection, the molding surface is flat, and the cracking condition is not generated.
Table 8 shows the fluorescent test results of the tablet after the imported binder and the binder of example 2 of the present invention were molded in an intelligent factory for five materials, each of which was molded into six sheets, 3 sheets of the imported binder were added, and 3 sheets of the binder of example 2 of the present invention were added.
TABLE 8 fluorescence measurements of different materials tested in an Intelligent factory
Figure BDA0003119503990000151
Figure BDA0003119503990000161
Table 9 shows the maximum fluorescence detection deviations for the different materials of Table 8 using two binders, which indicates that the maximum fluorescence detection deviation for the materials of the invention is less than that for the imported binders, indicating that the tablets formed using the invention are more uniform.
TABLE 9 maximum deviation of fluorescence data repetition for different materials in TABLE 8
Figure BDA0003119503990000162
Figure BDA0003119503990000171
Particle size distribution: table 10 shows the particle size X of the five materials after grinding50The data, the material index of the grinding is the same, the grinding condition and time are the same, the dosage of the added caking agent is the same, and the difference is only in the cakingAnd (4) selecting an agent. It can be seen that the powder of example 2 using the present invention has a smaller particle size, indicating that it is more sufficiently ground.
TABLE 10 particle size X of the above materials50Data of
Material Imported binder X50/μm Inventive example 2X50/μm
Raw material 3.85 3.78
Clinker 9.60 9.56
Cement 8.00 7.96
Sandstone 4.11 4.02
Limestone 2.65 2.41
The abrasive discs after application of the adhesive of example 2 of the invention were visually observed to have no smearing.
Example 3
The solid binder comprises a binder powder and an outer coating, wherein the binder powder comprises the following raw materials in parts by weight:
binder powder: 55 parts of methyl cellulose (viscosity 1500 mPas), 5 parts of microcrystalline cellulose (particle size 40 mu m), 30 parts of alpha-lactose monohydrate, 5 parts of paraffin and 15 parts of polyvinylpyrrolidone (molecular weight 24000).
Coating the outer layer: accounting for 3 percent of the mass of the binder powder. The outer coating is provided by Beijing Engramme pharmaceutical Co.
The preparation method of the solid binder comprises the following steps: under the condition of the rotating speed of 30r/min, firstly mixing the adhesive, the dispersing agent and the tackifying adhesive according to the formula amount, stirring clockwise for 10min, stopping for 2min, then stirring anticlockwise for 10min, stopping for 2min, repeating the above operations, wherein the whole process is 1.8h, then adding the lubricant according to the formula amount, stirring clockwise for 10min, stopping for 2min, then stirring anticlockwise for 10min, stopping for 2min, and repeating the above operations for 0.5 h.
Putting the prepared solid binder into a tablet press to prepare tablets; the tablet size is 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 operation time is 1.2h, the tablets can be uniformly coated, the average weight of the coated tablets is 0.3g, and the difference of each tablet is +/-0.01 g.
The binder prepared in example 3 of the present invention and the auxiliary agent purchased from smith in denmark (auxiliary agent provided with smith import equipment) were compared with the above-mentioned cement as the main material in terms of the tabletting condition, the fluorescence test result and the particle distribution condition, respectively. In the detection process, when the binder and the imported binder are subjected to the same main material experiment, the main materials are selected to be the same, the experiment conditions and parameters are the same, and only the binder is selected to be different. The fluorescent test conditions are satisfied: the repeatability of the pressed sheet formed by powder ground by adding the same batch of material into the binder meets the requirement of the fluorescent analysis repeatability limit of GB/T176.
The grinding conditions of the tablet forming condition tested by the laboratory are as follows: grinding for 60s with a vibration mill (model SM-1 vibration mill grinder, dandongbei yuan instruments ltd.), tabletting conditions: the ground tablets were tabletted and formed at 30MPa using a tablet press (BP-1 type powder press, dan northeast aster instruments ltd). The inlet binder is the same as the main material used in the binder test of the invention, and the experimental condition parameters are the same, and the difference is only in the selection of the binder.
Results of the sheeting test:
as shown in table 11, √ denotes that the condition is satisfied, and × denotes that it is not satisfied. The specific standard is as follows: and observing the condition of no splinter by naked eyes to meet the condition, and the condition of splinter is not met. The results show that example 3 of the present invention allows more material to be formed and exhibits better adhesion.
TABLE 11 laboratory Tablebbing after addition of imported Binder and example 3 of the invention to various materials
Material Imported binder Inventive example 3 adhesive
Raw material
Clinker
Cement
Sandstone
Limestone
Iron ore ×
Silica fume ×
X-ray fluorescence detection results and errors:
the fluorescence detection is according to GB/T176 'Cement chemistry analysis method', the repeatability limit is the requirement of the method, the following is the fluorescence result of the test after samples of different materials are added with imported binding agent and the binding agent of example 3 are ground into powder and are molded into 3 pieces respectively, and the requirement of GB/T176 repeatability limit is met. The fluorescent test conditions are satisfied: the repeatability of the pressed sheet formed by powder ground by adding the same batch of material into the binder meets the requirement of the fluorescent analysis repeatability limit of GB/T176.
Table 12 shows the results of fluorescence measurements of the flakes obtained in laboratory tests with binders according to the invention added to different materials (same test conditions), wherein silica fume and iron ore were not formable using the imported binders, all only with fluorescence data according to the invention. Table 13 shows the maximum deviation of different elements in each material, and the deviation is less than the repeatability limit, so that the GB/T176 fluorescence detection requirement is met.
TABLE 12 results of fluorescence measurements in the laboratory after the addition of the imported binder and example 3 of the present invention to different materials
Figure BDA0003119503990000191
Figure BDA0003119503990000201
TABLE 13 maximum deviation of fluorescence data in TABLE 12
Figure BDA0003119503990000202
Figure BDA0003119503990000211
The particle distribution condition is as follows: table 14 shows the particle size X of the above-mentioned various materials after grinding with various binders50The data, the material index of the grinding is the same, the grinding condition and time are the same, the added binder dosage is the same, and the difference is only in binder selection.
Table 14 table 12 shows particle size X of the corresponding material after grinding with different binders50Data of
Figure BDA0003119503990000212
Figure BDA0003119503990000221
The results show that the particle size of the powder ground by using the binder of the invention is smaller, which indicates that the grinding is more sufficient by using the binder of the invention.

Claims (10)

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 dispersant, 1-5 parts of lubricant and 8-15 parts of tackifier.
2. The solid binder according to claim 1, wherein the binder is selected from one or more of methylcellulose, microcrystalline cellulose or starch.
3. Solid binder according to claim 1 or 2, characterized in that the dispersant is selected from lactose or galactose.
4. The solid binder according to claim 3, wherein the lactose is selected from at least one of alpha-lactose monohydrate or anhydrous lactose.
5. Solid binder according to claim 1 or 2, characterized in that the lubricant is selected from paraffin wax.
6. Solid adhesive according to claim 1 or 2, characterized in that the tackifier is selected from polyvinylpyrrolidone.
7. The solid binder as claimed in claim 1 or 2, wherein the binder further comprises an outer coating, the mass of the outer coating being 2-4% of the mass of the binder.
8. A method for preparing a solid binder according to any one of claims 1 to 7, characterized in that it comprises in particular:
and stirring and mixing the binder, the dispersant, the lubricant and the tackifier according to the formula ratio.
9. The method of claim 8, wherein the solid binder is placed in a tablet press to form a tablet; coating the surface of the tablet with an outer coating by using a coating machine.
10. Use of a solid binder according to any one of claims 1-7 for powder compression.
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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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