Fluorescent tablet binder as well as preparation method and application thereof

Abstract

The invention belongs to the technical field of building material detection, and provides a fluorescent tablet binder as well as a preparation method and application thereof. The fluorescent tabletting binder is prepared from the following raw materials in parts by mass: 10-20 parts of boric acid, 2-8 parts of stearic acid, 15-20 parts of low-pressure polyethylene and 5-15 parts of modified filler. According to the fluorescent tablet binder, boric acid, stearic acid and low-pressure polyethylene are added, a functional complementary binding-lubricating-strength balance system is formed, interference of the binder to a fluorescence test is reduced, meanwhile, the modified filler is adopted to replace part of a high polymer material, the production cost is reduced, and the service life of the binder is prolonged. The compatibility of inorganic filler and organic components is improved through chemical bonding, so that the filler is uniformly dispersed in a bonding system, the uniformity and the structural stability of the adhesive are remarkably improved, the interference to fluorescence signals is further reduced, and the adhesive is completely suitable for being applied to fluorescence analysis of cement-based materials.

Description

Technical Field

[0001] The present invention relates to the technical field of building material detection, and in particular to a fluorescent sheeting adhesive and a preparation method and application thereof. Background Art

[0002] In the fluorescence analysis of cement raw materials, clinker, and silicate materials, powder pelleting has become the preferred sample preparation method for pelleting in the cement industry due to its advantages such as fast analysis speed, wide detection range, high accuracy, and ease of operation. This method relies on the physical or chemical bonding of a binder to the sample powder, securing the powder particles and ensuring a smooth surface and uniform elemental distribution after pelleting, thus meeting the requirements of X-ray fluorescence spectrometers. Therefore, the choice of binder is crucial. However, traditional binders have significant drawbacks: single stearic acid suffers from poor thermal stability; single boric acid is susceptible to moisture and interferes with key elemental analysis; starches are hygroscopic, resulting in loose pellets; and celluloses may introduce carbon that interferes with fluorescence testing. Therefore, a single binder cannot achieve the desired balance of lubricity, bond strength, and low interference. While some composite binders can partially improve performance, they fail to address the interfacial compatibility issues of the binder components, which can still lead to insufficient pelleting uniformity and even interference with the fluorescence signal.

[0003] Therefore, there is an urgent need to develop a patented formula composite binder that can take into account the dispersibility, adhesion and low background requirements through synergistic effects, while adapting to the volatility of cement raw materials. Summary of the Invention

[0004] In view of this, the present invention provides a fluorescent sheeting adhesive and a preparation method and application thereof to solve the problems of existing fluorescent sheeting adhesives that are prone to interfere with fluorescent signals, have high production costs, and have poor stability and uniformity.

[0005] In order to achieve the above object, the present invention adopts the following technical solutions:

[0006] The present invention provides a fluorescent sheeting adhesive, comprising the following components in parts by mass:

[0007] 10-20 parts of boric acid, 2-8 parts of stearic acid, 15-20 parts of low-pressure polyethylene, 5-15 parts of modified filler;

[0008] The preparation method of the modified filler comprises the following steps:

[0009] 1) mixing a silane coupling agent with an alcohol solution and an acid to carry out a hydrolysis reaction to obtain a hydrolysis solution;

[0010] 2) The filler is mixed with the hydrolysis solution and subjected to modification treatment to obtain a modified filler.

[0011] Preferably, the pH value of the hydrolysis reaction in step 1) is 3-5, the temperature is 40-60° C., and the time is 0.5-1 h.

[0012] Preferably, in step 1), the mass ratio of the silane coupling agent to the alcohol solution is 1:5-10; and the volume concentration of the alcohol solution is 50-70%.

[0013] Preferably, the silane coupling agent in step 1) includes one or more of γ-aminopropyltriethoxysilane, 3-(2,3-epoxypropoxy)propyltrimethoxysilane, γ-aminopropyltrimethoxysilane and γ-methacryloxypropyltrimethoxysilane; the alcohol solution includes one or more of methanol solution, ethanol solution and isopropanol solution; and the acid includes acetic acid and / or hydrochloric acid.

[0014] Preferably, the temperature of the modification treatment in step 2) is 70-100° C. and the time is 2-4 hours.

[0015] Preferably, the mass ratio of the filler in step 2) to the silane coupling agent in step 1) is 5-15:0.2-5.

[0016] Preferably, the filler in step 2) comprises one or more of kaolin, bentonite, diatomaceous earth and aluminum hydroxide; and the particle size of the filler is 1 to 10 μm.

[0017] The present invention also provides a method for preparing a fluorescent sheeting adhesive, comprising the following steps:

[0018] Boric acid, stearic acid, low-pressure polyethylene and modified filler are mixed and ground to obtain a fluorescent tabletting adhesive.

[0019] Preferably, the particle size of the fluorescent sheeting binder is 10 to 30 μm.

[0020] The present invention also provides an application of a fluorescent pressed sheet adhesive prepared by the above-mentioned preparation method of the fluorescent pressed sheet adhesive in fluorescence analysis of cement-based materials.

[0021] It can be seen from the above technical solution that compared with the prior art, the present invention has the following beneficial effects:

[0022] The fluorescent sheeting adhesive of the present invention comprises 10 to 20 parts of boric acid, 2 to 8 parts of stearic acid, 15 to 20 parts of low-pressure polyethylene and 5 to 15 parts of modified filler. The modified filler is obtained by condensing a silane coupling agent with hydroxyl groups on the surface of the filler after hydrolysis, thereby forming a chemical bond to enhance interface bonding, solving the compatibility problem between the inorganic filler and the organic component, allowing the filler to be uniformly dispersed in the bonding system, significantly improving the uniformity and structural stability of the adhesive, thereby reducing interference with the fluorescent signal, ensuring the accuracy of fluorescence detection, and being fully suitable for application in fluorescence analysis of cement-based materials.

[0023] The low-pressure polyethylene in the fluorescent tabletting adhesive of the present invention is used as a bonding matrix, and combined with a modified filler, it can significantly improve the strength of the adhesive; boric acid auxiliary bonding can further improve the overall bonding stability of the adhesive, and boric acid, as a fluorescence interference inhibitor, can also reduce the interference of the adhesive to the target fluorescence signal; stearic acid can improve the lubricity of the adhesive, and can also assist in dispersion, improving the dispersibility of the filler in the bonding system; each raw material works synergistically to form a functionally complementary bonding-lubrication-strength balance system, reducing the interference of the adhesive itself to the fluorescence test, and finally preparing a fluorescent tabletting adhesive with low fluorescence interference and excellent stability and uniformity. In addition, the raw material sources of the present invention are extensive and the amount used is small, and fillers are also used to replace some polymer materials, which greatly reduces the production cost of the fluorescent tabletting adhesive, has significant economic benefits, and is conducive to promoting the large-scale production of fluorescent tabletting adhesives. DETAILED DESCRIPTION

[0024] The present invention provides a fluorescent sheeting adhesive, comprising the following components in parts by mass:

[0025] 10-20 parts of boric acid, 2-8 parts of stearic acid, 15-20 parts of low-pressure polyethylene, 5-15 parts of modified filler;

[0026] The preparation method of the modified filler comprises the following steps:

[0027] 1) mixing a silane coupling agent with an alcohol solution and an acid to carry out a hydrolysis reaction to obtain a hydrolysis solution;

[0028] 2) The filler is mixed with the hydrolysis solution and subjected to modification treatment to obtain a modified filler.

[0029] In the present invention, the boric acid is preferably 12 to 18 parts, more preferably 13 to 16 parts, more preferably 15 parts; the stearic acid is preferably 3 to 7 parts, more preferably 4 to 6 parts, more preferably 5 parts; the low-pressure polyethylene is preferably 15.5 to 19 parts, more preferably 16 to 18 parts, more preferably 17 parts; the modified filler is preferably 6 to 13 parts, more preferably 7 to 12 parts, more preferably 8 to 10 parts.

[0030] In the present invention, the pH value of the hydrolysis reaction in step 1) is 3 to 5, preferably 3.2 to 4.8, more preferably 3.5 to 4.5, and more preferably 4; the temperature of the hydrolysis reaction is 40 to 60° C., preferably 42 to 58° C., more preferably 45 to 55° C., and more preferably 50° C.; the time of the hydrolysis reaction is 0.5 to 1 h, preferably 0.6 to 0.9 h, more preferably 0.65 to 0.85 h, and more preferably 0.7 h.

[0031] In the present invention, the mass ratio of the silane coupling agent to the alcohol solution in step 1) is 1:5-10, preferably 1:6-9, more preferably 1:6.5-8.5, and more preferably 1:7; the volume concentration of the alcohol solution is 50-70%, preferably 52-68%, more preferably 55-65%, and more preferably 60%.

[0032] In the present invention, the silane coupling agent in step 1) includes one or more of γ-aminopropyltriethoxysilane, 3-(2,3-epoxypropoxy)propyltrimethoxysilane, γ-aminopropyltrimethoxysilane and γ-methacryloxypropyltrimethoxysilane; the alcohol solution includes one or more of methanol solution, ethanol solution and isopropanol solution; and the acid includes acetic acid and / or hydrochloric acid.

[0033] In the present invention, the temperature of the modification treatment in step 2) is 70-100°C, preferably 75-95°C, more preferably 80-90°C, and more preferably 85°C; the time of the modification treatment is 2-4h, preferably 2.2-2.8h, more preferably 2.3-2.6h, and more preferably 2.5h.

[0034] In the present invention, the mass ratio of the filler in step 2) to the silane coupling agent in step 1) is 5-15:0.2-5, preferably 6-13:0.5-4.5, more preferably 7-12:0.6-4, and more preferably 8-10:1-3.

[0035] In the present invention, the filler in step 2) comprises one or more of kaolin, bentonite, diatomaceous earth and aluminum hydroxide; the particle size of the filler is 1 to 10 μm, preferably 2 to 8 μm, more preferably 3 to 6 μm, and more preferably 5 μm.

[0036] The present invention also provides a method for preparing a fluorescent sheeting adhesive, comprising the following steps:

[0037] Boric acid, stearic acid, low-pressure polyethylene and modified filler are mixed and ground to obtain a fluorescent tabletting adhesive.

[0038] In the present invention, the mixing is preferably performed by first mixing the low-pressure polyethylene and the modified filler, and then adding boric acid and stearic acid; the low-pressure polyethylene acts as a bonding matrix, preferentially forming a physical package with the modified filler, thereby avoiding subsequent small molecules (stearic acid and boric acid) hindering their contact, and can improve the interfacial compatibility between the inorganic filler and the organic component.

[0039] In the present invention, the grinding speed is preferably 200-500 r / min, more preferably 250-450 r / min, more preferably 300-400 r / min; the grinding time is preferably 0.5-2 h, more preferably 1.0-1.8 h, more preferably 1.5 h.

[0040] In the present invention, the particle size of the fluorescent sheeting binder is 10 to 30 μm, preferably 11 to 25 μm, more preferably 13 to 20 μm, and even more preferably 15 μm.

[0041] The present invention also provides an application of a fluorescent pressed sheet adhesive prepared by the above-mentioned preparation method of the fluorescent pressed sheet adhesive in fluorescence analysis of cement-based materials.

[0042] The technical solutions provided by the present invention are described in detail below with reference to the embodiments, but they should not be construed as limiting the scope of protection of the present invention.

[0043] Example 1

[0044] Mix 1 part of γ-aminopropyltriethoxysilane with 5 parts of ethanol solution (volume concentration of 50%) and hydrochloric acid, control the pH value to 3, and carry out hydrolysis reaction at a temperature of 40°C for 1 hour to obtain a hydrolysis solution; then mix 5 parts of kaolin with a particle size of 1 μm with the above-mentioned hydrolysis solution, and carry out modification treatment at a temperature of 70°C for 3.5 hours to obtain modified kaolin; then mix 15 parts of low-pressure polyethylene with 6 parts of the above-mentioned modified kaolin, grind at a speed of 200 r / min for 5 minutes, then add 10 parts of boric acid and 3 parts of stearic acid, and continue grinding for 50 minutes to obtain a fluorescent sheeting adhesive with a particle size of 30 μm.

[0045] Example 2

[0046] Mix 2 parts of 3-(2,3-epoxypropoxy)propyltrimethoxysilane with 12 parts of methanol solution (volume concentration of 60%) and acetic acid, control the pH value to 4, and carry out hydrolysis reaction at a temperature of 45°C for 1 hour to obtain a hydrolysis solution; then mix 8 parts of aluminum hydroxide with a particle size of 3 μm with the above hydrolysis solution, and carry out modification treatment at a temperature of 80°C for 3.5 hours to obtain modified aluminum hydroxide; then mix 16 parts of low-pressure polyethylene with 7 parts of the above modified aluminum hydroxide, grind at a speed of 300 r / min for 5 minutes, then add 12 parts of boric acid and 4 parts of stearic acid, and continue grinding for 70 minutes to obtain a fluorescent sheeting adhesive with a particle size of 20 μm.

[0047] Example 3

[0048] Mix 3 parts of γ-aminopropyltrimethoxysilane with 24 parts of isopropanol solution (volume concentration of 70%) and acetic acid, control the pH value to 3, and carry out hydrolysis reaction at a temperature of 50°C for 0.8h to obtain a hydrolysis solution; then mix 10 parts of diatomaceous earth with a particle size of 5μm with the above-mentioned hydrolysis solution, and carry out modification treatment at a temperature of 90°C for 3h to obtain modified diatomaceous earth; then mix 18 parts of low-pressure polyethylene with 10 parts of the above-mentioned modified diatomaceous earth, grind at a speed of 400r / min for 5min, then add 15 parts of boric acid and 6 parts of stearic acid, and continue grinding for 1h to obtain a fluorescent sheeting adhesive with a particle size of 15μm.

[0049] Example 4

[0050] Mix 5 parts of γ-aminopropyltriethoxysilane with 50 parts of ethanol solution (volume concentration of 50%) and hydrochloric acid, control the pH value to 5, and carry out hydrolysis reaction at a temperature of 60°C for 0.5h to obtain a hydrolysis solution; then mix 15 parts of kaolin with a particle size of 10μm with the above-mentioned hydrolysis solution, and carry out modification treatment at a temperature of 100°C for 2h to obtain modified kaolin; then mix 20 parts of low-pressure polyethylene with 15 parts of the above-mentioned modified kaolin, grind at a speed of 500r / min for 3min, then add 20 parts of boric acid and 8 parts of stearic acid, and continue grinding for 1.5h to obtain a fluorescent sheeting adhesive with a particle size of 10μm.

[0051] Comparative Example 1

[0052] The only difference between Comparative Example 1 and Example 1 is that the low-pressure polyethylene is replaced by starch.

[0053] Comparative Example 2

[0054] The only difference between Comparative Example 2 and Example 1 is that the kaolin was not modified and unmodified kaolin was directly added.

[0055] Comparative Example 3

[0056] The only difference between Comparative Example 3 and Example 1 is that boric acid is replaced by paraffin.

[0057] X-ray fluorescence detection:

[0058] According to the fluorescence detection method specified in GB / T 176, "Chemical Analysis Methods for Cement," the fluorescent tableting binders prepared in Examples 1-4 and Comparative Examples 1-3 were added to the PO42.5 cement clinker to be tested and ground and pressed to produce seven groups of samples, wherein the mass of the fluorescent tableting binder was 0.3% of the mass of the cement clinker. Simultaneously, a control group of cement clinker without the fluorescent tableting binder was prepared using the same method. Fluorescence detection of the samples was then performed in accordance with GB / T 176. The fluorescence detection results are shown in Table 1.

[0059] Table 1 Fluorescence detection results

[0060]

[0061]

[0062] As can be seen from Table 1, the fluorescence component detection deviations of Examples 1 to 4 of the present invention and the control group are all lower than the repeatability limit of the national standard, while the fluorescence component detection deviations of Comparative Examples 1 to 3 and the control group are all higher than the repeatability limit of the national standard, which shows that the addition of the fluorescent tableting binder prepared by the present invention does not affect the chemical composition detection of cement clinker, that is, the fluorescent tableting binder of the present invention reduces the interference with the target fluorescent signal and ensures the accuracy of fluorescence detection.

[0063] The above is only a preferred embodiment of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principles of the present invention. These improvements and modifications should also be regarded as within the scope of protection of the present invention.

Claims

1. A fluorescent sheeting adhesive, characterized in that: The composition includes the following parts by mass: 10-20 parts of boric acid, 2-8 parts of stearic acid, 15-20 parts of low-pressure polyethylene, 5-15 parts of modified filler; The preparation method of the modified filler comprises the following steps: 1) mixing a silane coupling agent with an alcohol solution and an acid to carry out a hydrolysis reaction to obtain a hydrolysis solution; 2) The filler is mixed with the hydrolysis solution and subjected to modification treatment to obtain a modified filler.

2. The fluorescent sheeting adhesive according to claim 1, characterized in that: The pH value of the hydrolysis reaction in step 1) is 3-5, the temperature is 40-60° C., and the time is 0.5-1 h.

3. The fluorescent sheeting adhesive according to claim 2, characterized in that: In step 1), the mass ratio of the silane coupling agent to the alcohol solution is 1:5-10; and the volume concentration of the alcohol solution is 50-70%.

4. The fluorescent sheeting adhesive according to any one of claims 1 to 3, characterized in that: The silane coupling agent in step 1) includes one or more of γ-aminopropyltriethoxysilane, 3-(2,3-epoxypropyloxy)propyltrimethoxysilane, γ-aminopropyltrimethoxysilane and γ-methacryloxypropyltrimethoxysilane; The alcohol solution includes one or more of methanol solution, ethanol solution and isopropanol solution; The acid includes acetic acid and / or hydrochloric acid.

5. The fluorescent sheeting adhesive according to claim 4, characterized in that: The temperature of the modification treatment in step 2) is 70-100° C. and the time is 2-4 hours.

6. The fluorescent sheeting adhesive according to claim 5, characterized in that: The mass ratio of the filler in step 2) to the silane coupling agent in step 1) is 5-15:0.2-5.

7. The fluorescent sheeting adhesive according to claim 6, characterized in that: The filler in step 2) comprises one or more of kaolin, bentonite, diatomaceous earth and aluminum hydroxide; The particle size of the filler is 1 to 10 μm.

8. The method for preparing a fluorescent sheeting adhesive according to any one of claims 1 to 7, characterized in that: The steps include: Boric acid, stearic acid, low-pressure polyethylene and modified filler are mixed and ground to obtain a fluorescent tabletting adhesive.

9. The method for preparing a fluorescent sheeting adhesive according to claim 8, characterized in that: The particle size of the fluorescent sheeting adhesive is 10 to 30 μm.

10. Use of the fluorescent pressed sheet adhesive prepared by the preparation method of the fluorescent pressed sheet adhesive according to any one of claims 8 to 9 in fluorescence analysis of cement-based materials.

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