Preparation process and application of synthetic saponite
By optimizing the lithium saponite preparation process and adopting a mixing method of Mg source, Si source, Al source and pH adjuster, combined with a vertical filter press and a grinding mill, the problems of low quality stability and low efficiency in lithium saponite preparation were solved, and efficient and uniform saponite production was achieved.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- ZHEJIANG KELEI NEW MATERIAL CO LTD
- Filing Date
- 2024-04-03
- Publication Date
- 2026-07-21
AI Technical Summary
Existing methods for preparing lithium saponite suffer from poor product quality stability, high impurity content, and low production efficiency, making it difficult to meet the needs of industrial applications.
The soapstone is prepared by uniformly mixing Mg source, Si source, Al source and pH adjuster in sequence, combined with vertical filter press filtration and crystallization reaction at a specific temperature, and then prepared by grinding mill. The soapstone is then crushed and cleaned using a dedicated production line.
The preparation of soapstone with good expansion and dispersibility improved production efficiency, reduced impurity content, and enhanced product uniformity and dispersibility.
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Figure CN118324152B_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of inorganic mineral preparation, and specifically to a process for preparing synthetic soapstone. Background Technology
[0002] Saponite is a 2:1 type trioctahedral layered silicate belonging to the montmorillonite group of clay minerals. Its ideal molecular formula is: M x [Mg3][Si 4-x Al x ]O 10 (OH)₂·nH₂O, where M is an interlayer exchangeable cation. The saponite crystal structure has a central octahedron (essentially a brucite [Mg(OH)₂] structure), in which four of the six OH- groups are replaced by oxygen atoms. These oxygen atoms are located on either side of the central octahedron, forming two tetrahedra (composed of Si). 4+ and O 2- (Composition) Connection. The layer thickness is approximately 1 nm, and the lateral dimensions of the layer can range from 30 nm to several micrometers or larger. Typically, Al is formed on a tetrahedral layer. 3+ For Si 4+ The dominant isomorphic substitution results in a negatively charged synthetic soapstone, and the resulting net negative charge between layers is compensated by exchangeable cations between layers.
[0003] The structural unit of soapstone consists of two layers of Si-O tetrahedral sheets sandwiching a layer of Mg-O(OH) octahedral sheets. Al is present within the tetrahedral sheets. 3+ →Si 4+ The substitution process results in soapstone layers carrying excess negative charges; therefore, a certain amount of exchangeable cations (such as Na+) often exist between the layers. + Ca 2+ (etc.) to balance the negative charge carried by the soapstone structural layers. Besides possessing the common characteristics of clay minerals such as small particle size, large specific surface area, and exchangeable ions between layers, soapstone also exhibits high surface acidity, high thermal stability, and strong colloidal properties, making it widely used in chemical, textile, environmental, and pharmaceutical industries. Compared to the abundant bentonite resources, my country has very limited exploitable soapstone mineral resources, and naturally occurring soapstone has a high impurity content, making purification difficult and hindering its industrial applications to some extent.
[0004] Natural soapstone is formed by the weathering of magnesium-bearing rocks. Due to the complexity of the parent rock, its chemical composition, and its physicochemical conditions, Mg... 2+It can be replaced by isomorphic metals of different valence states. For industrial applications, it is crucial that the composition and properties of clay materials be tailored to the needs of different industries. However, the chemical composition and properties of natural soapstone vary greatly, depending on the chemical composition of the parent rock, the diagenetic process, and the provenance. This variability significantly limits the application of natural soapstone. Synthetic soapstone, on the other hand, not only avoids various impurities and cumbersome purification processes, yielding a homogeneous and highly pure solid product, but also allows for the synthesis of soapstone with controllable physicochemical properties as needed.
[0005] Lithium saponite is a clay mineral containing magnesium, lithium, and silicon, belonging to the vermiculite subgroup of the montmorillonite group. Its crystal structure is trioctahedral. It is generally grayish-white, with a fine texture, low hardness, and a slippery feel. When added to water, lithium saponite swells rapidly, forming a gel containing a large water network structure, exhibiting good thixotropic, dispersible, suspending, and thickening properties. Therefore, lithium saponite can be used in various coatings, cosmetics, pharmaceuticals, as a thickener, dispersant, suspending agent, aerosol agent, latex stabilizer, and rubber latex. Due to its superior properties, lithium saponite is widely used in many fields; however, its preparation and application still face many practical problems, such as poor product quality stability and low production efficiency. While the preparation methods for lithium saponite are basically mature, some shortcomings remain.
[0006] In recent years, lithium saponite has been widely used in industry as a thickener and anti-settling agent, but there is relatively little information on the preparation and related applications of saponite. Summary of the Invention
[0007] The purpose of this invention is to solve the problems in the prior art and provide a method for preparing a synthetic soapstone that can disperse and is transparent and has expansion properties.
[0008] The above-mentioned technical objective of the present invention is achieved through the following technical solution:
[0009] A process for preparing synthetic soapstone includes the following steps:
[0010] Step (1) Mixing and homogenizing raw materials
[0011] Step (2) Liquid crystallization reaction
[0012] Step (3) Filtration and washing of the slurry after crystallization
[0013] Step (4) Drying the filter cake
[0014] Step (5) Crushing the dried filter cake
[0015] Lithium saponite or natural saponite prepared by existing technologies suffer from problems such as low impurity content, poor product quality stability, and low production efficiency. Therefore, this invention addresses these issues by proposing a preparation process for synthetic saponite that can be dispersed, transparent, and has expansion properties.
[0016] Preferably, step (1) involves mixing and homogenizing the raw materials.
[0017] First, a Mg source is added and homogenized with stirring. Then, a Si source is added and homogenized with stirring. Finally, an Al source and a pH adjuster are added and homogenized with stirring to obtain a mixed slurry. The Mg source is dissolved in water in a homogenization container and heated to 80°C. The Si source is then dissolved in water and slowly added to the homogenization container, stirred until homogeneous. Finally, the Al source and pH adjuster are dissolved in water and slowly added to the homogenization container, stirred continuously until all three are thoroughly mixed to obtain a homogenized mixed slurry. The Mg source is MgO, MgCl2, Mg(OH)2, and... The composition includes: MgSO4 (35-40 parts by mass); Si source (40-45 parts by mass) of either silica sol or Na2SiO3; Al source (0.01-0.06 parts by mass) of either NaAlO2, Al2(SO4)3, or AlCl3; pH adjuster (0.05-0.12 parts by mass of NaOH and 0.04-0.06 parts by mass of Na2CO3); and the remainder is deionized water.
[0018] The advantages of using this invention are that the raw material mixing in step (1) is carried out in a homogenization container with stirring and heating, and the raw materials are added to the homogenization container in the order of Mg source, Si source, Al source and pH adjuster and stirred for a certain period of time; the raw materials are dissolved in water first and then added to the homogenization container for stirring, which can make the whole system more uniform and the mixing more thorough; soapstone with expansion properties can be obtained by using Mg source, Si source, Al source and pH adjuster as raw materials.
[0019] Preferably, step (2) involves liquid crystallization reaction.
[0020] The raw material homogenized slurry obtained in step (1) is transferred to a stainless steel reactor and heated for crystallization reaction. After the reaction is completed, it is cooled to room temperature and the stainless steel reactor is removed to obtain the crystallized slurry. The crystallization reaction temperature is 150-200℃, the reactor pressure is 1.5-2.2MPa, and the crystallization time is 5-24h.
[0021] Preferably, the slurry is filtered and washed after crystallization in step (3).
[0022] The slurry obtained in step (2) is filtered by a vertical filter press and washed with water to obtain a filter cake. The filtration and washing are carried out by a vertical filter press. After filtration, a filter cake is formed. Water is then added to wash away free ionic impurities in the filter cake. Water is added to wash until the conductivity of the effluent is less than 1000 μS / cm.
[0023] The advantage of using this invention is that, compared with other intermittently operating filter presses (such as cartridge type, horizontal blade, and vertical blade filter presses), the vertical automatic plate and frame filter press is more like a continuously operating filter press because its operating cycle is very short, reaching 6-7 minutes per cycle, almost similar to a continuously operating filter press; the advantages of the vertical compressor are:
[0024] (1) When a filter cake with very low moisture content is required, it can save a lot of energy compared to a vacuum filter and reduce transportation costs. It can ensure that the minimum safe moisture content of the filter cake is required during transportation;
[0025] (2) The filter cake washing efficiency is high, which can save the amount of water used for washing liquid to the greatest extent;
[0026] (3) Since the vertical automatic plate and frame filter press operates almost continuously, the filter cake storage tank can be made much smaller than that of the horizontal automatic plate and frame filter press.
[0027] Preferably, step (4) involves drying the filter cake.
[0028] The filter cake obtained in step (3) is dried; the filter cake is dried using a tunnel drying device to reduce the moisture content of the filter cake to below 10%.
[0029] Preferably, step (5) involves crushing the dried filter cake.
[0030] The dried filter cake obtained in step (4) is crushed to obtain synthetic soapstone; the dried product is crushed by a grinding mill and then passed through a 60-mesh sieve to achieve a fineness of over 60 mesh.
[0031] The advantage of using this invention is that after drying the filter cake, grinding it into powder and sieving it through a 60-mesh sieve can achieve a powder fineness of over 60 mesh, which is beneficial for obtaining a final product with high dispersibility.
[0032] Preferably, the grinding process in step (5) uses a production line device for preparing soapstone, including a main body, two sets of rollers, a power mechanism, four sets of support rods and a base plate. The bottom of the main body is uniformly connected to the top of the four sets of support rods, and the bottom of the four sets of support rods is connected to one end of the top of the base plate. The main body is provided with a working chamber, and the rear end of the working chamber is rotatably connected to the rear end of the two sets of rollers. The two sets of rollers mesh. The front end of the main body is provided with a power mechanism, and the front ends of the two sets of rollers pass through the front end of the working chamber and are connected to the power mechanism. The device also includes two sets of support blocks, two sets of cleaning brushes, four sets of first clamping blocks, four sets of first clamping plates, a mounting plate, two sets of first bidirectional screws, four sets of first sliders, four sets of second clamping blocks, a buffer assembly, an auxiliary assembly and a collection assembly. The left and right ends of the working chamber of the main body are each provided with a set of reserved holes, and the top and bottom of the two sets of reserved holes are each provided with two sets of slots. The four sets of first clamping blocks are respectively connected to the main body. The device is equipped with a slotted mounting system. The top and bottom of two sets of support blocks are connected to one end of two sets of first sliders, and the two sets of support blocks are also fitted into the pre-drilled holes in the main body of the device. One end of each set of support blocks is connected to one end of a cleaning brush via a buffer assembly. The other ends of the two sets of cleaning brushes are in close contact with one end of a rolling roller. A set of mounting plates is provided at the top of the left and right ends of the main body of the device. A set of sliding grooves is provided at the bottom of each set of mounting plates. The front and rear ends of the two sets of first bidirectional screws are rotatably connected to the sliding grooves of the mounting plates. The four sets of first sliders are threaded to one end of each first bidirectional screw, and the four sets of first sliders are slidably connected to the sliding grooves of the mounting plates. The bottom of each set of first sliders is connected to the top of the first clamping plate. A set of slots is provided at the rear and front ends of each set of support blocks. One end of each set of second locking blocks is fitted into the slot of the support block, and the other end of each set of second locking blocks is connected to one end of the first clamping plate. An auxiliary assembly is provided at the bottom of the main body of the device, and a collection assembly is provided at the top of the bottom plate.
[0033] Preferably, the buffer assembly includes four sets of second sliders, two sets of connecting blocks, multiple sets of telescopic rods, and multiple sets of connecting springs. Each of the two sets of supporting blocks has a groove at one end, and each of the two sets of supporting blocks has a sliding groove at the top and bottom of the groove. The four sets of second sliders are slidably connected to the sliding grooves of the supporting blocks, and each of the two sets of connecting blocks is connected to a set of second sliders at the top and bottom. Each of the two sets of connecting blocks is evenly connected to one end of multiple sets of telescopic rods, and the other end of each set of telescopic rods is connected to one end of the groove of the supporting block. Each of the multiple sets of telescopic rods has a connecting spring on its outer side, and the other end of each of the two sets of connecting blocks is connected to one end of the cleaning brush.
[0034] Preferably, the collection assembly includes a fixed plate, two sets of third sliders, two sets of fourth sliders, a second bidirectional screw, two sets of arc-shaped clamps, and a collection bucket. The top of the bottom plate is evenly provided with two sets of sliding grooves. The bottom of the two sets of third sliders is slidably connected to the sliding grooves of the bottom plate. The bottom of the fixed plate is evenly connected to the top of the two sets of third sliders. The top of the fixed plate is provided with a set of sliding grooves. The front end and rear end of the second bidirectional screw are rotatably connected to one end of the sliding groove of the fixed plate. The two sets of fourth sliders are threaded to one end of the second bidirectional screw. The two sets of fourth sliders are slidably connected to the sliding grooves of the fixed plate. The bottom of the two sets of arc-shaped clamps is connected to the top of the fourth sliders. One end of the two sets of arc-shaped clamps is tightly attached to one end of the collection bucket.
[0035] Preferably, the auxiliary components include a first annular plate, a second annular plate, a funnel, two sets of connecting screws, two sets of limiting blocks, two sets of threaded blocks, and two sets of positioning plates. A pre-drilled hole is provided at the bottom of the main body of the device. The bottom of the main body of the device is connected to the top of the first annular plate. A set of pre-drilled holes is provided at the left and right ends of the first annular plate. The two sets of limiting blocks are slidably connected to the pre-drilled holes of the first annular plate. A set of positioning blocks is provided at the bottom of the left and right ends of the first annular plate. The two sets of connecting screws are threadedly connected to the positioning blocks. The tops of the two sets of connecting screws are rotatably connected to one end of the bottom of the main body of the device. The two sets of threaded blocks are threadedly connected to the connecting screws. One end of each set of connecting blocks is connected to one end of a limiting block. The other ends of each set of limiting blocks are connected to one end of the second annular plate. A funnel is provided on the inner side of the second annular plate.
[0036] Preferably, it also includes five sets of rotating nuts, with a set of rotating nuts provided at the front ends of the two sets of first bidirectional screws and the two sets of bidirectional screws, and a set of rotating nuts also provided at the bottom of the two sets of connecting screws.
[0037] Preferably, it also includes two sets of anti-slip mats, with one set of anti-slip mats at one end of each of the two sets of arc-shaped clamps, and the other ends of the two sets of anti-slip mats are respectively in close contact with one end of the collection bucket;
[0038] Preferably, it also includes a hand handle, and a set of hand handles is provided at the top front end of the fixed plate;
[0039] Preferably, it also includes two sets of guide vanes, with one set of guide vanes respectively provided at the top of the left and right ends of the main body of the device.
[0040] The advantages of using this invention are that it improves the efficiency and effectiveness of cleaning work for staff and enhances its practicality.
[0041] In summary, the present invention has the following beneficial effects:
[0042] 1. Using Mg source, Si source, Al source and pH adjuster as raw materials for synthesizing soapstone and combining them with a sequential stirring process can make the subsequent crystallization and the soapstone product have better expansion properties and more uniform distribution.
[0043] 2. Using a vertical compressor for filtration and washing can improve the efficiency of filter cake filtration, compression, and washing, save production time, and increase production efficiency.
[0044] 3. The selection of a soapstone preparation production line device for grinding reduces the workload of workers, thereby improving the efficiency and effectiveness of cleaning work and enhancing its practicality.
[0045] 4. Grinding the obtained dried filter cake into powder and then sieving it through a 60-mesh sieve can result in a finer soapstone product with improved dispersibility. Attached Figure Description
[0046] Figure 1 This is a process flow diagram for the preparation of a synthetic soapstone.
[0047] Figure 2 XRD pattern of SP-1 synthesized saponite;
[0048] Figure 3 SEM image of SP-3 synthesized soapstone;
[0049] Figure 4 The FTIR spectrum of SP-3 synthesized soapstone;
[0050] Figure 5 XRD pattern of SP-3 synthetic soapstone;
[0051] Figure 6 XRD pattern of SP-4 synthetic soapstone;
[0052] Figure 7 XRD pattern of lithium saponite;
[0053] Figure 8 Viscosity comparison chart of 3% dispersion after standing for 24 hours;
[0054] Figure 9 Schematic diagram of a production apparatus for preparing saponite;
[0055] Figure 10 This is a schematic diagram of the cross-section of the structure viewed from the front.
[0056] Figure 11 This is a schematic diagram of the right-side structural cross-section;
[0057] Figure 12 This is a magnified schematic diagram of a local structure of A. Detailed Implementation
[0058] The following specific embodiments are merely illustrative of the present invention and are not intended to limit the invention. After reading this specification, those skilled in the art can make modifications to these embodiments without contributing any inventive step, but such modifications are protected by patent law as long as they fall within the scope of the claims of the present invention.
[0059] The present invention will now be described in detail with reference to the accompanying drawings and embodiments.
[0060] Example 1
[0061] Step (1) Mixing and homogenizing raw materials
[0062] Dissolve 300g of MgCl2 in water in a homogenization container and heat to 80℃. Then, dissolve 298g of silica sol in water and slowly add it to the homogenization container, stirring until homogeneous. Finally, dissolve 23g of AlCl3, 40g of Na2CO3, and 80g of NaOH in water and slowly add them to the homogenization container, stirring continuously until the three are evenly mixed. The total mass concentration of the mixture is 7%, resulting in a homogenized slurry.
[0063] Step (2) Liquid crystallization reaction
[0064] The homogenized slurry obtained in step (1) is transferred to a stainless steel reactor and heated for crystallization reaction. The temperature of the crystallization reaction is 200℃, the pressure of the reactor is 1.5-2.2MPa, and the crystallization time is 5h. After the reaction is completed, the reactor is cooled to room temperature and the stainless steel reactor is removed to obtain the crystallized slurry.
[0065] Step (3) Filtration and washing of the slurry after crystallization
[0066] The slurry obtained in step (2) is filtered by a vertical filter press and washed with water to obtain a filter cake. Water is then added to wash away free ionic impurities in the filter cake, and water is added to wash until the conductivity of the effluent is less than 1000 μS / cm.
[0067] Step (4) Drying the filter cake
[0068] The filter cake obtained in step (3) is dried; the filter cake is dried using a tunnel drying device to reduce the moisture content of the filter cake to below 10%.
[0069] Step (5) Crushing the dried filter cake
[0070] The dried filter cake obtained in step (4) is crushed to obtain synthetic soapstone; the dried product is crushed by a grinding mill, and after grinding, it is passed through a 60-mesh sieve. The fineness of the powder reaches more than 60 mesh, thus obtaining the synthetic soapstone SP-1.
[0071] Example 2
[0072] Step (1) Mixing and homogenizing raw materials
[0073] 296.2g of MgCl2 was dissolved in water in a homogenization container and heated to 80℃. Then, 312g of silica sol was dissolved in water and slowly added to the homogenization container, and stirred until homogeneous. Finally, 30.24g of AlCl3, 55g of Na2CO3, and 45g of NaOH were dissolved in water and slowly added to the homogenization container, and stirred until homogeneous. The total mass concentration of the mixture was 10%, resulting in a homogenized slurry.
[0074] Step (2) Liquid crystallization reaction
[0075] The homogenized slurry obtained in step (1) is transferred to a stainless steel reactor and heated for crystallization reaction. The temperature of the crystallization reaction is 200℃, the pressure of the reactor is 1.5-2.2MPa, and the crystallization time is 12h. After the reaction is completed, the reactor is cooled to room temperature and the stainless steel reactor is removed to obtain the crystallized slurry.
[0076] Step (3) Filtration and washing of the slurry after crystallization
[0077] The slurry obtained in step (2) is filtered by a vertical filter press and washed with water to obtain a filter cake. Water is then added to wash away free ionic impurities in the filter cake, and water is added to wash until the conductivity of the effluent is less than 1000 μS / cm.
[0078] Step (4) Drying the filter cake
[0079] The filter cake obtained in step (3) is dried; the filter cake is dried using a tunnel drying device to reduce the moisture content of the filter cake to below 10%.
[0080] Step (5) Crushing the dried filter cake
[0081] The dried filter cake obtained in step (4) is crushed to obtain synthetic soapstone; the dried product is crushed by a grinding mill, and after grinding, it is passed through a 60-mesh sieve. The fineness of the powder reaches more than 60 mesh, thus obtaining the synthetic soapstone SP-2.
[0082] Example 3
[0083] Step (1) Mixing and homogenizing raw materials
[0084] Dissolve 326g of MgSO4 in water in a homogenization container and heat to 80℃. Then, dissolve 343g of Na2SiO3 (SiO2 content 25%) in water and slowly add it to the homogenization container, stirring until homogeneous. Finally, dissolve 50g of Al2(SO4)3, 50g of Na2CO3, and 40g of NaOH in water and slowly add them to the homogenization container, stirring continuously until the three are mixed evenly. The total mass concentration of the mixture is 15%, resulting in a homogenized slurry.
[0085] Step (2) Liquid crystallization reaction
[0086] The homogenized slurry obtained in step (1) is transferred to a stainless steel reactor and heated for crystallization reaction. The temperature of the crystallization reaction is 200℃, the pressure of the reactor is 1.5-2.2MPa, and the crystallization time is 24h. After the reaction is completed, the reactor is cooled to room temperature and the stainless steel reactor is removed to obtain the crystallized slurry.
[0087] Step (3) Filtration and washing of the slurry after crystallization
[0088] The slurry obtained in step (2) is filtered by a vertical filter press and washed with water to obtain a filter cake. Water is then added to wash away free ionic impurities in the filter cake, and water is added to wash until the conductivity of the effluent is less than 1000 μS / cm.
[0089] Step (4) Drying the filter cake
[0090] The filter cake obtained in step (3) is dried; the filter cake is dried using a tunnel drying device to reduce the moisture content of the filter cake to below 10%.
[0091] Step (5) Crushing the dried filter cake
[0092] The dried filter cake obtained in step (4) is crushed to obtain synthetic soapstone; the dried product is crushed by a grinding mill, and after grinding, it is passed through a 60-mesh sieve. The fineness of the powder reaches more than 60 mesh, thus obtaining the synthetic soapstone SP-3.
[0093] like Figures 9 to 12As shown, a production line device for soapstone preparation includes a main body 1, two sets of rolling rollers 2, a power mechanism 3, four sets of support rods 4, and a base plate 5. The bottom of the main body 1 is evenly connected to the top of the four sets of support rods 4, and the bottom of each of the four sets of support rods 4 is connected to one end of the top of the base plate 5. The main body 1 is provided with a working chamber, and the rear end of the working chamber of the main body 1 is rotatably connected to the rear end of each of the two sets of rolling rollers 2, with the two sets of rolling rollers 2 meshing. The power mechanism 3 is provided at the front end of the main body 1, and the front ends of the two sets of rolling rollers 2 pass through the front end of the working chamber of the main body 1 and are connected to the power mechanism 3. The device also includes two sets of support blocks 6, two sets of cleaning brushes 7, four sets of first clamping blocks 8, four sets of first clamping plates 9, a mounting plate 10, two sets of first bidirectional screws 11, and four sets of first... The device consists of a slider 12, four sets of second locking blocks 13, a buffer assembly, an auxiliary assembly, and a collection assembly. The working chamber of the main body 1 has a set of reserved holes at the left and right ends, and the top and bottom of the two sets of reserved holes are respectively provided with two sets of slots. The four sets of first locking blocks 8 are respectively engaged with the slots of the main body 1. The top and bottom of the two sets of support blocks 6 are respectively connected to one end of the two sets of first sliders 12, and the two sets of support blocks 6 are respectively engaged with the reserved holes of the main body 1. One end of the two sets of support blocks 6 is respectively connected to one end of the cleaning brush 7 through the buffer assembly. The other end of the two sets of cleaning brushes 7 is respectively in close contact with one end of the rolling roller 2. A set of mounting plates 10 is respectively provided at the top of the left and right ends of the main body 1, and the bottom of the two sets of mounting plates 10 is respectively provided with a... The device consists of a set of sliding grooves. The front and rear ends of two sets of first bidirectional screws 11 are rotatably connected to the sliding grooves of the mounting plate 10. Four sets of first sliders 12 are threadedly connected to one end of each of the first bidirectional screws 11, and slidably connected to the sliding grooves of the mounting plate 10. The bottoms of the four sets of first sliders 12 are connected to the tops of the first clamping plates 9. Two sets of support blocks 6 have a set of slots at their rear and front ends. Four sets of second clamping blocks 13 have one end engaged with the slots of the support blocks 6, and the other end connected to one end of the first clamping plates 9. The device body 1 has auxiliary components at its bottom, and the base plate 5 has a collecting component at its top. The operator starts the power mechanism, causing the two sets of rollers to rotate. The operator then completes the processing... The powder is poured into the main working chamber of the device, where it is then crushed and ground by the crushing rollers. It then falls through pre-drilled holes into the collection assembly. Simultaneously, two sets of cleaning brushes clean the powder adhering to the surface of the crushing rollers as the two sets of crushing rollers rotate. After the work is completed, the operator rotates the two sets of first bidirectional screws, causing the four sets of first sliders to slide along the first clamping plates until the second locking block and support block disengage. The operator then pulls the support block until the cleaning brushes disengage from the main working chamber of the device, allowing for quick cleaning of the crushing roller surface. This reduces the workload of the operator, improving cleaning efficiency and effectiveness, thus enhancing practicality.
[0094] The buffer assembly includes four sets of second sliders 14, two sets of connecting blocks 15, multiple sets of telescopic rods 16, and multiple sets of connecting springs 17. Each of the two sets of support blocks 6 has a groove at one end, and a sliding groove at the top and bottom of the groove. The four sets of second sliders 14 are slidably connected to the sliding grooves of the support blocks 6. The top and bottom of each of the two sets of connecting blocks 15 are connected to a second slider 14. One end of each of the two sets of connecting blocks 15 is evenly connected to one end of each of the multiple sets of telescopic rods 16, and the other end of each of the multiple sets of telescopic rods 16 is connected to one end of the groove in the support block 6. A connecting spring 17 is provided on the outer side of each of the multiple sets of telescopic rods 16, and the other end of each of the two sets of connecting blocks 15 is connected to one end of a cleaning brush 7. When the two sets of cleaning brushes and the pressing roller are in close contact, a force is generated, causing the two sets of connecting blocks to slide through the second sliders. This reduces the damage to the pressing roller caused by the force generated by the squeezing contact during the extension and retraction of the connecting springs driven by the telescopic rods, thus enhancing practicality.
[0095] The collection assembly includes a fixed plate 18, two sets of third sliders 19, two sets of fourth sliders 20, a second bidirectional screw 21, two sets of arc-shaped clamps 22, and a collection bucket 23. Two sets of sliding grooves are evenly distributed on the top of the base plate 5. The bottoms of the two sets of third sliders 19 are slidably connected to the sliding grooves of the base plate 5. The bottom of the fixed plate 18 is evenly connected to the tops of the two sets of third sliders 19. A set of sliding grooves is provided on the top of the fixed plate 18. The front and rear ends of the second bidirectional screw 21 are rotatably connected to one end of the sliding groove of the fixed plate 18. The two sets of fourth sliders 20 are threadedly connected to one end of the second bidirectional screw 21. The fourth slider 20 is slidably connected to the groove of the fixed plate 18. The bottom of the two sets of arc-shaped clamps 22 are connected to the top of the fourth slider 20, and one end of the two sets of arc-shaped clamps 22 is tightly attached to one end of the collection bucket 23. After grinding is completed, the worker pulls the fixed plate and then selects the second bidirectional screw, so that the two sets of fourth sliders drive the arc-shaped clamps to slide until the two sets of arc-shaped clamps are separated from the collection bucket. Then the worker can move the powder in the collection bucket to the next process. This allows the worker to quickly take out the soapstone powder after grinding, thus enhancing its practicality.
[0096] The auxiliary components include a first annular plate 24, a second annular plate 25, a funnel 26, two sets of connecting screws 27, two sets of limiting blocks 28, two sets of threaded blocks 29, and two sets of positioning plates 30. The bottom of the main body 1 has a pre-drilled hole, and the bottom of the main body 1 is connected to the top of the first annular plate 24. The left and right ends of the first annular plate 24 each have a set of pre-drilled holes. The two sets of limiting blocks 28 are slidably connected to the pre-drilled holes of the first annular plate 24. The bottom of the left and right ends of the first annular plate 24 each have a set of positioning blocks. The two sets of connecting screws 27 are threadedly connected to the positioning blocks, and the tops of the two sets of connecting screws 27 are connected to the main body 1. The bottom end is rotatably connected, and two sets of threaded blocks 29 are threadedly connected to the connecting screws 27 respectively. One end of each of the two sets of connecting blocks 15 is connected to one end of the limiting block 28, and the other end of each of the two sets of limiting blocks 28 is connected to one end of the second annular plate 25. A funnel 26 is provided on the inner side of the second annular plate 25. When the collection bucket is placed under the main body of the device, the operator rotates the two sets of connecting screws, so that the two sets of threaded blocks drive the limiting blocks to slide. The second annular plate then drives the funnel to slide until the funnel is inserted into the collection bucket. This effectively prevents the powder at the end of the grinding process from falling out of the collection bucket, thus enhancing its practicality.
[0097] Each of the two sets of first bidirectional screws 11 and second bidirectional screws 21 has a set of rotating nuts 31 at its front end, and each of the two sets of connecting screws 27 also has a set of rotating nuts 31 at its bottom; this allows workers to rotate more quickly, thus enhancing practicality.
[0098] Each of the two sets of arc-shaped clamps 22 has a set of anti-slip pads 32 at one end, and the other end of the two sets of anti-slip pads 32 is in close contact with one end of the collection bucket 23; this improves the anti-slip effect and prevents the collection bucket from moving, thus enhancing its practicality.
[0099] A set of hand handles 33 is provided at the top front end of the fixed plate 18; this allows the staff to pull the fixed plate more quickly, thus enhancing its practicality.
[0100] A set of guide plates 34 are respectively provided on the top of the left and right ends of the main body 1; these can guide the soapstone to be ground and crushed, making it easier to grind, thus enhancing its usability.
[0101] Example 4
[0102] Step (1) Mixing and homogenizing raw materials
[0103] Dissolve 3.91 kg of MgSO4 in water in a homogenization container and heat to 80°C. Then, dissolve 4.1 kg of Na2SiO3 (SiO2 content 25%) in water and slowly add it to the homogenization container, stirring until homogeneous. Finally, dissolve 0.18 kg of NaAlO2, 0.6 kg of Na2CO3, and 0.48 kg of NaOH in water and slowly add them to the homogenization container, continuing to stir until the three are evenly mixed. The total mass concentration of the mixture is 15%, resulting in a homogenized slurry.
[0104] Step (2) Liquid crystallization reaction
[0105] The homogenized slurry obtained in step (1) is transferred to a stainless steel reactor and heated for crystallization reaction. The temperature of the crystallization reaction is 200℃, the pressure of the reactor is 1.5-2.2MPa, and the crystallization time is 12h. After the reaction is completed, the reactor is cooled to room temperature and the stainless steel reactor is removed to obtain the crystallized slurry.
[0106] Step (3) Filtration and washing of the slurry after crystallization
[0107] The slurry obtained in step (2) is filtered by a vertical filter press and washed with water to obtain a filter cake. Water is then added to wash away free ionic impurities in the filter cake, and water is added to wash until the conductivity of the effluent is less than 1000 μS / cm.
[0108] Step (4) Drying the filter cake
[0109] The filter cake obtained in step (3) is dried; the filter cake is dried using a tunnel drying device to reduce the moisture content of the filter cake to below 10%.
[0110] Step (5) Crushing the dried filter cake
[0111] The dried filter cake obtained in step (4) is crushed to obtain synthetic soapstone; the dried product is crushed by a grinding mill, and after grinding, it is passed through a 60-mesh sieve. The fineness of the powder reaches more than 60 mesh, thus obtaining the synthetic soapstone SP-4.
[0112] Comparative Example 1
[0113] Step (1) Mixing and homogenizing raw materials
[0114] Weigh 400 g of MgCl2, dissolve it in water in a homogenization container, and heat it to 80℃. Weigh 30 g of Li2CO3, dissolve it in water, add it to the homogenization container, and stir until homogeneous. Weigh 200 g of Na salt, dissolve it in water, slowly add it to the homogenization container, and stir for 30 min to 2 h. Weigh 580 g of Na2SiO3, add it to the homogenization container, and continue stirring until the three are mixed evenly to obtain a mixture. Adjust the pH to between 11 and 12 using NaOH. The total mass concentration of the mixture is 30%.
[0115] Step (2) Liquid crystallization reaction
[0116] The homogenized slurry obtained in step (1) is transferred to a stainless steel reactor and heated for crystallization reaction. The temperature of the crystallization reaction is 150℃, the pressure of the reactor is 1.5-2.2MPa, and the crystallization time is 12h. After the reaction is completed, the reactor is cooled to room temperature and the stainless steel reactor is removed to obtain the crystallized slurry.
[0117] Step (3) Filtration and washing of the slurry after crystallization
[0118] The slurry obtained in step (2) is filtered by a vertical filter press and washed with water to obtain a filter cake. Water is then added to wash away free ionic impurities in the filter cake, and water is added to wash until the conductivity of the effluent is less than 1000 μS / cm.
[0119] Step (4) Drying the filter cake
[0120] The filter cake obtained in step (3) is dried; the filter cake is dried using a tunnel drying device to reduce the moisture content of the filter cake to below 10%.
[0121] Step (5) Crushing the dried filter cake
[0122] The dried filter cake obtained in step (4) is crushed to obtain synthetic soapstone; the dried product is crushed by a grinding mill, and after grinding, it is passed through a 60-mesh sieve. The fineness of the powder reaches more than 60 mesh, which is lithium soapstone RD.
[0123] The SP-1, SP-4, SP-3, SP-4 and RD obtained from Examples 1-4 and Comparative Example 1 were tested. The specific testing methods are as follows:
[0124] 1. SEM morphological observation
[0125] Scanning electron microscopy (SEM) is an observation method that falls between transmission electron microscopy and optical microscopy, and it can be used to observe microscopic morphology.
[0126] 2. FTIR and XRD structural inspection
[0127] Fourier Transform Infrared Spectrometer (FTIR Spectrometer) is an infrared spectrometer that differs from dispersive infrared spectrometers in that it is based on the principle of Fourier transforming the interferometric infrared light. When the sample is irradiated with infrared light of continuously varying frequencies, the molecular groups absorb the radiation at characteristic frequencies. The vibrational or rotational motion of these groups causes changes in the dipole moment, resulting in transitions between the vibrational and rotational energy levels of the molecules from the ground state to excited states, forming the molecular absorption spectrum.
[0128] X-ray diffraction phase analysis is a technique that uses the diffraction effect of X-rays in crystalline materials to analyze the structure of materials.
[0129] 3. Viscosity test of 3% dispersion after standing for 24 hours.
[0130] Using the sol permeability and sol viscosity of lithium saponite as standards, the product was prepared into a dispersion with a mass fraction of 3%. The sol permeability and the sol viscosity after standing for 15 min and 24 h were collected and compared with those of lithium saponite in Comparative Example 1.
[0131] The test results are shown in Table 1 below:
[0132]
[0133] It can be seen that the soapstone synthesized in this invention (Examples 3 and 4) can be rapidly and uniformly dispersed in water to form a transparent sol with swelling properties and good viscosity. After storage, it can form a gel. In addition, the synthesized soapstone can also react with cellulose and other substances to form a more stable bond structure, resulting in greater viscosity, which is more conducive to the thickening, anti-settling and rheological effect improvement of the system.
[0134] The synthesized saponite of this invention exhibits a trioctahedral structure under FTIR and XRD, similar to that of lithium saponite, but differs in interlayer spacing. Scanning electron microscopy (SEM) indicates that it is a nanosheet material; viscosity and dispersion transparency tests show that it possesses dispersion transparency and expansion properties comparable to lithium saponite.
Claims
1. A process for preparing synthetic soapstone, characterized in that... The process includes the following steps: mixing and homogenizing raw materials, liquid crystallization reaction of slurry, washing and filtering of slurry after crystallization, drying of filter cake and crushing of dried filter cake; Step (1) Mixing and homogenizing raw materials: First, add Mg source and stir for homogenization, then add Si source and stir for homogenization, and finally add Al source and pH adjuster and stir for homogenization to obtain a mixed slurry; the Mg source is one of MgO, MgCl2, Mg(OH)2 and MgSO4, with a mass fraction of 35-40 parts; the Si source is one of silica sol and Na2SiO3, with a mass fraction of 40-45 parts; the Al source is one of NaAlO2, Al2(SO4)3 and AlCl3, with a mass fraction of 0.01-0.06 parts; the pH adjuster is NaOH and Na2CO3, with NaOH having a mass fraction of 0.05-0.12 parts and Na2CO3 having a mass fraction of 0.04-0.06 parts; the remainder is deionized water; The raw materials are mixed and homogenized in a homogenization container equipped with stirring and heating. After homogenization and stirring, the raw materials are mixed with water to form a slurry with a mass fraction of 7%-30%. Step (2) Crystallization reaction of slurry: The homogenized slurry of raw materials obtained in step (1) is transferred to a stainless steel reactor and heated for crystallization reaction. After the reaction is completed, it is cooled to room temperature and the stainless steel reactor is removed to obtain the crystallized slurry. The temperature of the crystallization reaction is 150-200℃, the pressure of the reactor is 1.5-2.2MPa, and the crystallization time is 5-24h. Step (3) Filtration and washing of slurry after crystallization: The slurry obtained in step (2) is filtered by a vertical filter press and water is added to wash away free ionic impurities in the filter cake until the conductivity of the effluent is less than 1000 μS / cm, and the filter cake is obtained. Step (4) Filter cake drying: The filter cake obtained in step (3) is dried; a tunnel drying device is used to reduce the moisture content of the filter cake to below 10%; Step (5) Crushing of dried filter cake: The dried filter cake obtained in step (4) is crushed to obtain synthetic soapstone; the dried product is crushed by a grinding mill, and after grinding, it is passed through a 60-mesh sieve, and the fineness of the powder reaches more than 60 mesh. The grinding mill for soapstone preparation production line includes a main body (1), two sets of rolling rollers (2), a power mechanism (3), four sets of support rods (4), and a base plate (5). The bottom of the main body (1) is evenly connected to the top of the four sets of support rods (4), and the bottom of the four sets of support rods (4) is connected to one end of the top of the base plate (5). The main body (1) is provided with a working chamber. The rear end of the working chamber of the main body (1) is rotatably connected to the rear end of the two sets of rolling rollers (2), and the two sets of rolling rollers (2) mesh. The front end of the main body (1) is provided with a power mechanism (3), and the front ends of the two sets of rolling rollers (2) pass through the main body (1). 1) The front end of the working chamber is connected to the power mechanism (3); characterized in that it also includes two sets of support blocks (6), two sets of cleaning brushes (7), four sets of first clamping blocks (8), four sets of first clamping plates (9), mounting plate (10), two sets of first bidirectional screws (11), four sets of first sliders (12), four sets of second clamping blocks (13), buffer assembly, auxiliary assembly and collection assembly, the left and right ends of the working chamber of the device body (1) are respectively provided with a set of reserved holes, and the top and bottom of the two sets of reserved holes of the device body (1) are respectively provided with two sets of slots, and the four sets of first clamping blocks (8) are respectively connected to the slots of the device body (1). The two sets of support blocks (6) are connected to one end of the two sets of first sliders (12) at their top and bottom respectively, and the two sets of support blocks (6) are respectively fitted into the reserved holes of the main body (1) of the device. One end of the two sets of support blocks (6) is connected to one end of the cleaning brush (7) through the buffer component. The other end of the two sets of cleaning brushes (7) is tightly attached to one end of the rolling roller (2). A set of mounting plates (10) is provided on the top of the left and right ends of the main body (1). A set of sliding grooves is provided on the bottom of the two sets of mounting plates (10). The front end and rear end of the two sets of first bidirectional screws (11) are rotatably connected to the sliding grooves of the mounting plates (10) respectively. The four sets of first sliders (12) are threaded to one end of the first bidirectional screw (11), and the four sets of first sliders (12) are slidably connected to the mounting plate (10) groove. The bottom of the four sets of first sliders (12) is connected to the top of the first clamping plate (9). The rear end and front end of the two sets of support blocks (6) are respectively provided with a set of slots. One end of the four sets of second blocks (13) is respectively engaged with the slot of the support block (6), and the other end of the four sets of second blocks (13) is respectively connected to one end of the first clamping plate (9). The bottom of the device body (1) is provided with auxiliary components, and the top of the base plate (5) is provided with collection components.
2. The preparation process of synthetic soapstone according to claim 1, characterized in that: In step (1), the Mg source is dissolved in water in a homogenization container and heated to 50-100℃. Then, the Si source is dissolved in water and slowly added to the homogenization container and stirred evenly. Finally, the Al source and pH adjuster are dissolved in water and slowly added to the homogenization container and stirred continuously to ensure that the three are mixed evenly and a homogenized slurry is obtained.
3. The preparation process of synthetic soapstone according to claim 2, characterized in that, The buffer assembly includes four sets of second sliders (14), two sets of connecting blocks (15), multiple sets of telescopic rods (16) and multiple sets of connecting springs (17). Each of the two sets of supporting blocks (6) has a groove at one end. The top and bottom of the grooves of the two sets of supporting blocks (6) are provided with a sliding groove. The four sets of second sliders (14) are slidably connected to the sliding grooves of the supporting blocks (6). The top and bottom of the two sets of connecting blocks (15) are connected to a set of second sliders (14). One end of the two sets of connecting blocks (15) is evenly connected to one end of multiple sets of telescopic rods (16). The other end of the multiple sets of telescopic rods (16) is connected to one end of the groove of the supporting block (6). A set of connecting springs (17) is provided on the outside of the multiple sets of telescopic rods (16). The other end of the two sets of connecting blocks (15) is connected to one end of the cleaning brush (7).
4. The preparation process of synthetic soapstone according to claim 3, characterized in that, The collection assembly includes a fixed plate (18), two sets of third sliders (19), two sets of fourth sliders (20), a second bidirectional screw (21), two sets of arc-shaped clamps (22), and a collection bucket (23). The top of the base plate (5) is evenly provided with two sets of sliding grooves. The bottom of the two sets of third sliders (19) is slidably connected to the sliding grooves of the base plate (5). The bottom of the fixed plate (18) is evenly connected to the top of the two sets of third sliders (19). The top of the fixed plate (18) is provided with a set of sliding grooves. The front end and rear end of the second bidirectional screw (21) are rotatably connected to one end of the sliding groove of the fixed plate (18). The two sets of fourth sliders (20) are threadedly connected to one end of the second bidirectional screw (21). The two sets of fourth sliders (20) are slidably connected to the sliding grooves of the fixed plate (18). The bottom of the two sets of arc-shaped clamps (22) is connected to the top of the fourth sliders (20). One end of the two sets of arc-shaped clamps (22) is tightly attached to one end of the collection bucket (23).
5. The preparation process of synthetic soapstone according to claim 4, characterized in that, The auxiliary components include a first annular plate (24), a second annular plate (25), a funnel (26), two sets of connecting screws (27), two sets of limiting blocks (28), two sets of threaded blocks (29), and two sets of positioning plates (30). The device body (1) has a pre-drilled hole at its bottom. The bottom of the device body (1) is connected to the top of the first annular plate (24). The left and right ends of the first annular plate (24) each have a set of pre-drilled holes. The two sets of limiting blocks (28) are slidably connected to the pre-drilled holes of the first annular plate (24). The first annular plate (26) 24) A set of positioning blocks are provided at the bottom of the left and right ends respectively. Two sets of connecting screws (27) are threadedly connected to the positioning blocks respectively. The top of the two sets of connecting screws (27) is rotatably connected to one end of the bottom of the main body (1) of the device respectively. Two sets of threaded blocks (29) are threadedly connected to the connecting screws (27) respectively. One end of the two sets of threaded blocks (29) is connected to one end of the limiting block (28) respectively. The other end of the two sets of limiting blocks (28) is connected to one end of the second annular plate (25) respectively. A funnel (26) is provided on the inner side of the second annular plate (25).
6. The preparation process of synthetic soapstone according to claim 5, characterized in that, Two sets of first bidirectional screws (11) and second bidirectional screws (21) are each provided with a set of rotating nuts (31) at their front ends, and two sets of connecting screws (27) are also provided with a set of rotating nuts (31) at their bottoms; two sets of arc-shaped clamps (22) are each provided with a set of anti-slip pads (32) at one end, and the other end of the two sets of anti-slip pads (32) is in close contact with one end of the collection bucket (23); a set of hand handles (33) is provided at the front end of the top of the fixing plate (18); a set of guide plates (34) are provided at the top of the left and right ends of the main body of the device (1).
7. A synthetic soapstone, characterized in that: The synthetic soapstone is prepared according to any one of claims 1-6.
8. An application of a synthetic soapstone, characterized in that: The synthetic soapstone is prepared according to any one of claims 1-6 and applied to a novel water-based thickening rheology modifier.