Preparation method of attapulgite-based lubricating oil friction-reducing and anti-wear additive

By dissociating rod-corrosive rocks and modifying rod-corrosive rocks, the problem of poor dispersion of inorganic silicate clay minerals in lubricating oil is solved, and a high-performance rod-corrosive rock-based lubricating oil friction-reducing and anti-wear additive is prepared. The friction and wear performance of lubricating oil is significantly improved, and the modifier has environmental advantages.

CN116376619BActive Publication Date: 2024-12-10LANZHOU INSTITUTE OF CHEMICAL PHYSICS CHINESE ACADEMY OF SCIENCES
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Patent Information

Application Number
CN202310271699.4
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-03-20
Publication Date
2024-12-10
Estimated Expiration
2043-03-20

AI Technical Summary

Technical Problem

Inorganic silicate clay minerals have poor dispersion and suspension stability in lubricating oils, which limits their large-scale application in the field of lubricating oil additives. Commonly used dispersants and surface modifiers have a great impact on oil performance and may be ecologically toxic. .

Method used

By dissociating the activated sand removal concave and concave rock stone, dissociated concave and concave rock stone with high dispersion, large specific surface area and porous channels is obtained, and lubricating oil base oil is used as a modifier, supplemented with ester The solvents are used as solvents, and they are organically modified to prepare high-performance concave and concave rock-based lubricating oil friction-reducing and anti-wear additives.

Benefits of technology

It significantly improves the dispersion and suspension stability of the concave and concave rock stone, forms a ceramic protective layer with high hardness and low friction coefficient, reduces friction and wear, improves the friction and wear performance of lubricating oil, and the modifier is renewable and degradability, suitable for industrial applications.

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Abstract

The invention discloses a method for preparing a attapulgite-based lubricating oil friction-reducing and anti-wear additive, wherein dissociated attapulgite is first obtained by rod crystal bundle dissociation treatment, and then the dissociated attapulgite is organically modified with lubricating oil base oil and ester and ether substances as composite modifiers to obtain the lubricating oil friction-reducing and anti-wear additive. The invention utilizes the structural characteristics of highly dispersible attapulgite nanorod crystals and multi-porous channels, and further modifies the composite modifier with base oil as a key component, thereby greatly improving the dispersibility and suspension stability of the attapulgite-based friction-reducing and anti-wear additive in a solid-liquid composite lubrication system, improving the thickness, strength and toughness of the friction reaction film, playing a role in anti-wear, friction reduction and self-repair, and realizing the high-value application of attapulgite in the field of lubricating oil.
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Description

Technical Field

[0001] The invention belongs to the technical field of fine chemical industry, relates to a lubricating oil friction reducing and anti-wear additive and a preparation method thereof, and specifically relates to a preparation method of an attapulgite-based lubricating oil friction reducing and anti-wear additive. Background Art

[0002] During the long-term operation of mechanical equipment and systems, mild surface micro-damage will gradually develop into serious surface damage or even failure. In particular, the friction, wear or failure of mechanical equipment in industrial production will bring huge energy consumption, material loss and economic losses to society; and friction and wear will also cause a large amount of greenhouse gas emissions and even serious environmental pollution. Lubricating oil or synthetic lubricating esters are usually added to reduce the friction and wear of mechanical equipment. The anti-friction and anti-wear additives can effectively improve the working performance and service life of mechanical systems and equipment. Therefore, in order to continuously pursue the advancement of lubricant technology to improve equipment efficiency and reliability, the research and development of anti-friction and anti-wear additives and the application technology research have become a hot research topic in the fields of tribology, chemistry, surface engineering and mechanical engineering.

[0003] With the rapid development of micro-nano science and functional materials, layered silicate minerals, tungsten disulfide (WS 2 ), molybdenum disulfide (MoS 2), nano soft metals (Cu, Zn) and ionic liquids as lubricating additives have been experimentally proven to have anti-friction and anti-wear effects. In particular, silicate mineral powders with lamellar structures such as serpentine, talc, kaolinite, montmorillonite and muscovite can significantly improve the lubrication properties of friction materials as anti-wear and anti-friction additives; under the action of friction mechanics, friction chemistry and friction electrochemistry, a reaction film mainly composed of mineral characteristic elements such as Si, Al, Mg and Fe elements will be formed on the friction surface. This reaction film can effectively repair the microscopic damage of the wear surface and enhance its mechanical properties, significantly reduce friction and wear, and improve the operating conditions of mechanical equipment under harsh working conditions such as high speed and heavy load, showing good application prospects. At the same time, organic anti-wear and anti-friction additives containing active elements such as phosphorus, sulfur and nitrogen can also form an adsorption film on the surface of the engine friction pair, which can effectively reduce the friction coefficient and reduce engine wear, showing good anti-friction and anti-wear properties. However, inorganic clay mineral additives always have defects such as poor dispersibility and suspension stability in lubricating oils, making it difficult to exert friction reduction, anti-wear and self-repair functions. They may also cause abrasive wear due to nanoparticle agglomeration, which has become a key factor limiting their large-scale application in the field of lubricating oil additives. In order to solve the problems of dispersibility of inorganic clay mineral micro-nano materials in lubricating oil media, adding dispersants or surface modification are commonly used technical means, but the direct introduction of dispersants or surface modifiers into lubricating oil products will not only affect the final performance of the oil products, but also some dispersants or surface modifiers have poor biodegradability and even have ecotoxicity. The environmental pollution problems caused by them have also attracted widespread attention.

[0004] Attapulgite is a hydrated magnesium-aluminum silicate clay mineral with regular pores (0.37nm×0.64nm) and one-dimensional rod crystals (about 1~5μm long and about 20~70nm in diameter). Its unique crystal structure and excellent colloid, adsorption, carrier and reinforcement properties make it play an important role in many fields of the national economy. With the cross-integration of mineralogy, chemistry, materials science and other disciplines and the rapid development of mineral processing technology, attapulgite has been expanded to high-end application fields such as catalysis, energy storage, tissue engineering, membrane separation, functional coatings, corrosion protection and 3D printing. Based on the systematic understanding of the lubrication mechanism of silicate clay minerals and the structural characteristics and treatment process of attapulgite, the present invention treats the activated and desanded attapulgite slurry with rod crystal bundle dissociation to obtain highly dispersible, large specific surface area and multi-porous dissociated attapulgite. (Scale-up disaggregation of palygorskite crystal bundles via ultrasonic process for using as potentialdrilling fluid, Ultrasonics Sonochemistry, 2022, 89, 106128), further using lubricating oil base oil as a modifier, supplemented by esters, ethers or benzene series as solvents, the highly dispersible dissociated attapulgite is organically modified to obtain a lubricating oil friction reducing additive with high dispersibility and suspension stability in a solid-liquid composite lubrication system. This technology or process can be used as one of the important ways to achieve high-value utilization of attapulgite in the field of lubricating oil friction reducing additives, and there is no relevant research report on this technology, nor is there a precedent for its application. Summary of the invention

[0005] The purpose of the present invention is to provide a method for preparing a attapulgite-based lubricating oil friction reducing and antiwear additive in view of the shortcomings of the above-mentioned inorganic silicate clay minerals, especially attapulgite, in the process of applying the anti-friction and anti-wear and self-repairing of lubricating oils. The method comprises the steps of subjecting the activated and desanded attapulgite to rod crystal bundle dissociation treatment, and then subjecting the dissociated highly dispersed attapulgite to base oil & ester modification to obtain a high-performance attapulgite-based lubricating oil friction reducing and anti-wear additive.

[0006] 1. Preparation of Friction Reducing and Antiwear Additives for Attapulgite-based Lubricating Oils

[0007] The present invention provides a method for preparing a attapulgite-based lubricating oil friction reducing and anti-wear additive, comprising the following steps:

[0008] (1) Dissociation of attapulgite rod crystal bundles: The natural attapulgite ore is first crushed and treated with three rollers, then evenly dispersed in an acidic aqueous solution with a pH value of 3 to 4 and stirred for reaction for 4 to 8 hours. The attapulgite is then subjected to cyclone classification, rod crystal bundle dissociation treatment, filter pressing and strong drying treatment in sequence to obtain dissociated attapulgite.

[0009] Among them, the crushing is to crush the attapulgite to 50-100 meshes, and the subsequent three-roll treatment tears or bulks the attapulgite rod crystal bundles or aggregates through differential extrusion, which is convenient for hydration expansion and depolymerization dispersion; the attapulgite after crushing and extrusion treatment is evenly dispersed in an acidic aqueous solution and stirred for 4-8 hours, which can effectively remove soluble salts and cements between rod crystal bundles, so that the cavitation effect can play a role in the heterogeneous interface or microstructure during the dissociation process; sand removal is to perform hydrocyclone classification treatment on the activated attapulgite slurry, and the content of large-particle quartz sand associated with the attapulgite product can be reduced to 0.5-3.0%. The subsequent rod crystal bundle dissociation treatment is to obtain nano-attapulgite with high dispersibility, large specific surface area and multi-porous structure through processes such as ultrasound, high-pressure homogenization or ultrasonic cell disruption. Organic modification using highly dispersible nano-attapulgite will greatly improve the modification efficiency. The rod crystal bundle dissociation treatment is to subject the attapulgite desanding mortar to cyclic ultrasonic treatment for 10 to 15 minutes at an ultrasonic frequency of 20 to 50 kHz and a power density of 10 to 40 w / L for dissociation; or subject the attapulgite desanding mortar to high pressure homogenization at 30 MPa; or use an ultrasonic cell disruptor to treat the attapulgite desanding mortar at a power of 300-500 W for 20 to 40 minutes. The strong drying temperature of the dissociated attapulgite slurry is 90 to 110°C, and the classification frequency is 5 to 15 Hz, and a nano-attapulgite powder with a moisture content of 2 to 4% can be obtained.

[0010] (2) Preparation of lubricating oil friction-reducing and anti-wear additive: using lubricating oil base oil with a mass content of 5 to 30% of dissociated attapulgite as a modifier, and at least one of ethanol, hexane, petroleum ether, borate ester, oleate ester, phosphate ester or benzene series as a solvent, the modifier and the solvent are mixed to obtain a modified solution; the dissociated attapulgite is dispersed in the modified solution at a high speed and stirred for reaction for 0.5 to 2 hours, and then a paste-like lubricating oil friction-reducing additive is obtained by solid-liquid separation.

[0011] Wherein, the lubricating oil base oil is at least one of mineral base oil, synthetic base oil and bio-based oil; the boric acid ester is at least one of glycerol borate, tributyl borate and triethanolamine borate; the oleic acid ester is at least one of polyethylene glycol oleate, pentaerythritol oleate, monoolein, trimethylolpropane trioleate and triethanolamine monooleate; the benzene series is at least one of benzene, toluene and xylene. The high-speed dispersion process is stirring at 6000-12000rpm for 20-40min, which can realize the full reaction and close combination between the nano-attapulgite rod crystals, base oil and ether and ester molecules. Finally, the solid-liquid separation of the lubricating oil friction and anti-wear additive is achieved by pressure filtration, suction filtration, centrifugation or static sedimentation.

[0012] 2. Performance Characterization of Attapulgite-based Friction Reducing Additives for Lubricating Oils

[0013] There are strong electrostatic attraction and hydrogen bond interactions between natural attapulgite rod crystals, and most of them exist in the form of "wood pile"-shaped rod crystal bundles and their aggregates. Before they are dissociated or dispersed into independent rod crystals, it is difficult to exert the inherent nanorod crystals, pore structure, adsorption, colloid and toughening and reinforcement characteristics, which restricts the high-value utilization of attapulgite resources. Therefore, the efficient dissociation of attapulgite rod crystal bundles is the only way to achieve its high-value and large-scale application. Among them, the dry dissociation of attapulgite has limited effect on the dissociation of rod crystal aggregates, and repeated high-intensity shearing will break the rod crystals and lose the functionality and colloidal properties of the nanomaterial; while the wet rod crystal bundle dissociation (such as high-speed mechanical stirring, ultrasound, microwave, high-pressure homogenization and other methods) can achieve efficient disaggregation and dispersion of attapulgite rod crystal bundles or aggregates without damaging the nanorod crystal structure, which is conducive to the application of attapulgite in high-end functional materials. From the chemical composition changes of attapulgite before and after dissociation (Table 1), it can be seen that the mass fraction of skeleton metal elements (such as Si, Al, Mg, and Fe) in attapulgite has almost no change after dissociation, indicating that its unique layered chain structure has not been destroyed, while the specific surface area has increased from 154 m 2 / g increased to 197 m 2 / g, and the micropore specific surface area increased by 2.7 times. This is because the dispersibility of the rod crystals is improved after dissociation, and the dispersed rod crystals are disorderly accumulated to form a multi-porous structure, which increases the specific surface area and pore volume (Table 2, Figure 2 ); SEM and TEM images before and after dissociation from attapulgite ( Figure 1 ) It is more intuitively observed that the dispersibility of the rod crystals is improved after dissociation, the number of individually dispersed nanorod crystals increases, and the surface electronegativity of the attapulgite increases after dissociation (see Zeta potential in Table 2), which leads to an increase in the repulsive force between the rod crystals and an improvement in the suspension stability, which is conducive to the formation of a three-dimensional network structure between the rod crystals and improves the viscosity and suspension stability of the suspension; Figure 3 The rotational viscosity, rheological properties and suspension stability of the dissociated attapulgite after redispersion have been greatly improved, which also confirms that the dispersibility, suspension stability and colloidal properties of the dissociated attapulgite will be greatly improved. Therefore, the dissociated nano-attapulgite is conducive to the subsequent modification process, so that as many organic molecules as possible such as base oil, ester, ether, etc. are adsorbed on the surface of the attapulgite or reside in the pores, thereby improving the modification effect and rate.

[0014]

[0015]

[0016] After activation and sand removal, the attapulgite is dispersed in lubricating oil at high speed and will show obvious sedimentation within 24 hours (see Figure 4 , Figure 5Right), its suspension stability in lubricating oil does not meet the basic requirements of lubricating oil additives; after the dissociated attapulgite is modified by lubricating oil base oil, ester, ether, etc., the lipophilicity of the attapulgite and the dispersion stability in the oil phase are greatly improved. After standing for 10 days, the attapulgite dispersed in the oil phase has almost no sedimentation, showing good dispersibility and suspension stability (see Figure 5 ). Under the action of friction and load, attapulgite nanorod crystals can be woven into a uniform and dense network structure on the friction surface, and further react to form a continuously adhered friction reaction film, which plays a certain role in isolating the friction pair; the highly active metal atoms in the attapulgite rod crystal structure form a high-hardness, low-friction coefficient ceramic protective layer on the friction pair surface through tribochemical reactions, which has a good anti-friction and anti-wear effect; at the same time, attapulgite nanorod crystals are extremely small in size and have a large specific surface area, which can be easily adsorbed or filled in the dents and damaged areas on the friction pair surface, playing a repair and smoothing role, further reducing the friction and wear on the friction pair surface. From the change in friction coefficient after adding attapulgite-based lubricant anti-friction additives, it can be seen that after adding attapulgite-based lubricant anti-friction additives, the average friction coefficient of the lubricant can be reduced from 0.3817 without addition to 0.1941, and the wear scar diameter and groove depth are smaller, showing excellent anti-friction and anti-wear performance (see Figure 6 ).

[0017] In summary, the attapulgite-based lubricant anti-friction additive of the present invention has the following advantages compared with the prior art:

[0018] 1. Based on a full understanding of the lubrication mechanism of clay minerals and the nanostructure characteristics of attapulgite, the present invention firstly improves the dispersibility of attapulgite nanorod crystals by dissociating the attapulgite rod crystal bundles, thereby obtaining nano attapulgite with high adsorption and suspension properties, which greatly improves the modification efficiency of subsequent base oils; further, the dissociated attapulgite is compositely modified by lubricating oil base oils, esters, ethers, etc., to obtain an attapulgite-based anti-friction and anti-wear additive, which exhibits good anti-friction and anti-wear performance and industrial application prospects.

[0019] 2. The present invention makes full use of the high dispersion, suspension stability and multi-porous structure characteristics of dissociated attapulgite nanorod crystals, and preferably uses lubricating oil base oil and substances such as borate, oleate or petroleum ether to carry out organic modification reaction on the dissociated attapulgite to obtain a attapulgite-based anti-friction and anti-wear additive; under the action of friction and load, a ceramic surface protection film with high hardness and low friction coefficient will be quickly and continuously formed behind the friction surface, which plays a role in reducing friction and anti-wear. The obtained lubricating oil has good thermal stability, and the nanorod crystals are adsorbed or filled in the dents and damaged parts on the surface of the friction pair to play a self-repairing role.

[0020] 3. The lubricating oil friction reduction and anti-wear additive prepared by the present invention has good dispersibility and suspension when added in an amount of 0.25-2.0 wt.% in the lubricating oil; when the added amount is 0.5%, the friction coefficient is reduced by 48.46% compared with that without addition, which significantly improves the friction and wear performance of various lubricating oils; the used attapulgite is a natural green nano-mineral material, and modifiers such as esters and ethers have the advantages of renewability and degradability, which can improve the friction noise and heat transfer of the metal surface, and the chemical reagents used in the preparation process can be recycled, so the preparation process has the advantages of controllable cost and improved quality and efficiency. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] Figure 1 SEM (a, b) and TEM (c, d) images of attapulgite and dissociated attapulgite;

[0022] Figure 2 is the N before and after attapulgite dissociation 2 Adsorption-desorption curve (a) and pore size distribution curve (b);

[0023] Figure 3 The rotational viscosity change curve of attapulgite before and after dissociation (a); the shear stress change curve (b); the sedimentation curve of 2% suspension (c);

[0024] Figure 4 To determine the suspension stability of attapulgite ore in lubricating oil after sand removal;

[0025] Figure 5 The comparison of suspension stability of attapulgite-based lubricant anti-friction additives in lubricant;

[0026] Figure 6 The change of friction coefficient with or without adding attapulgite-based lubricant anti-friction additive. DETAILED DESCRIPTION

[0027] The preparation method and performance of the attapulgite-based lubricant anti-friction additive of the present invention are further described below by means of specific examples. The friction experiment is tested by a ball-disc friction and wear tester, the upper sample is an 8 mm steel ball fixed in a fixture, the lower sample is a steel sheet, and the lubrication method is oil drip lubrication.

[0028] Example 1

[0029] The preparation method of the attapulgite-based lubricating oil friction reducing additive is as follows: first, the mixed attapulgite clay is crushed (<100 mesh) and treated with three rollers, then uniformly dispersed in a sulfuric acid aqueous solution with a pH value of 4 and stirred for 8 hours, and then subjected to three-stage hydrocyclone sand removal, ultrasonic rod crystal beam dissociation treatment, filter pressing and strong drying treatment (110℃, 5Hz) to obtain the dissociated mixed attapulgite clay; wherein the ultrasonic rod crystal beam dissociation treatment is a cyclic ultrasonic treatment for 15 minutes at an ultrasonic frequency of 20kHz and a power density of 40w / L. 10g of the dissociated mixed attapulgite clay is dispersed at high speed (8000 rpm, 40 min) in a mixed solution of 100mL of petroleum ether and polyalphaolefin synthetic oil PAO6 (containing 3g PAO6) and stirred for 2 hours, and the attapulgite-based lubricating oil friction reducing and anti-wear additive is obtained by suction filtration.

[0030] Take 0.15g of the above-mentioned lubricant anti-friction additive, disperse it at high speed (6000rpm, 40min) in 30g of polyalphaolefin synthetic oil PAO6, and observe the dispersibility and suspension of the anti-friction additive in the lubricant. The results show that after standing for 10 days, the anti-friction additive is still well dispersed in the lubricant phase (see Figure 5 ).

[0031] Example 2

[0032] The preparation method of the attapulgite-based lubricating oil friction reducing additive is as follows: first, after the mixed-dimensional attapulgite clay is crushed (<100 mesh) and treated with three rollers, it is uniformly dispersed in a sulfuric acid aqueous solution with a pH value of 3 and stirred for 4 hours, and then subjected to three-stage hydrocyclone sand removal, rod crystal bundle dissociation treatment, filter pressing and strong drying treatment (90℃, 15Hz) to obtain the dissociated mixed-dimensional attapulgite clay; wherein the rod crystal bundle dissociation treatment is achieved by high-pressure homogenization treatment of the attapulgite desanding slurry at 30MPa. 10g of the dissociated mixed-dimensional attapulgite clay is dispersed at high speed (8000 rpm, 40 min) in 100mL of a mixed solution of triethanolamine monooleate and polyalphaolefin synthetic oil PAO6 (containing 0.5g PAO6) and stirred for 0.5h, and the attapulgite-based lubricating oil friction reducing and anti-wear additive is obtained by centrifugation.

[0033] Take 0.15g of the above-mentioned lubricating oil anti-friction and anti-wear additive, disperse it at high speed (12000rpm, 20min) in 30g of polyalphaolefin synthetic oil PAO6, and observe the dispersibility and suspension of the anti-friction and anti-wear additive in the lubricating oil. The results show that after standing for 10 days, the anti-friction and anti-wear additive of the lubricating oil is still well dispersed in the lubricating oil phase (see Figure 5). The friction test confirmed that the lubricating oil sample with the attapulgite-based lubricating oil friction and anti-wear additive had a smaller average friction coefficient than the sample without the friction and anti-wear additive (see Figure 6 Left).

[0034] Example 3

[0035] The preparation method of the attapulgite-based lubricating oil friction reducing additive is as follows: first, the mixed attapulgite clay is crushed (<100 mesh) and treated with three rollers, then uniformly dispersed in a sulfuric acid aqueous solution with a pH value of 4 and stirred for 8 hours, and then subjected to three-stage hydrocyclone sand removal, rod crystal bundle dissociation treatment, filter pressing and strong drying treatment (110℃, 15Hz) to obtain the dissociated mixed attapulgite clay; wherein, the rod crystal bundle dissociation treatment uses an ultrasonic cell disruptor to treat the attapulgite sand removal slurry at a power of 500W for 40 minutes. 10g of the dissociated mixed attapulgite clay is dispersed at high speed (8000 rpm, 40 min) in a mixed solution of 100mL of glycerol borate and poly α-olefin synthetic oil PAO6 (containing 0.5g PAO6) and stirred for 2 hours, and the attapulgite-based lubricating oil friction reducing and anti-wear additive is obtained by suction filtration.

[0036] Take 0.3g of the above lubricant anti-friction additive, disperse it at high speed (10000rpm, 40min) in 30g of polyalphaolefin synthetic oil PAO6, and observe the dispersibility and suspension of the anti-friction additive in the lubricant. The results show that after standing for 10 days, the anti-friction additive is still well dispersed in the lubricant phase (see Figure 5 ).

[0037] Example 4

[0038] The preparation method of the attapulgite-based lubricating oil friction reducing additive is as follows: first, the Xuyi attapulgite (taken from the Baihushan mine) is crushed (<100 mesh) and treated with three rollers, then evenly dispersed in a sulfuric acid aqueous solution with a pH value of 3 and stirred for 8 hours, and then subjected to three-stage hydrocyclone sand removal, rod crystal bundle dissociation treatment, filter pressing and strong drying treatment (110°C, 15Hz) to obtain dissociated attapulgite; wherein the ultrasonic rod crystal bundle dissociation treatment is a cyclic ultrasonic treatment for 10 minutes at an ultrasonic frequency of 50kHz and a power density of 40w / L. 10g of the dissociated attapulgite is dispersed at high speed (10000 rpm, 40 min) in a mixed solution of 100mL of monoolein and dimethyl silicone oil (containing 3g of dimethyl silicone oil) and stirred for 2 hours, and the attapulgite-based lubricating oil friction reducing and anti-wear additive is obtained by suction filtration.

[0039] 0.15g of the above-mentioned attapulgite-based lubricant anti-friction additive was dispersed in 30g of dimethyl silicone oil at high speed (10000rpm, 40min), and the dispersibility and suspension of the anti-friction additive in the lubricant were observed. The results showed that after standing for 10 days, the anti-friction additive was still well dispersed in the lubricant phase (see Figure 5 ). The friction test confirmed that the lubricating oil sample with the attapulgite-based lubricating oil friction and anti-wear additive had a smaller average friction coefficient than the sample without the friction and anti-wear additive (see Figure 6 right).

[0040] Comparative Example 1

[0041] The mixed-dimensional attapulgite clay was crushed (<100 mesh) and treated with three rollers, then evenly dispersed in a sulfuric acid aqueous solution with a pH value of 4 and stirred for reaction for 8 hours. After three-stage hydrocyclone sand removal and drying, the purified mixed-dimensional attapulgite clay was obtained. 0.15g of the above-mentioned purified mixed-dimensional attapulgite clay was taken and dispersed at high speed (8000 rpm, 40 min) in 30 g of poly-α-olefin synthetic oil PAO6, and the dispersibility and suspension of the mixed-dimensional attapulgite clay in the lubricating oil were observed. The results showed that after standing for 12 hours, the purified mixed-dimensional attapulgite clay in the oil phase had obviously settled, and a clear solid-liquid two-phase interface appeared (see Figure 4 ).

[0042] Comparative Example 2

[0043] The Xuyi attapulgite (taken from the Baihushan mine) was crushed (<100 mesh), treated with three rollers, and then evenly dispersed in a sulfuric acid aqueous solution with a pH value of 3 and stirred for 4 hours. After three-stage hydrocyclone sand removal and drying, purified attapulgite was obtained. 0.15g of the above purified attapulgite was taken and dispersed at high speed (11000 rpm, 20 min) in 30g of dimethyl silicone oil. The dispersibility and suspension of the purified attapulgite in the lubricating oil were observed. The results showed that after standing for 24 hours, the purified attapulgite in the oil phase had obviously settled (see Figure 5 ).

Claims

1. A method for preparing an attapulgite-based lubricating oil friction reducing and anti-wear additive, comprising the following steps: (1) Treatment of dissociation of attapulgite rod crystal bundles: First, the natural attapulgite ore is crushed and treated with three rollers, then evenly dispersed in an acidic aqueous solution with a pH value of 3 to 4 and stirred for reaction for 4 to 8 hours, and then subjected to cyclone classification, rod crystal bundle dissociation treatment, filter pressing and strong drying treatment in sequence to obtain dissociated attapulgite; The crushing is to crush the attapulgite to 50-100 meshes; the temperature of the strong drying treatment is 90-110°C, and the classification frequency is 5-15Hz; the rod crystal bundle dissociation treatment is to subject the attapulgite desanding mortar to a cyclic ultrasonic treatment at a frequency of 20-50kHz and a power density of 10-40w / L for 10-15min, or to subject the attapulgite desanding mortar to a high-pressure homogenization treatment at 30MPa, or to use an ultrasonic cell disruptor to treat the attapulgite desanding mortar at a power of 300-500W for 20-40min; (2) Preparation of lubricating oil friction reducing and anti-wear additive: dissociated attapulgite is dispersed in a modified solution at a solid-liquid ratio of 1:5 to 1:10 at high speed, and the modified solution is continuously stirred for 0.5 to 2 hours, and then the lubricating oil friction reducing and anti-wear additive is obtained by solid-liquid separation; wherein, The modified solution is obtained by mixing lubricating base oil with 5-30% of the mass of dissociated attapulgite as a modifier and at least one of ethanol, hexane, petroleum ether, boric acid ester, oleic acid ester, phosphate ester, polyol ester and benzene series as a solvent.

2. The method for preparing a attapulgite-based antifriction and antiwear additive for lubricating oil according to claim 1, characterized in that: In step (2), the borate ester is at least one of glycerol borate, tributyl borate and triethanolamine borate; the oleate ester is at least one of polyethylene glycol oleate, pentaerythritol oleate, glyceryl monooleate, trimethylolpropane trioleate and triethanolamine monooleate; and the benzene series is at least one of benzene, toluene and xylene.

3. The method for preparing a attapulgite-based antifriction and antiwear additive for lubricating oil according to claim 1, characterized in that: In step (2), the high-speed dispersion is stirring at 6000-12000 rpm for 20-40 minutes.