阅读说明：本技术 一种水溶性纳米轮带高温超润滑剂的制备方法 (Preparation method of water-soluble nano wheel belt high-temperature super-lubricant ) 是由 武刚 谢兴存 于 2021-08-10 设计创作，主要内容包括：本发明提供一种水溶性纳米轮带高温超润滑剂的制备方法,首先是三明治结构固体添加剂MoS-(2)/石墨烯/MoS-(2)和水性生物基杀菌剂碳纳米管/溶菌酶的制备；然后是油相混合液和水相溶液的制备：取润滑剂、乳化剂、油性杀菌剂依次添加到基础油中,于50～60℃下,充分搅拌,得油相混合液；取防腐防锈剂、水性生物基杀菌剂碳纳米管/溶菌酶依次添加到水中,充分溶解,得水相溶液；接着,将水相溶液添加到油相混合液中,搅拌均匀,得乳化液；随后,将三明治结构固体添加剂MoS-(2)/石墨烯/MoS-(2)添加到乳化液中,搅拌,得胶质混合物；最后,将胶质混合物在三辊球磨机中进行均质2～3遍,即得水溶性纳米轮带高温超润滑剂。该产品可降低轮带和垫板之间的相对摩擦,提高设备寿命和降低能耗。(The invention provides a preparation method of a water-soluble nano high-temperature super lubricant for a belt wheel, which comprises the following steps of firstly, preparing a sandwich structure solid additive MoS 2 graphene/MoS 2 And preparing the water-based bio-based bactericide carbon nano tube/lysozyme; then preparing an oil phase mixed solution and an aqueous phase solution: sequentially adding a lubricant, an emulsifier and an oily bactericide into base oil, and fully stirring at 50-60 ℃ to obtain an oil phase mixed solution; adding the corrosion-resistant antirust agent and the water-based bio-based bactericide carbon nano tube/lysozyme into water in sequence, and fully dissolving to obtain a water-phase solution; then, adding the water phase solution into the oil phase mixed solution, and uniformly stirring to obtain an emulsion; subsequently, the sandwich structure solid additive MoS 2 graphene/MoS 2 Adding into the emulsion, and stirring to obtain colloid mixture; and finally, homogenizing the colloid mixture in a three-roll ball mill for 2-3 times to obtain the water-soluble nano wheel belt high-temperature super-lubricant. The product can reduce the relative friction between the belt and the backing plate, prolong the service life of equipment and reduce energy consumption.)

1. The preparation method of the water-soluble nano high-temperature super lubricant for the wheel belt is characterized by comprising the following steps of:

1) solid additive sandwich structure MoS₂graphene/MoS₂The preparation of (1): adding molybdenum disulfide into an organic hydrocarbon solution in an organic lithium salt, and magnetically stirring for 2-3 h, wherein the molar weight ratio of the molybdenum disulfide to the organic lithium salt is 1: 2; stirring the mixed solution for 5-8 days under the condition of inert argon atmosphere at room temperature, washing with an organic hydrocarbon solvent and drying under reduced pressure to obtain LiMoS₂(ii) a Mixing LiMoS₂Adding the mixture into deionized water, and carrying out ultrasonic treatment for 2-3 h to obtain the LiMoS with the layer stripped₂(ii) a CTAB is completely dissolved into deionized water (the mass ratio of CTAB to deionized water is 1:5), and LiMoS is stripped from the layer₂Fully mixing and carrying out ultrasonic treatment for 2-3 h to form LiMoS with peeled stratum₂-CTA⁺A solution; to the above LiMoS₂-CTA⁺Adding a dispersion solution of Graphene Oxide (GO) into the solution, and continuing to perform ultrasonic treatment for 2-3 h to form LiMoS₂-CTA⁺-GO solution; adding a reducing agent to the LiMoS₂-CTA⁺Transferring the GO solution into a reaction kettle to react for 6-8 h at 160-180 ℃, filtering the precipitate, washing the precipitate with deionized water and ethanol for 3-5 times, and freeze-drying the precipitate for 18-24 h to obtain MoS₂graphene/MoS₂；

2) Preparing the water-based bio-based bactericide: adding carbon nanotubes to a molar concentration of 10^-3 ~10^-4Putting the solution into an ultrasonic bath for 15-20 min in a mol/L lysozyme water solution, then putting the solution into an ice bath, performing ultrasonic treatment for 60-90 min, and centrifuging to obtain the carbon nano tube/lysozyme;

3) preparing an oil phase mixed solution: sequentially adding a lubricant, an emulsifier and an oily bactericide into base oil, and fully stirring at 50-60 ℃ to obtain an oil phase mixed solution;

4) preparation of aqueous phase solution: adding the corrosion-resistant antirust agent and the water-based bio-based bactericide carbon nano tube/lysozyme into water in sequence, and fully dissolving;

5) preparation of an emulsion: adding the water phase solution obtained in the step 4) into the oil phase mixed solution obtained in the step 3), and uniformly stirring;

6) preparation of gum mixture: adding solid additive into MoS with sandwich structure₂graphene/MoS₂Adding the mixture into the emulsion obtained in the step 5), and stirring;

7) homogenizing the colloid mixture obtained in the step 6) in a three-roll ball mill for 2-3 times to obtain the water-soluble nano wheel belt high-temperature super-lubricant.

2. The method for preparing the water-soluble nano wheel belt high-temperature super-lubricant according to claim 1, wherein in the step 1), the organic lithium salt is one or a combination of n-butyl lithium, lithium lactate and isoamyl lithium; the organic hydrocarbon is one or the combination of n-pentane, isopropane or n-butane; the reducing agent is one or the combination of thiourea or sodium borohydride.

3. The preparation method of the water-soluble nano-sized high-temperature super-lubricant for the belt wheel as claimed in claim 1, wherein in the step 3), the lubricant is composed of pentaerythritol oleate and polyether, and the weight ratio of the pentaerythritol oleate to the polyether is 2: 1-4: 1; the composite emulsifier consists of tween-80, petroleum sodium sulfonate and span-80, wherein the weight ratio of the tween-80 to the petroleum sodium sulfonate to the span-80 is 6:2: 1-3: 1: 0.1; the oily bactericide consists of BK, BIT-20 and IPBC, wherein the weight ratio of the BK, the BIT-20 and the IPBC is 10:5: 1-10: 10: 1; the base oil is one or the combination of mineral oil, trimellitate and PAO.

4. The method for preparing the water-soluble nano high-temperature super-lubricant for the wheel belt according to claim 1, wherein in the step 4), the corrosion-resistant and rust-proof agent is one or a combination of triethanolamine, triethanolamine sebacate and benzotriazole.

Technical Field

The invention relates to the technical field of lubricants, in particular to a preparation method of a water-soluble nano wheel belt high-temperature super lubricant.

Background

At present, in rotary kilns in the cement industry, high-temperature equipment in the industries of steel, chemical engineering and the like, a lubricating technology is a key link of production; the development of lubricants restricts the development of the industry. Taking a rotary kiln as an example, the rotary kiln is a key device for cement plant production. The device rotates through a gear, and a support consisting of three groups of riding wheels and a wheel belt is arranged in the middle of the device and performs rotary motion; the backing plate is a strip-shaped support which is arranged in an arc-shaped gap between the rotary kiln body and the belt wheel and plays the roles of cooling the cylinder body and the belt wheel, transmitting torque and facilitating the installation of the belt wheel.

The rotary kiln wheel belt plays a role in supporting the kiln body, a certain gap exists between the wheel belt and the kiln body, and the wheel belt and the kiln body move relatively in the rotary kiln running process to form a sliding friction pair. Therefore, sufficient care must be taken to lubricate the inner surface of the belt and the kiln body pad at the corresponding position. If the lubrication of the area is insufficient or improper, the accelerated abrasion of the backing plate can be caused, and the running stability of the kiln body is influenced, so that the stability of the kiln bricks is reduced, even the bricks fall off, the kiln is stopped, and the production is reduced.

The rotary kiln wheel belt continuously works for a long time at the high temperature of 270-370 ℃ and under several tens of tons of heavy loads, and the working conditions are very harsh. At present, products in the market mainly adopt oil-based products, for example, Chinese patent CN102559348A can form a high-strength high-temperature protection lubricating film, and effectively prevent the rotary kiln from shaking, twisting, deforming and falling off of refractory bricks. Although oil-based oil has good lubricity, under the condition of high temperature of 300 ℃, oil products are seriously oxidized and volatilized, oil products are seriously smoky, and fire disasters can occur, so that the environment is polluted, and the safe use of equipment is endangered. The pure water-based tyre agent has high volatilization speed at high temperature, no flash point and no smoke generation, but is difficult to ensure continuous and effective lubrication.

With the increasing attention on environmental protection and energy conservation in the world, the oil-based belting agent widely used at present has the defects of poor biodegradability and environmental pollution, and is facing the severe test of environmental requirements, while the lubricating performance of water-based lubricating products can not reach satisfactory degree; therefore, the development of a belt pulley agent product which is environment-friendly, high-temperature resistant, good in lubricating property and safe to use becomes a new development direction.

Therefore, a preparation method of the water-soluble nano wheel belt high-temperature super-lubricant is provided. MoS with sandwich structure prepared by charge attraction and hydrothermal reduction method₂graphene/MoS₂. The invention inserts graphene into layered MoS₂In the form of a layered MoS₂MoS with sandwich structure with increased interlayer spacing₂graphene/MoS₂Molybdenum disulfide is not easy to carbonize at high temperature, so that the molybdenum disulfide keeps better lubricity and the reduction of the service life of the molybdenum disulfide due to the influence of high temperature can be effectively avoided; meanwhile, the carbon nano tube and the lysozyme are compounded in the water-based bio-based bactericide, so that the dispersity of the lysozyme can be improved, and the bactericidal performance of the lysozyme is further improved. The lubricating and heat dissipating functions and the controllability of biological colonies are good, the service lives of the belt and the equipment can be greatly reduced, and the energy transition loss caused by friction is reduced.

Disclosure of Invention

The invention aims to provide a preparation method of a water-soluble nano wheel belt high-temperature super lubricant₂graphene/MoS₂Meanwhile, the lubricating property of the lubricant is improved by adopting a water-oil-based mixing mode, the dual characteristics of the oil-based lubricant and the water-based lubricant are combined, the inevitable defects of the oil-based lubricant and the water-based lubricant are overcome, and the lubricant is a product with very high cost performance. MoS based on insertion of graphene into a layer₂In the form of a layered MoS₂MoS with sandwich structure with increased interlayer spacing₂graphene/MoS₂Molybdenum disulfide is not easy to carbonize at high temperature, so that the molybdenum disulfide keeps good lubricity; in the aqueous bio-based bactericideThe carbon nano tube is compounded with the lysozyme, so that the dispersity of the lysozyme can be improved, and the sterilization performance of the lysozyme can be improved.

In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of a water-soluble nano wheel belt high-temperature super lubricant comprises the following steps,

1) solid additive sandwich structure MoS₂graphene/MoS₂The preparation of (1): adding molybdenum disulfide into an organic hydrocarbon solution in an organic lithium salt, and magnetically stirring for 2-3 h, wherein the molar weight ratio of the molybdenum disulfide to the organic lithium salt is 1: 2; stirring the mixed solution for 5-8 days under the condition of inert argon atmosphere at room temperature, washing with an organic hydrocarbon solvent and drying under reduced pressure to obtain LiMoS₂(ii) a Mixing LiMoS₂Adding the mixture into deionized water, and carrying out ultrasonic treatment for 2-3 h to obtain the LiMoS with the layer stripped₂(ii) a CTAB is completely dissolved into deionized water (the mass ratio of CTAB to deionized water is 1:5), and LiMoS is stripped from the layer₂Fully mixing and carrying out ultrasonic treatment for 2-3 h to form LiMoS with peeled stratum₂-CTA⁺A solution; to the above LiMoS₂-CTA⁺Adding a dispersion solution of Graphene Oxide (GO) into the solution, and continuing to perform ultrasonic treatment for 2-3 h to form LiMoS₂-CTA⁺-GO solution; adding a reducing agent to the LiMoS₂-CTA⁺Transferring the GO solution into a reaction kettle to react for 6-8 h at 160-180 ℃, filtering the precipitate, washing the precipitate with deionized water and ethanol for 3-5 times, and freeze-drying the precipitate for 18-24 h to obtain MoS₂graphene/MoS₂；

2) Preparing the water-based bio-based bactericide: adding carbon nanotubes to a molar concentration of 10^-3～10^-4Putting the solution into an ultrasonic bath for 15-20 min in a mol/L lysozyme water solution, then putting the solution into an ice bath, performing ultrasonic treatment for 60-90 min, and centrifuging to obtain the carbon nano tube/lysozyme;

3) preparing an oil phase mixed solution: sequentially adding a lubricant, an emulsifier and an oily bactericide into base oil, and fully stirring at 50-60 ℃ to obtain an oil phase mixed solution;

4) preparation of aqueous phase solution: adding the corrosion-resistant antirust agent and the water-based bio-based bactericide carbon nano tube/lysozyme into water in sequence, and fully dissolving;

5) preparation of an emulsion: adding the water phase solution obtained in the step 4) into the oil phase mixed solution obtained in the step 3), and uniformly stirring;

6) preparation of gum mixture: adding solid additive into MoS with sandwich structure₂graphene/MoS₂Adding the mixture into the emulsion obtained in the step 5), and stirring;

7) homogenizing the colloid mixture obtained in the step 6) in a three-roll ball mill for 2-3 times to obtain the product.

Preferably, in the step 1), the organic lithium salt is one or a combination of n-butyl lithium, lithium lactate and isoamyl lithium; the organic hydrocarbon is one or the combination of n-pentane, isopropane or n-butane; the reducing agent is one or the combination of thiourea or sodium borohydride;

preferably, in the step 3), the lubricant is composed of pentaerythritol oleate and polyether, and the weight ratio of the pentaerythritol oleate to the polyether is 2: 1-4: 1; the composite emulsifier consists of tween-80, petroleum sodium sulfonate and span-80, wherein the weight ratio of the tween-80 to the petroleum sodium sulfonate to the span-80 is 6:2: 1-3: 1: 0.1; the oily bactericide consists of BK, BIT-20 and IPBC, wherein the weight ratio of the BK, the BIT-20 and the IPBC is 10:5: 1-10: 10: 1; the base oil is one or the combination of mineral oil, trimellitate and PAO;

preferably, in the step 4), the anticorrosive and antirust agent is one or a combination of triethanolamine, triethanolamine sebacate and benzotriazole.

Compared with the prior art, the invention has the following beneficial effects:

MoS is added into the water-soluble nano wheel belt high-temperature super-lubricant provided by the invention₂graphene/MoS₂Meanwhile, the lubricating property of the lubricant is improved by adopting a water-oil-based mixing mode, and the dual characteristics of an oil-based lubricant and a water-based lubricant are achieved. MoS based on insertion of graphene into a layer₂In the form of a layered MoS₂The interlayer spacing is increased, so that the molybdenum disulfide and the graphene are combined through chemical bonds, and the MoS with a sandwich structure₂graphene/MoS₂Make twoMolybdenum sulfide is not easy to carbonize at high temperature, so that the molybdenum sulfide keeps good lubricating and heat dissipating properties; the carbon nano tube and the lysozyme are compounded in the water-based bio-based bactericide, so that the dispersity of the lysozyme can be improved, and the bactericidal performance of the lysozyme is further improved.

Drawings

FIG. 1 is a MoS sandwich structure of example 1₂graphene/MoS₂SEM image of

FIG. 2 is an SEM image of the water-soluble nanowheel belt diluted with the high-temperature super-lubricant in example 2

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

The first embodiment is as follows:

1) solid additive sandwich structure MoS₂graphene/MoS₂The preparation of (1): adding molybdenum disulfide into an n-pentane solution in n-butyllithium, and magnetically stirring for 2 hours, wherein the molar weight ratio of the molybdenum disulfide to the n-butyllithium is 1: 2; stirring the mixed solution for 5 days under the condition of inert argon atmosphere at room temperature, washing the mixed solution by using an n-pentane solvent and drying the mixed solution under the reduced pressure condition to obtain LiMoS₂(ii) a Mixing LiMoS₂Adding into deionized water, and performing ultrasonic treatment for 2h to obtain layered LiMoS₂(ii) a CTAB is completely dissolved into deionized water (the mass ratio of CTAB to deionized water is 1:5), and LiMoS is stripped from the layer₂Mixing thoroughly and sonicating for 2h to form exfoliated LiMoS₂-CTA⁺A solution; to the above LiMoS₂-CTA⁺Adding a dispersion solution of Graphene Oxide (GO) into the solution, and continuing to perform ultrasonic treatment for 2 hours to form LiMoS₂-CTA⁺-GO solution; thiourea was added to the LiMoS₂-CTA⁺Transferring the solution to a reaction kettle for reacting for 8 hours at 160 ℃ in the-GO solution, filtering the precipitate, washing the precipitate for 3 times by deionized water and ethanol, and obtaining MoS through freeze drying for 18 hours₂graphene/MoS₂；

2) Preparing the water-based bio-based bactericide: adding carbon nanotubes to a molar concentration of 10^-3Putting the solution in an ultrasonic bath for 15min in a mol/L lysozyme water solution, then putting the solution in an ice bath for ultrasonic treatment for 60min, and centrifuging to obtain the carbon nano tube/lysozyme;

3) preparing an oil phase mixed solution: taking lubricant pentaerythritol oleate and polyether (the weight ratio is 3:1), emulsifier Tween-80, sodium petroleum sulfonate and span-80 (the weight ratio is 3:2:1), oily bactericide BK, BIT-20 and IPBC (the weight ratio is 10:6: 1); sequentially adding into base oil, and stirring at 50 deg.C to obtain oil phase mixture;

4) preparation of aqueous phase solution: sequentially adding the corrosion-resistant antirust agent triethanolamine and the water-based bio-based bactericide carbon nano tube/lysozyme into water, and fully dissolving;

5) preparation of an emulsion: adding the water phase solution obtained in the step 4) into the oil phase mixed solution obtained in the step 3), and uniformly stirring;

6) preparation of gum mixture: adding solid additive into MoS with sandwich structure₂graphene/MoS₂Adding the mixture into the emulsion obtained in the step 5), and stirring;

7) homogenizing the colloid mixture obtained in the step 6) in a three-roll ball mill for 2 times to obtain the water-soluble nano wheel belt high-temperature super-lubricant.

Example two:

1) solid additive sandwich structure MoS₂graphene/MoS₂The preparation of (1): adding molybdenum disulfide into a normal butane solution in lithium lactate, and magnetically stirring for 3 hours, wherein the molar weight ratio of the molybdenum disulfide to the lithium lactate is 1: 2; stirring the mixed solution for 8 days under the condition of inert argon atmosphere at room temperature, washing with n-butane solvent and drying under reduced pressure to obtain LiMoS₂(ii) a Mixing LiMoS₂Adding into deionized water, and performing ultrasonic treatment for 3h to obtain layered LiMoS₂(ii) a CTAB is completely dissolved into deionized water (the mass ratio of CTAB to deionized water is 1:5), and LiMoS is stripped from the layer₂Mixing thoroughly and sonicating for 2h to form exfoliated LiMoS₂-CTA⁺A solution; to the above LiMoS₂-CTA⁺Adding a dispersion solution of Graphene Oxide (GO) into the solution, and continuing to perform ultrasonic treatment for 2 hours to form LiMoS₂-CTA⁺-GO solution; thiourea was added to the LiMoS₂-CTA⁺Transferring the solution to a reaction kettle for reaction at 180 ℃ for 6h, filtering the precipitate, washing the precipitate with deionized water and ethanol for 3 times, and freeze-drying the precipitate for 24h to obtain MoS₂graphene/MoS₂；

2) Preparing the water-based bio-based bactericide: adding carbon nanotubes to a molar concentration of 10^-4Putting the solution into an ultrasonic bath for 20min in a mol/L lysozyme water solution, then putting the solution into an ice bath, performing ultrasonic treatment for 90min, and centrifuging to obtain the carbon nano tube/lysozyme;

3) preparing an oil phase mixed solution: taking lubricant pentaerythritol oleate and polyether (weight ratio is 2:1), emulsifier Tween-80, sodium petroleum sulfonate and span-80 (weight ratio is 6:2:1), oily bactericide BK, BIT-20 and IPBC (weight ratio is 10:5: 1); sequentially adding into base oil, and stirring at 60 deg.C to obtain oil phase mixed solution;

4) preparation of aqueous phase solution: sequentially adding the corrosion-resistant antirust agent triethanolamine sebacate and the water-based bio-based bactericide carbon nano tube/lysozyme into water, and fully dissolving;

5) preparation of an emulsion: adding the water phase solution obtained in the step 4) into the oil phase mixed solution obtained in the step 3), and uniformly stirring;

6) preparation of gum mixture: adding solid additive into MoS with sandwich structure₂graphene/MoS₂Adding the mixture into the emulsion obtained in the step 5), and stirring;

7) homogenizing the colloid mixture obtained in the step 6) in a three-roll ball mill for 2 times to obtain the water-soluble nano wheel belt high-temperature super-lubricant.

Example 3

1) Solid additive sandwich structure MoS₂graphene/MoS₂The preparation of (1): adding molybdenum disulfide into an isopropane solution in isoamyl lithium, and magnetically stirring for 3 hours, wherein the molar weight ratio of the molybdenum disulfide to the isoamyl lithium is 1: 2; stirring the mixture for 5 days under the condition of inert argon atmosphere at room temperature, and dissolving the mixture in isopropyl alcoholWashing with the solvent and drying under reduced pressure to obtain LiMoS₂(ii) a Mixing LiMoS₂Adding into deionized water, and performing ultrasonic treatment for 3h to obtain layered LiMoS₂(ii) a CTAB is completely dissolved into deionized water (the mass ratio of CTAB to deionized water is 1:5), and LiMoS is stripped from the layer₂Mixing thoroughly and sonicating for 2h to form exfoliated LiMoS₂-CTA⁺A solution; to the above LiMoS₂-CTA⁺Adding a dispersion solution of Graphene Oxide (GO) into the solution, and continuing to perform ultrasonic treatment for 2 hours to form LiMoS₂-CTA⁺-GO solution; sodium borohydride was added to the LiMoS₂-CTA⁺Transferring the solution to a reaction kettle for reaction at 180 ℃ for 6h, filtering the precipitate, washing the precipitate with deionized water and ethanol for 3 times, and freeze-drying the precipitate for 24h to obtain MoS₂graphene/MoS₂；

2) Preparing the water-based bio-based bactericide: adding carbon nanotubes to a molar concentration of 10^-3Putting the solution into an ultrasonic bath for 20min in a mol/L lysozyme water solution, then putting the solution into an ice bath, performing ultrasonic treatment for 90min, and centrifuging to obtain the carbon nano tube/lysozyme;

3) preparing an oil phase mixed solution: taking lubricant pentaerythritol oleate and polyether (weight ratio is 4:1), emulsifier Tween-80, sodium petroleum sulfonate and span-80 (weight ratio is 3:1:1), oily bactericide BK, BIT-20 and IPBC (weight ratio is 10:8: 1); sequentially adding into base oil, and stirring at 60 deg.C to obtain oil phase mixed solution;

4) preparation of aqueous phase solution: adding the anti-corrosion antirust agent benzotriazole and the aqueous bio-based bactericide carbon nano tube/lysozyme into water in sequence, and fully dissolving;

5) preparation of an emulsion: adding the water phase solution obtained in the step 4) into the oil phase mixed solution obtained in the step 3), and uniformly stirring;

6) preparation of gum mixture: adding solid additive into MoS with sandwich structure₂graphene/MoS₂Adding the mixture into the emulsion obtained in the step 5), and stirring;

7) homogenizing the colloid mixture obtained in the step 6) in a three-roll ball mill for 3 times to obtain the water-soluble nano wheel belt high-temperature super-lubricant.

TABLE 1 Bactericidal Properties of Water-soluble nanometer wheel-band high-temperature super-lubricant

Sample (I)	Colibacillus killing rate	Staphylococcus aureus killing rate	Candida albicans killing rate
				Example 1	99.9％	99.9％	99.9％
Example 2	99.9％	99.9％	99.9％
				Example 3	99.9％	99.9％	99.9％

TABLE 2 Performance test results of water-soluble nanowheel high-temperature super-lubricants