阅读说明：本技术 一种环保型复合铝基润滑脂及其制备方法 (Environment-friendly composite aluminum-based lubricating grease and preparation method thereof ) 是由 高晓谋 高荣权 何甲生 于 2020-05-12 设计创作，主要内容包括：本发明公开了一种环保型复合铝基润滑脂及其制备方法,该复合铝基润滑脂是以基础油、膨润土润滑脂、铝源、高分子酸与低分子酸作为主要成分,其中基础油是以植物油为原料,通过水解、酯化与环氧化反应,从而消除了脂肪酸醇酯中的大量碳碳双键,进而提升了基础油的氧化安定性,同时在制备过程中,采用离子交换树脂作为催化剂,以植物油作为原料制备基础油,减少了矿物油的使用,同时植物油可降解的性质也大大提升了润滑脂产品的环境友好性,而所述膨润土润滑脂是以有机膨润土与基础油为原料制备而成,大大减少了润滑脂中游离油的含量,从而提升润滑脂的滴点,降低润滑脂的分油率。(The invention discloses an environment-friendly composite aluminum-based lubricating grease and a preparation method thereof, the composite aluminum-based lubricating grease takes base oil, bentonite lubricating grease, an aluminum source, a high molecular acid and a low molecular acid as main components, wherein the base oil takes vegetable oil as a raw material, and a large amount of carbon-carbon double bonds in fatty acid alcohol ester are eliminated through hydrolysis, esterification and epoxidation reactions, so that the oxidation stability of the base oil is improved, meanwhile, in the preparation process, ion exchange resin is adopted as a catalyst, the vegetable oil is adopted as a raw material to prepare the base oil, the use of mineral oil is reduced, meanwhile, the degradable property of the vegetable oil also greatly improves the environment-friendly property of a lubricating grease product, and the bentonite lubricating grease is prepared by taking organic bentonite and the base oil as raw materials, so that the content of free oil in the lubricating grease is greatly reduced, and the dropping point of the lubricating grease is improved, the oil separation rate of the lubricating grease is reduced.)

1. The environment-friendly composite aluminum-based lubricating grease is characterized by being prepared by processing the following raw materials:

base oil, bentonite lubricating grease, an aluminum source, high molecular acid, low molecular acid, a solid lubricant, an extreme pressure antiwear agent, an antioxidant and an antirust agent;

wherein the addition amount of the bentonite grease is 22-32% of the weight of the base oil;

the adding amount of the aluminum source is 12-21% of the weight of the base oil; the mass ratio of the aluminum source to the low molecular acid to the high molecular acid is 1:0.8-1: 0.9-1.1;

the addition amount of the solid lubricant is 0.5-6% of the weight of the base oil;

the addition amount of the extreme pressure antiwear agent is 0.5 to 6 percent of the weight of the base oil;

the addition amount of the antioxidant and the antirust agent is 0.1-1% of the weight of the base oil.

2. The environment-friendly composite aluminum-based grease as claimed in claim 1, wherein the solid lubricant is one or a mixture of at least two of tungsten disulfide, molybdenum disulfide, boron nitride, and polytetrafluoroethylene in any proportion.

3. The environment-friendly composite aluminum-based lubricating grease as claimed in claim 1, wherein the extreme pressure antiwear agent is one or a mixture of at least two of sulfurized isobutylene, dibenzyl disulfide and borate in any proportion.

4. The environment-friendly composite aluminum-based grease as claimed in claim 1, wherein the antioxidant is one of diphenylamine, phenyl-alpha-naphthylamine and organic sulfide antioxidant; the antirust agent is petroleum sodium sulfonate.

5. The preparation method of the environment-friendly composite aluminum-based lubricating grease is characterized by comprising the following steps:

step one, preparing base oil;

heating the vegetable oil to 40-50 ℃, stirring the vegetable oil at the rotating speed of 60-300r/min, then adding a mixed solution of phosphoric acid and sulfuric acid, after the mixed solution of phosphoric acid and sulfuric acid is completely added, raising the reaction temperature to 80-120 ℃, after reacting for 6-12h, raising the temperature to 180-250 ℃, introducing inert gas under the condition of reduced pressure, and condensing and recovering a product carried by the inert gas to obtain mixed fatty acid; in the first step, the mass concentration of phosphoric acid is 65-70%, the mass concentration of sulfuric acid is 60%, and the volume ratio of phosphoric acid solution to sulfuric acid solution is 1: 2;

adding polyalcohol and a catalyst into mixed fatty acid, reacting for 8-14h at 60-120 ℃ to obtain mixed fatty acid alcohol ester, adding ion exchange resin and a peroxyacetic acid aqueous solution with the mass concentration of 20% -35% into the mixed fatty acid alcohol ester, adjusting the reaction temperature to 45-80 ℃, reacting for 6-10h, standing and layering reaction products, and taking an upper layer product to obtain epoxy fatty acid polyalcohol ester, namely base oil;

adding organic bentonite into base oil, adding glycerol as a dispersing agent into the base oil, carrying out ultrasonic treatment for 5-15min, adjusting the stirring speed to 2000-4000r/min, carrying out high-speed mixing and stirring for 15-50min, wherein the mass ratio of the organic bentonite to the base oil is 3:6.5-7, adjusting the temperature to 150-180 ℃, and carrying out heat preservation and stirring for 30-60min to obtain bentonite lubricating grease;

step three, weighing base oil with the total dosage of 1/3, adding the base oil into a container, heating to 105-120 ℃, adding an aluminum source into the container, carrying out heat preservation and stirring reaction until the aluminum source is completely dissolved, then adding high molecular acid and low molecular acid into the mixture, carrying out heat preservation and stirring reaction for 30-60min, and carrying out saponification reaction;

step four, adding deionized water into the reaction vessel, wherein the water addition amount is 25-40% of the weight of the aluminum source, adjusting the reaction temperature to 105 ℃, stirring for reaction for 30-60min, then raising the temperature to 120 ℃, stirring for dehydration to completely remove the water in the base oil, then adding the base oil with the total amount of 1/3 into the reaction vessel, stirring and mixing uniformly, raising the temperature to 160-180 ℃, reacting for 20-30min for thickening, finally raising the temperature to 200-220 ℃, and refining at high temperature for 15-30 min;

step five, adding the residual base oil with the total amount of 1/3 into the product obtained in the step one, stirring and mixing uniformly, adding the bentonite lubricating grease obtained in the step two, adjusting the temperature to 90-105 ℃, stirring and mixing uniformly, and cooling;

and step six, grinding and degassing the reaction product obtained in the step one to obtain the composite aluminum-based lubricating grease.

6. The method for preparing the environment-friendly composite aluminum-based grease as claimed in claim 5, wherein in the first step, the polyol comprises one of neopentyl glycol and pentaerythritol; the ion exchange resin is one of strong acid styrene cation exchange resin and perfluorinated sulfonic acid ion exchange resin, and the addition amount of the ion exchange resin is 5-10% of the weight of the mixed fatty acid alcohol ester.

7. The method for preparing the environment-friendly composite aluminum-based grease as claimed in claim 5, wherein in step three, the polymeric acid is one or a mixture of at least two of stearic acid, lauric acid, palmitic acid and 12-hydroxystearic acid; the low molecular acid is one or a mixture of at least two of benzoic acid, sebacic acid, azelaic acid and phthalic acid, and the aluminum source is aluminum isopropoxide.

8. The method for preparing the environment-friendly composite aluminum-based lubricating grease as claimed in claim 5, wherein the method for preparing the organic bentonite comprises the following steps:

adding bentonite into deionized water, performing ultrasonic soaking treatment, filtering after cleaning to obtain a filter cake, dispersing the filter cake in the deionized water, adding sodium chloride or sodium carbonate into the deionized water, raising the reaction temperature to 60-90 ℃, completing sodium treatment on the bentonite, replacing calcium ions in the bentonite by sodium ions, filtering to obtain a filter cake, flushing the filter cake for 2-5 times by the deionized water, and finally drying and crushing to obtain sodium bentonite;

adding sodium bentonite into deionized water, stirring and dispersing uniformly, adding quaternary ammonium salt, stirring and reacting at 70-80 ℃ for 3-5h, filtering, washing the obtained filter cake with deionized water for 2-5 times, drying, and grinding until the particle size is less than 150 mu m to obtain the organic bentonite for later use.

9. The method for preparing the environment-friendly composite aluminum-based lubricating grease as claimed in claim 8, wherein the quaternary ammonium salt is cetyl trimethyl ammonium bromide.

Technical Field

The invention belongs to the technical field of lubricants, and particularly relates to environment-friendly composite aluminum-based lubricating grease and a preparation method thereof.

Background

The lubricating grease is an indispensable lubricating agent for the operation of various machines, has better bearing capacity, dust-proof and moisture-proof performance, adhesion capacity and lower evaporation speed, and along with the rapid development of the industries such as machinery, metallurgy, chemical engineering, transportation and the like, the number of devices which operate in special environments such as high temperature, underwater and the like is gradually increased, so that the requirements of people on the lubricating grease are directly improved.

In order to ensure the performance of the composite aluminum-based lubricating grease, synthetic oil and mineral oil are mostly adopted as base oil to be processed in the process of preparing the composite aluminum-based lubricating grease, but the synthetic oil and the mineral oil have non-degradable property and cause environmental pollution when being used in large quantity, and vegetable oil or animal oil is adopted as a base oil raw material, although the problem can be solved, other performances of the composite aluminum-based lubricating grease can be influenced, so that the other performances of the composite aluminum-based lubricating grease can not be reduced when the composite aluminum-based lubricating grease is produced by adopting the animal and vegetable oil as the raw material, and the application range of the composite aluminum-based lubricating grease is widened.

Disclosure of Invention

The invention aims to provide environment-friendly composite aluminum-based lubricating grease and a preparation method thereof.

The technical problems to be solved by the invention are as follows:

in the process of preparing the composite aluminum-based lubricating grease, synthetic oil and mineral oil are mostly adopted as base oil for processing, but the synthetic oil and the mineral oil have non-degradable property, and can pollute the environment when being used in large quantities, and vegetable oil or animal oil is adopted as a base oil raw material, which can solve the problem, but can also influence other properties of the composite aluminum-based lubricating grease.

The purpose of the invention can be realized by the following technical scheme:

the environment-friendly composite aluminum-based lubricating grease is prepared by processing the following raw materials:

base oil, bentonite lubricating grease, an aluminum source, high molecular acid, low molecular acid, a solid lubricant, an extreme pressure antiwear agent, an antioxidant and an antirust agent;

wherein the addition amount of the bentonite grease is 22-32% of the weight of the base oil;

the adding amount of the aluminum source is 12-21% of the weight of the base oil; the mass ratio of the aluminum source to the low molecular acid to the high molecular acid is 1:0.8-1: 0.9-1.1;

the addition amount of the solid lubricant is 0.5-6% of the weight of the base oil;

the addition amount of the extreme pressure antiwear agent is 0.5 to 6 percent of the weight of the base oil;

the addition amount of the antioxidant and the antirust agent is 0.1-1% of the weight of the base oil;

the solid lubricant is one or a mixture of at least two of tungsten disulfide, molybdenum disulfide, boron nitride and polytetrafluoroethylene in any proportion;

the extreme pressure antiwear agent is one or a mixture of at least two of sulfurized isobutylene, dibenzyl disulfide and borate in any proportion;

the antioxidant is one of diphenylamine, phenyl-alpha-naphthylamine and an organic sulfide antioxidant;

the antirust agent is petroleum sodium sulfonate;

the preparation method of the environment-friendly composite aluminum-based lubricating grease comprises the following steps:

step one, preparing base oil;

heating the vegetable oil to 40-50 ℃, stirring the vegetable oil at the rotating speed of 60-300r/min, then adding a mixed solution of phosphoric acid and sulfuric acid, after the mixed solution of phosphoric acid and sulfuric acid is completely added, raising the reaction temperature to 80-120 ℃, after reacting for 6-12h, raising the temperature to 180-250 ℃, introducing inert gas under the condition of reduced pressure, and condensing and recovering a product carried by the inert gas to obtain mixed fatty acid; in the first step, the mass concentration of phosphoric acid is 65-70%, the mass concentration of sulfuric acid is 60%, and the volume ratio of phosphoric acid solution to sulfuric acid solution is 1: 2;

adding polyalcohol and a catalyst into mixed fatty acid, reacting for 8-14h at 60-120 ℃ to obtain mixed fatty acid alcohol ester, adding ion exchange resin and a peroxyacetic acid aqueous solution with the mass concentration of 20% -35% into the mixed fatty acid alcohol ester, adjusting the reaction temperature to 45-80 ℃, reacting for 6-10h, standing and layering reaction products, and taking an upper layer product to obtain epoxy fatty acid polyalcohol ester, namely base oil;

the polyol comprises one of neopentyl glycol and pentaerythritol;

the ion exchange resin is one of strong acid styrene cation exchange resin and perfluorinated sulfonic acid ion exchange resin, the addition amount of the ion exchange resin is 5-10% of the weight of the mixed fatty acid alcohol ester,

in the step, firstly, mixed solution of phosphoric acid and sulfuric acid is used for hydrolyzing vegetable oil to obtain fatty acid, then esterification reaction is carried out on added polyalcohol and fatty acid to obtain fatty acid alcohol ester, and finally catalyst and epoxidation reagent are added to enable fatty acid alcohol ester to carry out epoxidation reaction, so that a large number of carbon-carbon double bonds in the fatty acid alcohol ester are eliminated, and further oxidation stability of base oil is improved.

Adding organic bentonite into base oil, adding glycerol as a dispersing agent into the base oil, carrying out ultrasonic treatment for 5-15min, adjusting the stirring speed to 2000-4000r/min, carrying out high-speed mixing and stirring for 15-50min, wherein the mass ratio of the organic bentonite to the base oil is 3:6.5-7, adjusting the temperature to 150-180 ℃, and carrying out heat preservation and stirring for 30-60min to obtain bentonite lubricating grease;

in the step, the distance between the bentonite sheets is increased through ultrasonic and mechanical stirring, the base oil is accelerated to permeate between the bentonite sheets, and the glycerol is added as a dispersing agent, so that the distance between the bentonite sheets can be increased, and the distance between the bentonite sheets can be increased. The glycerol can enable the bentonite particles to form hydrogen bonds, so that the stability of the lubricating grease is improved;

step three, weighing base oil with the total dosage of 1/3, adding the base oil into a container, heating to 105-120 ℃, adding an aluminum source into the container, carrying out heat preservation and stirring reaction until the aluminum source is completely dissolved, then adding high molecular acid and low molecular acid into the mixture, carrying out heat preservation and stirring reaction for 30-60min, and carrying out saponification reaction;

the high molecular acid is one or a mixture of at least two of stearic acid, lauric acid, palmitic acid and 12-hydroxystearic acid; the low molecular acid is one or a mixture of at least two of benzoic acid, sebacic acid, azelaic acid and phthalic acid, and the aluminum source is aluminum isopropoxide;

step four, adding a certain amount of water into the reaction vessel, wherein the added water amount is 25-40% of the weight of the aluminum source, adjusting the reaction temperature to 105 ℃ and carrying out stirring reaction for 30-60min, in the step, an intermediate product generated by the reaction of the aluminum source and the organic acid and water are subjected to hydrolysis reaction to discharge isopropanol, then raising the temperature to 120 ℃, carrying out stirring dehydration to completely remove the water in the base oil, then adding the total amount of 1/3 base oil into the base oil, uniformly stirring and mixing, raising the temperature to 180 ℃ after stirring, carrying out reaction for 20-30min to carry out thickening, finally raising the temperature to 220 ℃ after stirring, and carrying out high-temperature refining for 15-30 min;

step five, adding the residual base oil with the total amount of 1/3 into the product obtained in the step one, stirring and mixing uniformly, adding the bentonite lubricating grease obtained in the step two, adjusting the temperature to 90-105 ℃, stirring and mixing uniformly, cooling,

and step six, grinding and degassing the reaction product in the last step to obtain the composite aluminum-based lubricating grease, specifically, adding the product in the last step into a four-roller machine to grind for 2-4 times, and carrying out vacuum degassing on the ground product to obtain the composite aluminum-based lubricating grease.

Through adding bentonite lubricating grease and carrying out the homogeneous mixing in to the base oil, the hydrogen bonding between the bentonite has promoted the effort between bentonite and the composite soap fibre, can show to promote the dropping point that has promoted lubricating grease.

The preparation method of the organic bentonite comprises the following steps:

adding bentonite into deionized water, carrying out ultrasonic soaking treatment, specifically, carrying out ultrasonic soaking for 3-10min for one time, changing water for 2-5 times, filtering to obtain a filter cake after cleaning, dispersing the filter cake in the deionized water, adding sodium chloride or sodium carbonate into the deionized water, raising the reaction temperature to 60-90 ℃, completing sodium treatment on the bentonite, replacing calcium ions in the bentonite by the sodium ions, filtering to obtain a filter cake, washing the filter cake for 2-5 times by the deionized water, and finally drying and crushing to obtain sodium bentonite;

adding sodium bentonite into deionized water, stirring and dispersing uniformly, adding quaternary ammonium salt, stirring and reacting at 70-80 ℃ for 3-5h, filtering, washing the obtained filter cake with deionized water for 2-5 times, drying, and grinding until the granularity is less than 150 mu m to obtain organic bentonite for later use;

in one embodiment of the invention, the quaternary ammonium salt is cetyltrimethylammonium bromide;

quaternary ammonium salt is the polar molecule in the bentonite lubricating grease, and can produce certain electrostatic action between the base oil, thereby promote the combining ability between bentonite and the base oil, simultaneously because contain the organic functional group of long chain oleophylic in the lamellar structure of bentonite, thereby make between the lamella that the base oil can permeate the bentonite, and have good adsorption effect between bentonite and the base oil, free oil's content in the lubricating grease has also significantly reduced to this kind of adsorption effect, thereby promote the dropping point of lubricating grease, and simultaneously, carry out homogeneous mixing with organophilic bentonite and aluminium base lubricating grease, the hydrogen bonding between the bentonite has promoted the effort between bentonite and the composite soap fibre, further promoted the dropping point of lubricating grease.

The invention has the beneficial effects that:

the composite aluminum-based lubricating grease of the invention takes base oil, bentonite lubricating grease, an aluminum source, high molecular acid and low molecular acid as main components, wherein the base oil takes vegetable oil as raw material, firstly, the vegetable oil is hydrolyzed by mixed solution of phosphoric acid and sulfuric acid to obtain fatty acid, then, the added polyalcohol and the fatty acid are subjected to esterification reaction to obtain fatty acid alcohol ester, and finally, the fatty acid alcohol ester is subjected to epoxidation reaction by adding a catalyst and an epoxidation reagent, thereby eliminating a large amount of carbon-carbon double bonds in the fatty acid alcohol ester, further improving the oxidation stability of the base oil, meanwhile, in the preparation process, ion exchange resin is adopted as the catalyst, on one hand, the product can be recycled, on the other hand, compared with the traditional concentrated sulfuric acid catalyst, the obtained product has lighter color, and the vegetable oil is taken as the raw material to prepare the base oil, the use of mineral oil is reduced, meanwhile, the environment friendliness of a lubricating grease product is greatly improved due to the degradable property of vegetable oil, the bentonite lubricating grease is prepared by taking organic bentonite and base oil as raw materials, wherein quaternary ammonium salt in the organic bentonite lubricating grease is a polar molecule and can generate a certain electrostatic action with the base oil, so that the binding capacity between the bentonite and the base oil is improved, meanwhile, as long-chain oleophylic organic functional groups are contained in a lamellar structure of the bentonite, the base oil can permeate into lamella of the bentonite, and the bentonite and the base oil have good adsorption effect, the content of free oil in the lubricating grease is greatly reduced due to the adsorption effect, so that the dropping point of the lubricating grease is improved, meanwhile, the organic bentonite and the aluminum-based lubricating grease are uniformly mixed, and the acting force between the bentonite and composite soap fibers is improved due to the hydrogen bond action between the bentonite and the composite soap fibers, further promoted the dropping point of lubricating grease, and through adding bentonite lubricating grease and misce bene in to the base oil, the hydrogen bond effect between the bentonite has promoted the effort between bentonite and the compound soap fibre, can show the dropping point that promotes lubricating grease, reduces the oil separation rate of lubricating grease.

Detailed Description

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