CN111876220A - Chemical-medium-resistant fluorine-silicon lubricating grease and preparation method thereof - Google Patents
Chemical-medium-resistant fluorine-silicon lubricating grease and preparation method thereof Download PDFInfo
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- CN111876220A CN111876220A CN202010773890.5A CN202010773890A CN111876220A CN 111876220 A CN111876220 A CN 111876220A CN 202010773890 A CN202010773890 A CN 202010773890A CN 111876220 A CN111876220 A CN 111876220A
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M177/00—Special methods of preparation of lubricating compositions; Chemical modification by after-treatment of components or of the whole of a lubricating composition, not covered by other classes
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/06—Metal compounds
- C10M2201/062—Oxides; Hydroxides; Carbonates or bicarbonates
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/10—Compounds containing silicon
- C10M2201/105—Silica
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
- C10M2209/10—Macromolecular compoundss obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- C10M2209/103—Polyethers, i.e. containing di- or higher polyoxyalkylene groups
- C10M2209/1033—Polyethers, i.e. containing di- or higher polyoxyalkylene groups used as base material
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
- C10M2209/10—Macromolecular compoundss obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- C10M2209/103—Polyethers, i.e. containing di- or higher polyoxyalkylene groups
- C10M2209/105—Polyethers, i.e. containing di- or higher polyoxyalkylene groups of alkylene oxides containing three carbon atoms only
- C10M2209/1055—Polyethers, i.e. containing di- or higher polyoxyalkylene groups of alkylene oxides containing three carbon atoms only used as base material
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
- C10M2209/10—Macromolecular compoundss obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- C10M2209/103—Polyethers, i.e. containing di- or higher polyoxyalkylene groups
- C10M2209/108—Polyethers, i.e. containing di- or higher polyoxyalkylene groups etherified
- C10M2209/1085—Polyethers, i.e. containing di- or higher polyoxyalkylene groups etherified used as base material
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2211/00—Organic non-macromolecular compounds containing halogen as ingredients in lubricant compositions
- C10M2211/02—Organic non-macromolecular compounds containing halogen as ingredients in lubricant compositions containing carbon, hydrogen and halogen only
- C10M2211/022—Organic non-macromolecular compounds containing halogen as ingredients in lubricant compositions containing carbon, hydrogen and halogen only aliphatic
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2213/00—Organic macromolecular compounds containing halogen as ingredients in lubricant compositions
- C10M2213/06—Perfluoro polymers
- C10M2213/0613—Perfluoro polymers used as thickening agents
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2213/00—Organic macromolecular compounds containing halogen as ingredients in lubricant compositions
- C10M2213/06—Perfluoro polymers
- C10M2213/062—Polytetrafluoroethylene [PTFE]
- C10M2213/0626—Polytetrafluoroethylene [PTFE] used as thickening agents
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2229/00—Organic macromolecular compounds containing atoms of elements not provided for in groups C10M2205/00, C10M2209/00, C10M2213/00, C10M2217/00, C10M2221/00 or C10M2225/00 as ingredients in lubricant compositions
- C10M2229/04—Siloxanes with specific structure
- C10M2229/041—Siloxanes with specific structure containing aliphatic substituents
- C10M2229/0415—Siloxanes with specific structure containing aliphatic substituents used as base material
Abstract
The invention provides a fluorine-silicon lubricating grease resistant to a chemical medium and a preparation method thereof. The fluorine-silicon lubricating grease comprises the following components in percentage by weight: compound fluorine-containing base oil: 60-80 wt%; a thickening agent: 10 to 35 wt%; high-temperature performance improver: 1-15 wt%; the composite base oil comprises fluorosilicone oil and linear perfluoropolyether oil. The fluorosilicone lubricating grease provided by the invention has excellent chemical medium resistance and high temperature resistance, can be used under extremely harsh working conditions of over 220 ℃, strong chemically active medium and the like, can effectively reduce friction, protects normal operation of equipment, and thus prolongs the service life of the equipment.
Description
Technical Field
The invention belongs to the technical field of lubricating materials, and particularly relates to a chemical-medium-resistant fluorosilicone lubricating grease and a preparation method thereof.
Background
With the continuous change of modern industrial technology, the rapid development of industrial technical fields such as petrochemical industry, automobile industry, gas processing industry and the like is promoted, and meanwhile, the types of related mechanical products in the industrial fields are more and more complicated, and the use working conditions are more and more severe. The requirements for the performance of lubricating grease are continuously increased due to the updating and upgrading of mechanical equipment, the requirements for the performance of lubricating grease products are increasingly strict particularly due to the mechanical equipment used under some complex working conditions, and the factors are power for accelerating the continuous development and upgrading of the lubricating grease industrial technology.
Fluorosilicone oil is widely used in the lubrication field because of its good chemical stability, lubricity and chemical stability. Fluorosilicones, which are composed of fluorosilicones and a thickener (such as fumed silica), have good metal corrosion resistance and water resistance, and are therefore commonly used for lubricating rubber and metal parts.
CN104862029A discloses a fluorosilicone grease composition, which is composed of fluorosilicone oil and fumed silica, and can effectively solve the technical problem existing in the lubrication between rubber seals and metals in oil production equipment. The fluorosilicone grease composition can improve the oil change period of a lubricating part by 3-5 times, improve the replacement period of a nitrile rubber sealing element by 2 times, but the hardness of fumed silica basic particles is high, the lubricating performance is poor, and if all the thickening agents use fumed silica, abrasive particles are easily formed on a friction metal interface and generate abrasive particle abrasion, so that the abrasion among devices is aggravated, and the service life of equipment is shortened.
CN102676285A discloses a perfluoro high-temperature lubricating grease which can be used for long-term lubrication protection in a high-temperature environment of more than 300 ℃, can also work under severe working conditions of high pressure, high vacuum, high load, strong acid and alkali, strong corrosion and the like, and has excellent chemical medium resistance and high temperature resistance. However, additives in the formula of the lubricating grease, such as phosphorus cyanide, sodium sebacate and sodium suberate, corrode rubber parts, obviously damage the rubber parts in the long-term lubrication process, and further influence the service life of the rubber parts.
US5356549 discloses high and low temperature resistant fluorosilicone grease, which adopts amino modified silicone oil as base oil, wherein the base oil has an application temperature range of-50-200 ℃, and the heat resistance of the fluorosilicone grease is effectively improved.
At present, common commercial chemical-resistant medium lubricating grease in the market is mostly prepared by mechanically mixing modified silicone oil (namely methyl silicone oil, phenyl silicone oil and fluorosilicone oil) and fumed silica (commonly called white carbon black) and other ingredients, and the traditional silicone grease has good high and low temperature resistance, viscosity-temperature performance and lubricating effect within a bearable temperature change range. When the traditional fluorine silicone grease is used at some special environmental temperatures, the problems of insufficient oil resistance, solvent resistance, high temperature resistance and the like are caused, so that the performances of lubrication protection and the like are obviously reduced, and especially, the traditional fluorine silicone grease can be obviously aged due to aggravation of oxidation reaction when the traditional fluorine silicone grease is operated for a long time under the working condition of more than 220 ℃, so that the limitation of the traditional fluorine silicone grease in the aspect of high and low temperature resistance is more and more obvious along with the development of material science and mechanical process. Perfluoropolyether oil has the characteristics of excellent chemical stability, thermal stability, compatibility and the like due to high fluorine content and stable molecular structure. By combining the defects of the prior fluorosilicone grease and the characteristics of perfluoropolyether oil, the chemical-medium-resistant high-temperature-resistant fluorosilicone grease is particularly developed.
Disclosure of Invention
The invention provides a chemical medium resistant fluorosilicone grease and a preparation method thereof, which are used for overcoming the defects in the prior art. The fluorosilicone lubricating grease provided by the invention has excellent chemical medium resistance and high temperature resistance, can be used under extremely harsh working conditions of over 220 ℃, strong chemically active medium and the like, can effectively reduce friction, protects normal operation of equipment, and thus prolongs the service life of the equipment.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a chemical medium resistant fluorine-silicon lubricating grease which comprises the following components in percentage by weight:
compound base oil: 60-80 wt%;
a thickening agent: 10 to 35 wt%;
high-temperature performance improver: 1-15 wt%;
the composite base oil comprises fluorosilicone oil and linear typeThe linear perfluoropolyether oil accounts for 5-15 wt% of the composite base oil, and the balance is fluorosilicone oil; the molecular structure of the linear perfluoropolyether oil is as follows: CF (compact flash)3-O-(-(CF3)CFCF2-O-)p-(-CF2-O-)q-CF3(p/q is 20-40); the fluorosilicone oil has the following structure: wherein n is an integer of 20 to 70,
in a preferred embodiment of the present invention, the fluorosilicone grease comprises the following components in percentage by weight:
compound fluorine-containing base oil: 68-78 wt%;
a thickening agent: 12-26 wt%;
high-temperature performance improver: 2 to 10 wt%.
Further preferably, the fluorosilicone grease comprises the following components in percentage by weight:
compound fluorine-containing base oil: 70-75 wt%;
a thickening agent: 23-25 wt%;
high-temperature performance improver: 5 to 7 wt%.
In the invention, the average molecular weight of the linear perfluoropolyether oil is 1000-6000, preferably 2000-4000.
In the invention, the kinematic viscosity of the fluorosilicone oil at 25 ℃ is 3000mm2/s～10000mm2S, preferably 8000mm2/s～10000mm2/s。
In the invention, the thickening agent is one or more of polytetrafluoroethylene, tetrafluoroethylene-hexafluoropropylene copolymer, chlorotrifluoroethylene-polyethylene copolymer and polyurea.
In the invention, the high-temperature performance improver is one or more of chlorotrifluoroethylene telomere, silicon dioxide, molybdenum disulfide and silicate.
The invention also provides a preparation method of the fluorosilicone grease, which comprises the following steps:
1) firstly, mixing fluorosilicone oil and linear perfluoropolyether oil according to the proportion, and mechanically stirring for 0.5-2 hours at 35-50 ℃ to obtain uniform composite fluorine-containing base oil;
2) blending the composite fluorine-containing base oil obtained in the step 1) with a thickening agent and a high-temperature performance improver, and then heating to 50-110 ℃ and stirring for 0.5-3 h to obtain a blend;
3) cooling the blend obtained in the step 2) to room temperature, and grinding to obtain the finished lubricating grease in a smooth grease state.
In a specific embodiment of the present invention, the preparation method of the fluorosilicone grease may further include the following steps:
1) firstly, mixing fluorosilicone oil and linear perfluoropolyether oil according to the proportion, and mechanically stirring for 0.5-2 hours at 35-50 ℃ to obtain uniform composite fluorine-containing base oil;
2) heating the composite fluorine-containing base oil obtained in the step 1) to 50-60 ℃, keeping the temperature for 20-60min, adding a thickening agent, stirring for 1-2 h, cooling to room temperature, adding a high-temperature performance improver, and stirring for 20-120 min to obtain a blend;
3) milling the blend obtained in step 2) to obtain a finished grease in the form of a smooth grease.
In the preparation method, in the step 1), mechanical stirring is preferably carried out for 1-1.5 hours at the temperature of 40-45 ℃; in step 2), heating to 60-100 ℃ is preferred. In the step 3), the grinding is preferably performed for 2-6 times.
The fluorosilicone oil and linear perfluoropolyether oil can be selected from existing commercially available products, and as an example, commercially available methyl-terminated fluorosilicone oil and linear perfluoropolyether base oil autonomously produced by petrochemical lubricating oil, Inc. can be used.
As used herein, "room temperature" refers to ambient temperature, typically 15-35 ℃.
The technical scheme provided by the invention has the following beneficial effects:
the invention adopts the composite fluorine-containing base oil consisting of the fluorosilicone oil and the linear perfluoropolyether oil, the base oil has a structure similar to an inorganic polymer, the bond energy is larger, and in addition, the shielding protection of a C-F bond in the structure is realized, so the base oil has excellent chemical stability, high temperature resistance and weather resistance; compared with mineral oil, the composite fluorine-containing base oil has wider use temperature, excellent chemical stability, good heat resistance, viscosity-temperature performance, thermal stability and solvent resistance, and the composite fluorine-containing base oil taken as the base oil of the lubricating grease can effectively improve the chemical medium resistance of the lubricating grease and prolong the service life of the lubricating grease under the high-temperature working condition. Compared with pure fluorine silicone oil, the fluorine content of the composite fluorine-containing base oil is higher, so that the composite fluorine-containing base oil has better chemical medium resistance, and in addition, the composite fluorine-containing base oil can form a stable oil film on a friction interface and has better lubricating performance, so that the composite fluorine-containing base oil can perform sufficient lubrication protection on equipment, and meanwhile, the replacement period of lubricating grease can be effectively prolonged, and the service life of the equipment is prolonged; the composite fluorine-containing base oil, the thickening agent and the additive have no corrosivity on metal parts and rubber parts, and cannot damage equipment. The addition of the high-temperature performance improver can well improve the high-temperature performance of the lubricating grease, improve the oxidation stability of the lubricating grease and enlarge the high-temperature use range of the lubricating grease. The lubricating grease has the advantages of simple manufacturing process, fewer influencing factors, capability of obtaining a stable product and contribution to realizing large-scale industrial production.
In conclusion, the fluorosilicone lubricating grease disclosed by the invention has extremely strong chemical inertness and good high and low temperature performances, can resist strong acid and strong alkali under a high-temperature working condition, and keeps excellent lubricity; has long bearing service life and no coking and carbon residue.
Detailed Description
In order to better understand the technical solution of the present invention, the following examples are further provided to illustrate the present invention, but the present invention is not limited to the following examples. The starting materials used in the following examples are all commercially available, unless otherwise specified.
In the embodiment of the invention, methyl-terminated fluorosilicone oil and linear perfluoropolyether base oil independently produced by China petrochemical lubricating oil company Limited are adopted.
The following description of the performance testing methods involved or likely to be involved in the examples is as follows:
| test items | Unit of | Test standard |
| Penetration of cone | mm/10 | GB/T 3498 |
| Dropping point | ℃ | GB/T 269 |
| Load of sintering | N | GB/T 3142 |
| Oil mass (100 ℃, 30h) | ％ | SH/T 0324 |
| Low temperature torque (-40 ℃ C.) | N·m | SH/T0338 |
| Swelling property | ％ | SH/T 0691-2000 |
Example 1
Selecting a 25 ℃ kinematic viscosity of 3000mm2Mixing fluorosilicone oil with per second and linear perfluoropolyether oil with the average molecular weight of 1000-3000 (p is 5-35, q is 0.25-0.87), heating to 35 ℃, and mechanically stirring for 1.5 hours to obtain composite fluorine-containing base oil (6 wt% of linear perfluoropolyether oil and 94 wt% of fluorosilicone oil); adding 60g of composite fluorine-containing base oil into a lubricating grease stirring reaction kettle, heating to 60 ℃, keeping the temperature for 30min, adding a tetrafluoroethylene-hexafluoropropylene copolymer thickening agent with the weight of 22g, and stirring for 1 h; cooling to room temperature of 25 deg.C, adding high temperature performance improver chlorotrifluoroethylene telomere with weight of 6g, and stirring for 30 min; grinding for 3 times by using a grinding device, and then carrying out vacuum degassing post-treatment on the ground lubricating grease to obtain the finished lubricating grease product with the properties shown in the following table 1.
Example 2
Selecting 25 ℃ kinematic viscosity of 5000mm2Mixing fluorosilicone oil with the average molecular weight of 2000-5000, heating to 40 ℃, and mechanically stirring for 1.5 hours to obtain composite fluorine-containing base oil (5 wt% of the linear perfluoropolyether oil and 95 wt% of the fluorosilicone oil); adding 68g of composite fluorine-containing base oil into a lubricating grease stirring reaction kettle, heating to 60 ℃, keeping the temperature for 30min, adding a tetrafluoroethylene-hexafluoropropylene copolymer with the weight of 10g, and stirring for 1 h; cooling to room temperature of 20 ℃, adding high temperature performance improver silicon dioxide with the weight of 9g, and stirring for 30 min; grinding for 2 times by using a grinding device, and then carrying out vacuum degassing post-treatment on the ground lubricating grease, so as to obtain a lubricating grease finished product, and packaging.
Example 3
Selecting kinematic viscosity at 25 ℃ of 10000mm2Mixing fluorosilicone oil with the average molecular weight of 3000-6000 with linear perfluoropolyether oil, heating to 40 ℃, and mechanically stirring for 1.5 hours to obtain composite fluorine-containing base oil (8 wt% of linear perfluoropolyether oil and 92 wt% of fluorosilicone oil); adding 70g of composite fluorine-containing base oil into a lubricating grease stirring reaction kettle, heating to 60 ℃, keeping the temperature for 30min, adding 25g of polytetrafluoroethylene thickening agent in weight ratio, and stirring for 1 h; cooling to room temperature of 30 ℃, adding 5g of high-temperature performance improver molybdenum dioxide, and stirring for 30 min; using grindingGrinding for 2 times by equipment, and then carrying out vacuum degassing post-treatment on the ground lubricating grease, thereby obtaining a lubricating grease finished product and packaging.
Example 4
Adding 7kg of the composite base oil prepared in the example 1 into a lubricating grease stirring reaction kettle, then adding 2.5kg of polytetrafluoroethylene, and finally adding 0.5kg of molybdenum dioxide; heating to 50 ℃, preserving heat for 1h, stirring for 2h, and cooling to room temperature of 25 ℃; and taking out the stirred lubricating grease, putting the lubricating grease into a three-roll grinder to grind for 6 times, thus obtaining a lubricating grease finished product, and packaging.
Example 5
Selecting kinematic viscosity at 25 ℃ of 10000mm2Mixing fluorosilicone oil with the average molecular weight of 2000-4000 and linear perfluoropolyether oil with the average molecular weight of 2000-4000, heating to 50 ℃, and mechanically stirring for 1h to obtain composite base oil (10 wt% of linear perfluoropolyether oil and 90 wt% of fluorosilicone oil); adding 70g of composite oil by weight into a reaction kettle, then adding 22g of polytetrafluoroethylene, and finally adding 3g of modifier silicon dioxide; heating to 110 ℃, preserving heat for 1h, stirring for 2h, and cooling to room temperature; and taking out the stirred lubricating grease, putting the lubricating grease into a three-roll grinder to grind for 3 times, thus obtaining a lubricating grease finished product, and packaging.
Example 6
Selecting kinematic viscosity at 25 ℃ of 10000mm2Mixing fluorosilicone oil with the average molecular weight of 2000-4000 and linear perfluoropolyether oil with the average molecular weight of 2000-4000, heating to 45 ℃, and mechanically stirring for 1h to obtain composite base oil (12 wt% of linear perfluoropolyether oil and 88 wt% of fluorosilicone oil); firstly, adding 75g of composite fluorine-containing base oil in weight ratio into a reaction kettle, then adding 25g of polytetrafluoroethylene in weight ratio, and finally adding 5g of silicon dioxide in weight ratio; heating to 100 ℃, preserving heat for 1h, stirring for 2h, and cooling to room temperature; and taking out the stirred lubricating grease, putting the lubricating grease into a three-roll grinder to grind for 4 times, thus obtaining a lubricating grease finished product, and packaging.
Example 7
Selecting 25 ℃ kinematic viscosity of 8000mm2Mixing fluorosilicone oil with per second and linear perfluoropolyether oil with the average molecular weight of 3000-6000, heating to 40 ℃, and mechanically stirring for 1.5 hours to obtain the compositeA fluorine-containing base oil (15 wt% of a linear perfluoropolyether oil and 85 wt% of a fluorosilicone oil); adding 8kg of composite fluorine-containing base oil into a lubricating grease stirring reaction kettle, heating to 60 ℃, keeping the temperature for 1h, adding 2.9kg of tetrafluoroethylene-hexafluoropropylene copolymer in weight ratio, and stirring for 1 h; cooling to room temperature of 25 ℃, adding 0.2kg of silicon dioxide according to the weight ratio, and stirring for 2 h; and taking out the stirred lubricating grease, grinding for 6 times by using grinding equipment to obtain a lubricating grease finished product, and packaging.
Comparative example 1
Selecting kinematic viscosity at 25 ℃ of 10000mm2Weighing 75g of fluorosilicone oil, adding the fluorosilicone oil into a lubricating grease stirring reaction kettle, heating to 60 ℃, keeping the temperature for 30min, and adding 25g of polytetrafluoroethylene in weight ratio; heating to 100 ℃, preserving heat for 1h, stirring for 2h, and cooling to room temperature; and taking out the stirred lubricating grease, putting the lubricating grease into a three-roll grinder to grind for 4 times, thus obtaining a lubricating grease finished product, and packaging.
Comparative example 2
Selecting fluorosilicone oil with 25 ℃ kinematic viscosity of 10000mm2/s, weighing 75g of the fluorosilicone oil, adding the fluorosilicone oil into a lubricating grease stirring reaction kettle, heating to 60 ℃, keeping the temperature for 30min, adding 25g of polytetrafluoroethylene by weight, and finally adding 5g of silicon dioxide by weight; heating to 100 ℃, preserving heat for 1h, stirring for 2h, and cooling to room temperature; and taking out the stirred lubricating grease, putting the lubricating grease into a three-roll grinder to grind for 4 times, thus obtaining a lubricating grease finished product, and packaging.
The samples obtained in the above examples 1 to 7 and comparative examples 1 and 2 were mounted on a main shaft bearing of a polypropylene horizontal chamber reactor and subjected to a 1000-hour test, and the low-temperature torque, sintering load and other performance indexes were measured. The performance indexes of the products of examples 1 to 7 and comparative examples 1 to 2 are shown in tables 1 and 2.
In the test process, the equipment runs well, does not react with reaction raw materials in the polypropylene horizontal reactor, can effectively resist external active chemical media, does not produce coking and carbon deposit, can effectively protect the equipment and prolong the service life of the equipment.
As shown in tables 1 and 2, according to the analysis of the measured performance indexes, the samples of examples 1-7 have excellent high and low temperature performance, the sintering load is large and can be used for heavy load conditions, the base oil is the composite fluorine-containing base oil consisting of fluorosilicone oil and linear perfluoropolyether oil, the base oil can be used for the work of corrosive media such as strong acid and strong base, and can not react with the polypropylene raw material, the normal operation of the main shaft bearing of the horizontal reactor of the polypropylene can be protected, the reaction with the strong acid and strong base can not occur, the lubricating grease does not react with the rubber sealing element, the swelling performance test index is excellent, the chemical medium resistance performance is strong, and the lubricating grease does not react with the rubber sealing element. And the performance indexes measured by small sample debugging and sample debugging have no obvious difference, so that the lubricant disclosed by the invention can be widely applied to production.
Therefore, the comparison of the sintering load, the working temperature, the reaction condition with strong acid and strong base and other data of the products of the example 6 and the comparative examples 1 and 2 can show that the fluorosilicone grease prepared from the composite fluorine-containing base oil shows more excellent chemical medium resistance and high temperature resistance after the high temperature improver is added. Inventive example 6 performed best.
TABLE 1
TABLE 2
It is obvious that the above-mentioned embodiments of the present invention are only examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention, and that various other modifications and variations can be made by those skilled in the art based on the above description.
Claims (10)
1. A chemical-medium-resistant fluorine-silicon lubricating grease is characterized in that: comprises the following components in percentage by weight:
compound fluorine-containing base oil: 60-80 wt%;
a thickening agent: 10 to 35 wt%;
high-temperature performance improver: 1-15 wt%;
the composite fluorine-containing base oil comprises fluorosilicone oil and linear perfluoropolyether oil, wherein the linear perfluoropolyether oil accounts for 5-15 wt% of the composite base oil, and the balance is fluorosilicone oil; the molecular structure of the linear perfluoropolyether oil is as follows: CF (compact flash)3-O-(-(CF3)CFCF2-O-)p-(-CF2-O-)q-CF3P/q is 20-40; the fluorosilicone oil has the following structure: wherein n is an integer of 20 to 70,
2. the fluorosilicone grease of claim 1, characterized in that: the fluorine-silicon lubricating grease comprises the following components in percentage by weight:
compound fluorine-containing base oil: 68-78 wt%;
a thickening agent: 12-26 wt%;
high-temperature performance improver: 2 to 10 wt%.
3. The fluorosilicone grease of claim 2, characterized in that: the fluorine-silicon lubricating grease comprises the following components in percentage by weight:
compound fluorine-containing base oil: 70-75 wt%;
a thickening agent: 20-25 wt%;
high-temperature performance improver: 5 to 7 wt%.
4. Fluorosilicone grease according to any one of claims 1 to 3, characterized in that: the average molecular weight of the linear perfluoropolyether oil is 1000-10000, preferably 1000-6000.
5. Fluorosilicone grease according to any one of claims 1 to 4, characterized in that: the kinematic viscosity of the fluorosilicone oil at 25 ℃ is 3000mm2/s～10000mm2S, preferably 8000mm2/s～10000mm2/s。
6. Fluorosilicone grease according to any one of claims 1 to 5, characterized in that: the thickening agent is one or more of polytetrafluoroethylene, tetrafluoroethylene-hexafluoropropylene copolymer, chlorotrifluoroethylene-polyethylene copolymer and polyurea.
7. Fluorosilicone grease according to any one of claims 1 to 6, characterized in that: the high-temperature performance improver is one or more of chlorotrifluoroethylene telomer, silicon dioxide, molybdenum disulfide and silicate.
8. The method for preparing fluorosilicone grease according to any one of claims 1 to 7, characterized in that: the method comprises the following steps:
1) firstly, mixing fluorosilicone oil and linear perfluoropolyether oil according to the proportion in claim 1, and mechanically stirring for 0.5-2 hours at 35-50 ℃ to obtain uniform composite fluorine-containing base oil;
2) blending the composite fluorine-containing base oil obtained in the step 1) with a thickening agent and a high-temperature performance improver, and then heating to 50-110 ℃ and stirring for 0.5-3 h to obtain a blend;
3) cooling the blend obtained in the step 2) to room temperature, and grinding to obtain the finished lubricating grease in a smooth grease state.
9. The method for preparing fluorosilicone grease according to any one of claims 1 to 7, characterized in that: the method comprises the following steps:
1) firstly, mixing fluorosilicone oil and linear perfluoropolyether oil according to the proportion in claim 1, and mechanically stirring for 0.5-2 hours at 35-50 ℃ to obtain uniform composite fluorine-containing base oil;
2) heating the composite fluorine-containing base oil obtained in the step 1) to 50-60 ℃, keeping the temperature for 20-60min, adding a thickening agent, stirring for 1-2 h, cooling to room temperature, adding a high-temperature performance improver, and stirring for 20-120 min to obtain a blend;
3) milling the blend obtained in step 2) to obtain a finished grease in the form of a smooth grease.
10. The method for preparing fluorosilicone grease according to claim 8 or 9, characterized in that: in the step 1), preferably, mechanically stirring for 1-1.5 h at 40-45 ℃; and/or, preferably, heating to 60-100 ℃ in step 2); and/or, grinding for 2-6 times at room temperature in the step 3).
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