A sealing protective grease for high temperature and high vacuum

Abstract

The present invention relates to a sealing protective grease for high temperature and high vacuum, the sealing protective grease comprising the following raw materials by weight: 60-85% perfluoropolyether oil (PFPE), 12-30% solid filler, and 3-10% stabilizer. The present invention relates to a sealing protective grease for high temperature and high vacuum conditions, which has excellent chemical inertness resistance, low temperature resistance and high temperature resistance, and extremely low volatility, and can meet the requirements of bearing and pump valve sealing under high temperature and high vacuum conditions, and can achieve the characteristics of no leakage and no loss, and can meet the sealing protection requirements of equipment under high temperature 200°C and vacuum conditions.

Description

Technical Field

[0001] The invention relates to the technical field of lubricating grease, and in particular to a sealing and protective lubricating grease used for high temperature and high vacuum. Background Art

[0002] At present, with the development of chip semiconductors, the popularization of automation equipment, and the growth rate of the semiconductor equipment market, in addition to the main lithography machines, etchers, and thin film deposition equipment as the main core equipment of semiconductor equipment, the automated production transportation and baking also involve the lubrication and sealing of screw rods, guide rails, sliders, sealing boxes, bearings, pumps, valves, and sealing rings of high vacuum environment equipment. At the same time, there are pumps and valves that are in contact with corrosive gases and liquids (such as halogens, liquid oxygen, etc.) in the production process. This kind of production environment requires equipment grease, high temperature resistance, high load, chemical corrosion environment bearings and parts requiring lifelong lubrication. Bearings, pumps and valves with sealing requirements need to have excellent chemical inertness, durability and low volatility grease to meet their requirements.

[0003] With the development of the times and the advancement of science and technology, more and more products are produced under high temperature and high vacuum conditions. At the same time, the requirements for lubrication protection of the environment and equipment are getting higher and higher. The requirements for bearing seals and pump valves are also higher, and higher sealing grease is needed to protect the operation of the equipment. At present, the commonly used sealing greases on the market are mostly high-viscosity silicone oil products, polybutene polymers, high-viscosity hydrocarbon-based greases, etc. Their characteristics can meet the general sealing environment requirements of normal temperature and pressure, no acid and alkali corrosion, etc., but they can no longer meet their application requirements under high temperature and high vacuum working conditions.

[0004] The existing sealing protective grease has poor volatile memory loss and permeability performance. In addition, the requirements for pump and valve sealing to achieve no leakage and no loss have poor performance, which limits the efficiency of product use. Summary of the invention

[0005] In view of the defects of the prior art, the object of the present invention is to provide a sealing and protective grease for high temperature and high vacuum to solve the problems raised in the above background technology.

[0006] The present invention solves the technical problem by adopting the following technical solution:

[0007] The present invention provides a sealing protective lubricating grease for high temperature and high vacuum, wherein the sealing protective lubricating grease comprises the following raw materials in parts by weight:

[0008] Perfluoropolyether oil (PFPE): 60-85%

[0009] Solid filler: 12-30%

[0010] Stabilizer: 3~10%.

[0011] Preferably, the

[0012] The solid filler is one or more combinations of polytetrafluoroethylene (PTFE), melamine cyanurate, fumed silica, zinc oxide and bentonite.

[0013] Preferably, the stabilizer is one or more combinations of polyethylene glycol, perfluoroacetic acid, ethanol, carbonated acrylic acid, and perfluororesin.

[0014] Preferably, the viscosity range of the perfluoropolyether (PFPE) is 1750 to 1900 mm2 / s at 20°C.

[0015] Preferably, the fumed silicon oxide is also subjected to a blending treatment;

[0016] The specific reconciliation method is:

[0017] 3-6 parts of flaky talc, 1-3 parts of nano-silica sol, 5-8 parts of sodium dodecylbenzene sulfonate solution and 1-2 parts of yttrium oxide are mixed and stirred thoroughly, and then filtered and dried to obtain modified flaky talc;

[0018] First immerse 5-8 parts of fumed silicon oxide into 6-10 parts of lanthanum nitrate solution, then add 2-3 parts of silane coupling agent KH550 and 1-3 parts of modified flaky talcum powder, and then perform ultrasonic treatment. After the ultrasonic treatment is completed, filter and dry.

[0019] Preferably, the mass fraction of the sodium dodecylbenzene sulfonate solution is 2-5%.

[0020] Preferably, the mass fraction of the lanthanum nitrate solution is 5-8%.

[0021] Preferably, the ultrasonic power of the ultrasonic treatment is 350-400W, and the ultrasonic time is 20-30min.

[0022] A preparation method of a sealing protective grease for high temperature and high vacuum comprises the following steps: mixing perfluoropolyether oil (PFPE) and a solid filler uniformly at a rotation speed of 46 rpm for 10-15 min, adding a stabilizer for dispersion and stirring for 10-15 min, heating to 100-110° C., keeping the temperature constant for 0.5-1 h, pouring out and cooling, grinding with a three-roller for 2-3 times to homogenize the grease, and after homogenization, degassing with a high vacuum disperser at 0.8 Mpa and a rotation speed of 295 rpm to obtain a finished product.

[0023] Through TGA detection and analysis of the example and the comparative example, it is found that the starting temperature of the example at high temperature and large-scale volatilization is 60°C higher than the starting temperature of the comparative example at high temperature and large-scale volatilization. This further illustrates that under the conditions of high temperature and high pressure, its volatility, leakage and loss performance can better meet the use of sealing protection.

[0024] Compared with the prior art, the present invention has the following beneficial effects:

[0025] The present invention provides a sealing protective grease for high-temperature and high-vacuum conditions. The sealing protective grease has excellent chemical inertness resistance, low-temperature resistance and high-temperature resistance, and extremely low volatility. It can meet the requirements of bearing and pump valve sealing under high-temperature and high-vacuum conditions, and can achieve the characteristics of no leakage and no loss. It can meet the sealing protection requirements of equipment under high temperature 200°C and vacuum conditions. BRIEF DESCRIPTION OF THE DRAWINGS

[0026] Figure 1 It is the TGA detection diagram of Example 1;

[0027] Figure 2 It is the TGA detection diagram of Example 2;

[0028] Figure 3 It is the TGA detection diagram of Example 3;

[0029] Figure 4 This is the TGA detection diagram of Comparative Example 1. DETAILED DESCRIPTION

[0030] The following is a clear and complete description of the technical solutions in the embodiments of the present invention in conjunction with specific embodiments. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0031] See also Figure 1-4 The sealing protective lubricating grease for high temperature and high vacuum of the present embodiment comprises the following raw materials in parts by weight:

[0032] Perfluoropolyether oil (PFPE): 60-85%

[0033] Solid filler: 12-30%

[0034] Stabilizer: 3~10%.

[0035] The solid filler of this embodiment is one or more combinations of polytetrafluoroethylene (PTFE), melamine cyanurate, fumed silica, zinc oxide, and bentonite.

[0036] The stabilizer of this embodiment is one or more combinations of polyethylene glycol, perfluoroacetic acid, ethanol, carbonated acrylic acid, and perfluororesin.

[0037] The viscosity range of the perfluoropolyether (PFPE) of this embodiment is 1750-1900 mm2 / s, kinematic viscosity at 20°C.

[0038] The fumed silicon oxide of this embodiment also adopts the blending treatment;

[0039] The specific reconciliation method is:

[0040] 3-6 parts of flaky talc, 1-3 parts of nano-silica sol, 5-8 parts of sodium dodecylbenzene sulfonate solution and 1-2 parts of yttrium oxide are mixed and stirred thoroughly, and then filtered and dried to obtain modified flaky talc;

[0041] First immerse 5-8 parts of fumed silicon oxide into 6-10 parts of lanthanum nitrate solution, then add 2-3 parts of silane coupling agent KH550 and 1-3 parts of modified flaky talcum powder, and then perform ultrasonic treatment. After the ultrasonic treatment is completed, filter and dry.

[0042] The mass fraction of the sodium dodecylbenzenesulfonate solution in this embodiment is 2-5%.

[0043] The mass fraction of the lanthanum nitrate solution in this embodiment is 5-8%.

[0044] The ultrasonic power of the ultrasonic treatment in this embodiment is 350-400W, and the ultrasonic time is 20-30min.

[0045] A method for preparing a sealing protective grease for high temperature and high vacuum comprises the following steps: mixing perfluoropolyether oil (PFPE) and a solid filler at a rotation speed of 46 rpm for uniform mixing for 10-15 min, adding a stabilizer for dispersion stirring for 10-15 min, heating to 100-110° C., maintaining the temperature for 0.5-1 h, pouring out and cooling, and then grinding with a three-roller for 2-3 times for homogenization. After homogenization, degassing is performed with a high vacuum disperser at 0.8 Mpa and a rotation speed of 295 rpm to obtain a finished product.

[0046] Example 1:

[0047] 007: Perfluoropolyether oil (PFPE): 82%

[0048] Solid filler: 15%

[0049] Stabilizer: 3%

[0050] In this example, the viscosity of perfluoropolyether (PFPE) (20°C kinematic viscosity) is 1800 mm2 / s; the solid filler is fumed silica with a particle size of 0.8 nm, and the stabilizer is polyethylene glycol with a pH value of 5.0.

[0051] A method for preparing a sealing protective grease for high temperature and high vacuum comprises the following steps: mixing perfluoropolyether oil (PFPE) and a solid filler at a rotation speed of 46 rpm for 12.5 min, adding a stabilizer for dispersion and stirring for 12 min, heating to 105° C., keeping the temperature constant for 0.7 h, pouring out and cooling, and then grinding with a three-roller for 3 times for homogenization, and after the homogenization is completed, degassing with a high vacuum disperser at 0.8 Mpa and a rotation speed of 295 rpm to obtain a finished product.

[0052] Example 2:

[0053] 008: Perfluoropolyether oil (PFPE): 74%

[0054] Solid filler: 20%

[0055] Stabilizer: 6%

[0056] In this example, the viscosity of the perfluoropolyether oil (PFPE) (20°C kinematic viscosity) is 1800 mm2 / s; the solid filler is fumed silica with a particle size of 0.8 nm, and the stabilizer is polyethylene glycol with a pH value of 5.0.

[0057] Fumed silica also uses a blending process;

[0058] The specific reconciliation method is:

[0059] 4.5 parts of flaky talc, 2 parts of nano-silica sol, 6.5 parts of sodium dodecylbenzene sulfonate solution and 1.5 parts of yttrium oxide were mixed and stirred thoroughly, and then filtered and dried to obtain modified flaky talc;

[0060] First immerse 6.5 parts of fumed silicon oxide into 8 parts of lanthanum nitrate solution, then add 2.5 parts of silane coupling agent KH550 and 2 parts of modified flaky talcum powder, and then perform ultrasonic treatment. After the ultrasonic treatment is completed, filter and dry.

[0061] The mass fraction of the sodium dodecylbenzenesulfonate solution in this embodiment is 3.5%.

[0062] The mass fraction of the lanthanum nitrate solution in this embodiment is 6.5%.

[0063] The ultrasonic power of the ultrasonic treatment in this embodiment is 370W, and the ultrasonic time is 25min.

[0064] A method for preparing a sealing protective grease for high temperature and high vacuum comprises the following steps: mixing perfluoropolyether oil (PFPE) and a solid filler at a rotation speed of 46 rpm for 12.5 min, adding a stabilizer for dispersion and stirring for 12 min, heating to 105° C., keeping the temperature constant for 0.7 h, pouring out and cooling, and then grinding with a three-roller for 3 times for homogenization, and after the homogenization is completed, degassing with a high vacuum disperser at 0.8 Mpa and a rotation speed of 295 rpm to obtain a finished product.

[0065] Example 3:

[0066] 009: Perfluoropolyether oil (PFPE): 67%

[0067] Solid filler: 25%

[0068] Stabilizer: 8%

[0069] In this example, the viscosity of perfluoropolyether (PFPE) (20°C kinematic viscosity) is 1800 mm2 / s; the solid filler is fumed silica with a particle size of 0.8 nm, and the stabilizer is polyethylene glycol with a pH value of 5.0.

[0070] A method for preparing a sealing protective grease for high temperature and high vacuum comprises the following steps: mixing perfluoropolyether oil (PFPE) and a solid filler at a rotation speed of 46 rpm for 12.5 min, adding a stabilizer for dispersion and stirring for 12 min, heating to 105° C., keeping the temperature constant for 0.7 h, pouring out and cooling, and then grinding with a three-roller for 3 times for homogenization, and after the homogenization is completed, degassing with a high vacuum disperser at 0.8 Mpa and a rotation speed of 295 rpm to obtain a finished product.

[0071] Comparative Example 1

[0072] 010: Methyl silicone oil: 80%

[0073] Fumed silicon oxide: 15%

[0074] Structural improver: 5%

[0075] This comparative example is a sealing protective grease solution circulating on the market, which uses silicone oil as the base oil and fumed silica as the thickener. The structure improver can be hydroxy silicone oil or polyethylene glycol. The viscosity of the methyl silicone oil in the comparative example (25°C kinematic viscosity) is 1780mm2 / s; the solid filler is fumed silica with a particle size of 0.8nm, and the structure improver is hydroxy silicone oil (25°C kinematic viscosity): 36mm2 / s.

[0076] Comparative Example Preparation Method

[0077] 011: Mix methyl silicone oil and solid filler fumed silica at a speed of 46rpm for 10-15min, add structure improver and disperse and stir for 10-15min, heat to 120-130℃, keep constant temperature for 1-1.5h, take samples for infrared spectrum detection during the constant temperature process, after there is no infrared spectrum peak of hydroxyl silicone oil in the spectrum, pour out and cool, then grind with three rollers for 2-3 times for fat homogenization, after fat homogenization, use high vacuum disperser for degassing at 0.8Mpa and speed of 295rpm to obtain the finished product.

[0078] 012: After refining the examples and comparison ratios, data detection and analysis were carried out, and the indicator data are as follows

[0079]

[0080] Through the detection of data, the above examples and comparative examples are all within the range of No. 2 grease (265-295). Through the test of oil separation and evaporation of steel mesh under high temperature conditions, it can be seen that the data parameters in the example scheme test are far better than the parameters of high temperature resistant sealing grease circulating on the market. The volatile memory loss and penetration under high temperature conditions have been greatly improved.

[0081] A sealing protective grease for high temperature and high vacuum conditions. This sealing protective grease has excellent chemical inertness resistance, low temperature resistance and high temperature resistance, and extremely low volatility. It can meet the requirements of bearing and pump valve sealing under high temperature and high vacuum conditions, and can achieve the characteristics of no leakage and no loss. It can meet the sealing protection requirements of equipment under high temperature 200℃ and vacuum conditions.

[0082] The fumed silicon oxide in the product of Example 2 is also blended. The performance of the lubricating oil product obtained is further improved by optimizing and improving the blending of the fumed silicon oxide.

[0083] In order to verify the characteristics of the example and the comparative example at high temperature again, TGA detection and analysis were carried out. Through the TGA detection and analysis of the example and the comparative example, the starting temperature of the example at high temperature and large-scale volatilization is higher than the starting temperature of the comparative example at high temperature and large-scale volatilization is 60°C higher than that of the comparative example. It can further be explained that under the conditions of high temperature and high pressure, its volatility, leakage and loss performance can better meet the use of sealing protection.

[0084] It will be apparent to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above and that the present invention can be implemented in other specific forms without departing from the spirit or essential features of the present invention. Therefore, the embodiments should be considered exemplary and non-restrictive in all respects, and the scope of the present invention is defined by the appended claims rather than the above description, and it is intended that all changes falling within the meaning and scope of the equivalent elements of the claims be included in the present invention.

[0085] In addition, it should be understood that although the present specification is described according to implementation modes, not every implementation mode contains only one independent technical solution. This description of the specification is only for the sake of clarity. Those skilled in the art should regard the specification as a whole. The technical solutions in each embodiment may also be appropriately combined to form other implementation modes that can be understood by those skilled in the art.

Claims

1. A sealing and protective grease for high temperature and high vacuum, characterized in that: The sealing protective grease comprises the following raw materials in parts by weight: Perfluoropolyether oil (PFPE): 60-85% Solid filler: 12-30% Stabilizer: 3-10%.

2. The sealing and protective lubricating grease for high temperature and high vacuum according to claim 1, characterized in that: Said The solid filler is one or more combinations of polytetrafluoroethylene (PTFE), melamine cyanurate, fumed silica, zinc oxide and bentonite.

3. The sealing and protective lubricating grease for high temperature and high vacuum according to claim 1, characterized in that: The stabilizer is one or more combinations of polyethylene glycol, perfluoroacetic acid, ethanol, carbonated acrylic acid and perfluororesin.

4. The sealing and protective lubricating grease for high temperature and high vacuum according to claim 1, characterized in that: The viscosity range of the perfluoropolyether (PFPE) is 1750 to 1900 mm2 / s at 20°C.

5. The sealing and protective lubricating grease for high temperature and high vacuum according to claim 2, characterized in that: The fumed silicon oxide is also treated by blending; The specific reconciliation method is: 3-6 parts of flaky talc, 1-3 parts of nano-silica sol, 5-8 parts of sodium dodecylbenzene sulfonate solution and 1-2 parts of yttrium oxide are mixed and stirred thoroughly, and then filtered and dried to obtain modified flaky talc; First immerse 5-8 parts of fumed silicon oxide into 6-10 parts of lanthanum nitrate solution, then add 2-3 parts of silane coupling agent KH550 and 1-3 parts of modified flaky talcum powder, and then perform ultrasonic treatment. After the ultrasonic treatment is completed, filter and dry.

6. The sealing and protective lubricating grease for high temperature and high vacuum according to claim 5, characterized in that: The mass fraction of the sodium dodecylbenzene sulfonate solution is 2-5%.

7. The sealing and protective lubricating grease for high temperature and high vacuum according to claim 5, characterized in that: The mass fraction of the lanthanum nitrate solution is 5-8%.

8. The sealing and protective lubricating grease for high temperature and high vacuum according to claim 5, characterized in that: The ultrasonic power of the ultrasonic treatment is 350-400W, and the ultrasonic time is 20-30min.

9. A method for preparing a sealing protective grease for high temperature and high vacuum, comprising the following steps: The perfluoropolyether oil (PFPE) and the solid filler are mixed and stirred evenly at a speed of 46 rpm for 10-15 minutes, and a stabilizer is added and dispersed and stirred for 10-15 minutes. The temperature is raised to 100-110°C and kept at a constant temperature for 0.5-1h. The mixture is poured out and cooled, and then ground with a three-roller for 2-3 times for fat homogenization. After the fat homogenization is completed, a high vacuum disperser is used for degassing at 0.8Mpa and a speed of 295rpm to obtain the finished product.

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