Wide-temperature grease composition prepared from waste PAO fully-synthetic lubricating oil and preparation method of wide-temperature grease composition

By mixing waste PAO fully synthetic lubricant with other components and performing specific process processing, a wide temperature grease composition is prepared, which solves the problems of recycling and utilization of waste PAO fully synthetic lubricant and improving grease performance, and achieves a wider use temperature range and better extreme pressure performance.

CN119614271APending Publication Date: 2025-03-14LIAONING LONGYUAN NEW ENERGY DEV CO LTD
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Patent Information

Application Number
CN202411637855.5
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-11-15
Publication Date
2025-03-14

AI Technical Summary

Technical Problem

The prior art is difficult to effectively recover and utilize waste PAO fully synthetic lubricating oil, and the existing grease has a narrow temperature range and low extreme pressure performance.

Method used

A wide-temperature grease composition is prepared by mixing waste PAO fully synthesized lubricating oil with mineral oil base oil, thickening agent, antioxidant and antirust agent, and saponification reaction, dehydration, high-temperature refining and high-pressure shearing.

Benefits of technology

It realizes the recycling and reuse of waste PAO fully synthetic lubricant, broadens the use temperature range of grease, and improves the performance of grease, especially suitable for low temperature and heavy load conditions.

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Abstract

The invention relates to a wide-temperature grease composition prepared from waste PAO total synthesis lubricating oil and a preparation method of the wide-temperature grease composition, and the wide-temperature grease composition comprises the following components in parts by weight: 60-100 parts of waste PAO total synthesis lubricating oil, 6-50 parts of mineral oil base oil, 5-18 parts of a thickening agent, 0.5-5 parts of an antioxidant and 1-9 parts of an antirust agent. The waste PAO fully-synthesized lubricating oil is directly used as a main raw material and is matched with other components, so that the lubricating grease meeting the requirements is obtained. By adding the waste PAO total synthesis lubricating oil, on one hand, recycling of the waste PAO total synthesis lubricating oil is achieved, waste is turned into wealth, on the other hand, the use temperature range of the lubricating grease is widened, and the performance of the lubricating grease is effectively improved.
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Description

Technical Field

[0001] The present invention relates to the technical field of lubricating grease, and in particular to a wide-temperature grease composition prepared by utilizing waste PAO fully synthetic lubricating oil and a preparation method thereof. Background Art

[0002] PAO (Poly-alpha-olefin) fully synthetic oil is a Class IV base oil and an important raw material for producing high-grade lubricating greases. It has excellent viscosity-temperature performance, low-temperature fluidity and high thermal oxidation stability. It can replace traditional petrochemical refining base oils to improve fuel economy and equipment life. It is currently mainly used in gear oils, hydraulic oils, engine oils, etc. The pour point is as low as -33°C, which can adapt to both high temperatures and severe cold areas.

[0003] PAO fully synthetic lubricants are composed of PAO and additives, with wind power gear oil as the main representative, and its PAO usage exceeds 80%. The main reasons for the deterioration of wind power gear oil are the entry of water and particulate matter and the decrease in additive content. Compared with waste mineral-based lubricants, its base oil has a lower degree of deterioration, and the performance of PAO is retained, and it still has a high recycling value. At present, for waste oil regeneration, the common treatment process is thermal sedimentation-distillation-solvent refining-white clay adsorption, which mainly targets waste mineral-based lubricants with a high degree of deterioration. However, the water content and particle content in wind power waste gear oil are low, and the thermal sedimentation process is energy-intensive and has little effect; in addition, PAO fully synthetic lubricants produce less than 20% of fractions at 350~500℃. If distillation is used directly, PAO cannot be directly separated. Therefore, the conventional regeneration route for the disposal of waste PAO fully synthetic lubricants cannot achieve the recycling effect.

[0004] In addition, the existing grease has a narrow operating temperature range and low extreme pressure performance. Therefore, it is very necessary to improve the performance of the grease while achieving the recycling of waste PAO fully synthetic lubricants. Summary of the invention

[0005] The purpose of the present invention is to provide a wide-temperature grease composition prepared using waste PAO fully synthetic lubricating oil and a preparation method thereof, so as to realize the recycling and reuse of waste PAO fully synthetic lubricating oil, effectively broaden the operating temperature range of the grease, and improve the performance of the grease.

[0006] In order to achieve the above-mentioned purpose, the present invention provides a wide-temperature grease composition prepared by using waste PAO fully synthetic lubricating oil. The wide-temperature grease composition comprises, by weight: 60 to 100 parts of waste PAO fully synthetic lubricating oil, 6 to 50 parts of mineral oil base oil, 5 to 18 parts of thickener, 0.5 to 5 parts of antioxidant, and 1 to 9 parts of rust inhibitor.

[0007] Optionally, the wide temperature grease composition preferably includes, by weight: 70-90 parts of waste PAO fully synthetic lubricating oil, 20-30 parts of mineral oil base oil, 10-18 parts of thickener, 0.5-3 parts of antioxidant, and 1-3 parts of rust inhibitor.

[0008] Optionally, the viscosity of the waste PAO fully synthetic lubricant at a temperature of 40°C is 350-390 mm 2 / s.

[0009] Optionally, the waste PAO fully synthetic lubricant is wind power waste gear oil; and the mineral oil base oil is one of 150N base oil and 500N base oil.

[0010] Optionally, the thickener includes 12-hydroxystearic acid, a low molecular weight organic acid and an inorganic base; the low molecular weight organic acid is sebacic acid or azelaic acid, and the inorganic base is liquid lithium or lime milk.

[0011] Optionally, the molar ratio of the 12-hydroxystearic acid to the low molecular weight organic acid is 3:1 to 5:1.

[0012] Optionally, the antioxidant is one of diphenylamine and N-phenyl-α-naphthylamine; the rust inhibitor is at least one of barium petroleum sulfonate, barium polyalkylbenzene sulfonate, and barium dinonylnaphthalene sulfonate.

[0013] Another aspect of the present invention provides a method for preparing a wide temperature range fat composition, the method comprising the following steps: Mixing waste PAO fully synthetic lubricating oil with mineral oil base oil to obtain a mixed base oil; Adding a thickener and an antioxidant to 1 / 2 of the mixed base oil for saponification reaction, and then adding 1 / 4 of the mixed base oil for dehydration and high-temperature refining to obtain a mixed material; The remaining 1 / 4 of the mixed base oil is added to the mixed material as quenching oil and stirred, and then a rust inhibitor is added, and high-pressure shearing, homogenization and vacuum degassing are performed after continued cooling; In parts by weight, the waste PAO fully synthetic lubricating oil is 60-100 parts, the mineral oil base oil is 6-50 parts, the thickener is 5-18 parts, the antioxidant is 0.5-5 parts, and the rust inhibitor is 1-9 parts.

[0014] Optionally, the saponification reaction temperature is 95-105°C, and the time is 80-130 min; the dehydration temperature is 130-150°C, and the time is 25-35 min; the high-temperature refining temperature is 180-220°C, and the time is 10-15 min.

[0015] Optionally, the temperature of the quenching oil is 0°C; the temperature after continued cooling is 100-130°C.

[0016] Through the above technical solution, the present invention directly uses waste PAO fully synthetic lubricating oil as the main raw material, and obtains grease that meets the requirements by combining with other components. The addition of waste PAO fully synthetic lubricating oil, on the one hand, realizes the recycling and reuse of waste PAO fully synthetic lubricating oil, turning waste into treasure, and on the other hand, broadens the use temperature range of grease, effectively improving the performance of grease.

[0017] Other features and advantages of the present invention will be described in detail in the following detailed description. DETAILED DESCRIPTION

[0018] The specific embodiments of the present invention are described in detail below. It should be understood that the specific embodiments described herein are only used to illustrate and explain the present invention, and are not used to limit the present invention.

[0019] The waste PAO fully synthetic lubricant of the present invention is waste oil generated after the use of lubricant blended with PAO base oil, which belongs to HW08 hazardous waste. At present, it is mainly recycled and regenerated according to the waste mineral-based lubricant regeneration process. The present invention has found through research that the waste PAO fully synthetic lubricant after a certain service life has a low degree of deterioration, mainly a small amount of water, impurities and the loss of some additives, and still has a high resource recovery value, but the thermal sedimentation process is energy-intensive and has little effect; in addition, PAO fully synthetic lubricant produces less than 20% of fractions at 350~500℃. If distillation is used, PAO cannot be directly separated. Therefore, the waste PAO fully synthetic lubricant cannot be recycled according to the current conventional regeneration route. In view of this, the present invention provides a wide temperature grease composition, which uses waste PAO fully synthetic lubricant as one of the base oil components.

[0020] Therefore, one aspect of the present invention provides a wide temperature grease composition prepared using waste PAO fully synthetic lubricating oil, which comprises, by weight: 60 to 100 parts of waste PAO fully synthetic lubricating oil, 6 to 50 parts of mineral oil base oil, 5 to 18 parts of thickener, 0.5 to 5 parts of antioxidant, and 1 to 9 parts of rust inhibitor.

[0021] According to the present invention, optionally, the wide temperature grease composition preferably includes, by weight: 70-90 parts of waste PAO fully synthetic lubricating oil, 20-30 parts of mineral oil base oil, 10-18 parts of thickener, 0.5-3 parts of antioxidant, and 1-3 parts of rust inhibitor.

[0022] According to the present invention, optionally, the viscosity of the waste PAO fully synthetic lubricating oil at a temperature of 40°C is 350-390 mm 2 / s.

[0023] According to the present invention, optionally, the waste PAO fully synthetic lubricant is wind power waste gear oil; and the mineral oil base oil is one of 150N base oil and 500N base oil.

[0024] According to the present invention, optionally, the thickener includes 12-hydroxystearic acid, a low molecular weight organic acid and an inorganic base; the low molecular weight organic acid is sebacic acid or azelaic acid, and the inorganic base is liquid lithium or lime milk. By selecting the above two acids to prepare the composite grease, the high temperature performance and extreme pressure performance of the obtained grease composition are better.

[0025] According to the present invention, optionally, the specific dosage relationship of the 12-hydroxystearic acid and the low-molecular organic acid of the present invention is not limited and can be changed within a certain range according to actual needs. For example, the amount ratio of the 12-hydroxystearic acid to the low-molecular organic acid is 3:1~5:1.

[0026] According to the present invention, optionally, the present invention does not limit the specific selection of antioxidants and rust inhibitors, and they can be antioxidants and rust inhibitors commonly used in the art, for example, the antioxidant is one of diphenylamine and N-phenyl-α-naphthylamine; the rust inhibitor is at least one of barium petroleum sulfonate, barium polyalkylbenzene sulfonate, and barium dinonylnaphthalene sulfonate.

[0027] Existing waste lubricating oil needs to be purified by pretreatment, distillation, clay adsorption and other processes before use, but the inventors of the present invention have found that by directly using waste PAO fully synthetic lubricating oil as raw material, without regeneration, a grease that meets the requirements can also be obtained. Therefore, directly using waste PAO fully synthetic lubricating oil as the main raw material, and obtaining a grease that meets the requirements by combining with other components, the process of regenerating waste oil into base oil and then mixing the base oil into grease is omitted, which can greatly reduce costs, reduce process, save energy and have considerable economic benefits.

[0028] In addition, although there are a certain amount of impurity particles and water in the waste PAO fully synthetic lubricant, by adjusting the amount of thickener and base oil, controlling the dehydration temperature and stirring time, the addition of waste PAO fully synthetic lubricant will not have an adverse effect on the final product.

[0029] Therefore, the waste PAO fully synthetic lubricant of the present invention is directly downgraded and utilized to replace the use of part of the mineral oil in the grease, giving full play to the low-temperature performance of PAO (pour point as low as -33°C), retaining the advantages of PAO extreme pressure and anti-wear, and can effectively solve the problems of limited use temperature and poor extreme pressure performance of mineral grease. The grease of the present invention is particularly suitable for the use of equipment lubrication under low temperature and heavy load conditions. Therefore, the addition of waste PAO fully synthetic lubricant, on the one hand, realizes the recycling and reuse of waste PAO fully synthetic lubricant, turning waste into treasure, and on the other hand, broadens the use temperature range of grease, effectively improving the performance of grease.

[0030] Therefore, another aspect of the present invention provides a method for preparing a wide temperature range fat composition, the method comprising the following steps: Mixing waste PAO fully synthetic lubricating oil with mineral oil base oil to obtain mixed base oil; Adding a thickener and an antioxidant to 1 / 2 of the mixed base oil for saponification reaction, and then adding 1 / 4 of the mixed base oil for dehydration and high-temperature refining to obtain a mixed material; The remaining 1 / 4 of the mixed base oil is added to the mixed material as quenching oil and stirred, and then a rust inhibitor is added, and high-pressure shearing, homogenization and vacuum degassing are performed after continued cooling; In parts by weight, the waste PAO fully synthetic lubricating oil is 60-100 parts, the mineral oil base oil is 6-50 parts, the thickener is 5-18 parts, the antioxidant is 0.5-5 parts, and the rust inhibitor is 1-9 parts.

[0031] According to the present invention, optionally, the present invention does not impose any specific restrictions on the ratio of the mixed base oil, as long as the mixed base oil and the thickener, antioxidant, and rust inhibitor can be fully mixed. For example, the mixed base oil can be preferably added at 1 / 2, 1 / 4, and 1 / 4 respectively.

[0032] According to the present invention, optionally, the specific parameters of the saponification reaction of the present invention can be changed within a certain range, as long as the mixed base oil, antioxidant and thickener can be mixed evenly. For example, the saponification reaction temperature is 95-105°C, and the time is 80-130min. In a specific embodiment, the saponification reaction of the present invention is carried out in two steps. In the first step, 12-hydroxystearic acid and antioxidant are added to 1 / 2 of the mixed base oil, heated to 95-105°C and stirred at a constant temperature, and liquid lithium or lime milk is added after complete dissolution, and the saponification reaction is 60-90min; in the second step, low molecular weight organic acid and liquid lithium or lime milk are added, and the saponification reaction is 20-40min.

[0033] According to the present invention, the specific parameters of the dehydration and high-temperature refining of the present invention can be optionally changed within a certain range, as long as the water can be completely removed. For example, the dehydration temperature is 130-150°C and the time is 25-35 minutes; the high-temperature refining temperature is 180-220°C and the time is 10-15 minutes.

[0034] According to the present invention, optionally, the temperature of the quenching oil is 0°C; and the temperature after further cooling is 100-130°C.

[0035] According to the present invention, optionally, a specific method for preparing a wide temperature fat composition comprises the following steps: Mixing waste PAO fully synthetic lubricating oil with mineral oil base oil to make a mixed base oil; Add 12-hydroxystearic acid and antioxidant to 1 / 2 of the mixed base oil, heat to 95-105°C and stir at constant temperature, add liquid lithium or lime milk after it is completely dissolved, and saponify for 60-90 minutes; then add low molecular weight organic acid and liquid lithium or lime milk, and saponify for 20-40 minutes; After saponification, add 1 / 4 mixed base oil to reduce the viscosity of the system, first heat to 130~150℃ for dehydration, the dehydration time is 25~35min, and then continue to heat to 180~220℃ for high-temperature refining, the refining time is 10~15min; The remaining 1 / 4 of the mixed base oil is added as quenching oil and stirred, and then a rust inhibitor is added; after cooling, high-pressure shearing, homogenization and vacuum degassing are performed.

[0036] The present invention mixes the components in the above order to achieve better mixing effect, thereby making the comprehensive performance of the prepared grease composition better.

[0037] The present invention is further illustrated by the following examples, but the present invention is not limited thereto.

[0038] Example 1 A composite lithium-based wide temperature grease, comprising the following raw material components in parts by weight: 320 # 72 parts of wind power waste gear oil; 20 parts of 500N base oil; 16 parts of thickener; 2.5 parts of diphenylamine; 1.5 parts of petroleum barium sulfonate. Among them, the thickener is 12-hydroxystearic acid, sebacic acid and liquid lithium, and the molar ratio of 12-hydroxystearic acid to sebacic acid is 3.5:1.

[0039] The preparation method of the composite lithium-based wide temperature grease comprises the following steps: Step 1: Convert 320 # The wind power waste gear oil is mixed with 500N base oil as mixed base oil; Step 2: Add 12-hydroxystearic acid and diphenylamine to 1 / 2 of the mixed base oil, heat to 100°C and stir at a constant temperature, add liquid lithium after complete dissolution, and saponify for 70 minutes; then add sebacic acid and liquid lithium, and saponify for 25 minutes; Step 3: After the saponification is completed, add 1 / 4 of the mixed base oil to reduce the viscosity of the system, first heat to 145°C for dehydration, the dehydration time is 30 minutes, and then continue to heat to 220°C for high-temperature refining, the refining time is 10 minutes; Step 4: Add the remaining 1 / 4 of the mixed base oil as quench oil and stir, then add petroleum barium sulfonate; Step 5: Continue cooling to 125°C and then perform high pressure shearing, homogenization and vacuum degassing.

[0040] Example 2 A composite calcium-based wide temperature grease, comprising the following raw material components in parts by weight: 320 # 88 parts of wind power waste gear oil; 28 parts of 150N base oil; 12 parts of thickener; 1 part of N-phenyl-α-naphthylamine; 3 parts of rust inhibitor. Among them, the thickener is 12-hydroxystearic acid, azelaic acid and lime milk, and the molar ratio of 12-hydroxystearic acid to azelaic acid is 4.5:1; the rust inhibitor is a mixture of polyalkylbenzene sulfonate barium and dinonylnaphthalene sulfonate barium.

[0041] The preparation method of the composite calcium-based wide temperature fat comprises the following steps: Step 1: Convert 320 # Wind power waste gear oil is mixed with 150N base oil as mixed base oil; Step 2: Add 12-hydroxystearic acid and N-phenyl-α-naphthylamine to 1 / 2 of the mixed base oil, heat to 95°C and stir at a constant temperature, add lime milk after complete dissolution, and saponify for 90 minutes; then add azelaic acid and lime milk, and saponify for 35 minutes; Step 3: After saponification, add 1 / 4 of the mixed base oil to reduce the viscosity of the system, first heat to 135°C for dehydration, the dehydration time is 30 minutes, and then continue to heat to 185°C for high-temperature refining, the refining time is 15 minutes; Step 4: adding the remaining 1 / 4 of the mixed base oil as quench oil and stirring, and then adding a mixture of barium polyalkylbenzene sulfonate and barium dinonylnaphthalene sulfonate; Step 5: Continue cooling to 110°C and then perform high pressure shearing, homogenization and vacuum degassing.

[0042] Comparative Example 1 The method described in Example 1 is used for implementation, except that the composite lithium-based grease contains the following raw material components in parts by weight: 108 parts of 500N base oil, 12 parts of 150N base oil, 14 parts of thickener, 2.5 parts of diphenylamine, and 2.5 parts of barium petroleum sulfonate. The thickener is 12-hydroxystearic acid, sebacic acid, and liquid lithium, and the molar ratio of 12-hydroxystearic acid to sebacic acid is 3:1.

[0043] Comparative Example 2 The method described in Example 2 is followed, except that the universal calcium-based grease contains the following raw material components in parts by weight: 320 # 72 parts of wind power waste gear oil; 20 parts of 500N base oil; 12 parts of thickener; 1 part of N-phenyl-α-naphthylamine; 3 parts of rust inhibitor. Among them, the thickener is 12-hydroxystearic acid and lime milk; the rust inhibitor is a mixture of polyalkylbenzene sulfonate barium and dinonylnaphthalene sulfonate barium.

[0044] The properties of the lubricating greases prepared by the formulation processes of the embodiments of the present invention and the comparative examples are shown in Table 1.

[0045] Table 1.

[0046]

[0047] It can be seen from Table 1 that the wide temperature grease prepared in Example 1-2 fully meets the technical index requirements, including: (1) the temperature range of use is as low as -40°C, with a wide range of application and strong temperature adaptability; (2) without the addition of anti-wear agents, the grease in the present invention has good extreme pressure performance, comparable to composite lithium-based grease and more than 25% higher than calcium-based grease; (3) it has good water and rust resistance and can be used for lubrication of equipment in humid environments.

[0048] The preferred embodiments of the present invention are described in detail above. However, the present invention is not limited to the specific details in the above embodiments. Within the technical concept of the present invention, a variety of simple modifications can be made to the technical solution of the present invention, and these simple modifications all belong to the protection scope of the present invention.

[0049] It should also be noted that the various specific technical features described in the above specific embodiments can be combined in any suitable manner without contradiction. In order to avoid unnecessary repetition, the present invention will not further describe various possible combinations.

[0050] In addition, various embodiments of the present invention may be arbitrarily combined, and as long as they do not violate the concept of the present invention, they should also be regarded as the contents disclosed by the present invention.

Claims

1. A wide temperature grease composition prepared by using waste PAO fully synthetic lubricating oil, characterized in that: In parts by weight, the wide temperature fat composition comprises: Waste PAO fully synthetic lubricating oil 60~100 parts, mineral oil base oil 6~50 parts, thickener 5~18 parts, antioxidant 0.5~5 parts, rust inhibitor 1~9 parts.

2. The wide temperature range fat composition according to claim 1, wherein: Preferably, the wide temperature grease composition comprises, by weight: 70-90 parts of waste PAO fully synthetic lubricating oil, 20-30 parts of mineral oil base oil, 10-18 parts of thickener, 0.5-3 parts of antioxidant, and 1-3 parts of rust inhibitor.

3. The wide temperature range fat composition according to claim 1, wherein: The viscosity of the waste PAO fully synthetic lubricating oil at a temperature of 40° C. is 350-390 mm 2 / s.

4. The wide temperature range fat composition according to claim 1, wherein: The waste PAO fully synthetic lubricating oil is wind power waste gear oil; The mineral oil base oil is one of 150N base oil and 500N base oil.

5. The wide temperature range fat composition according to claim 1, wherein: The thickener includes 12-hydroxystearic acid, low molecular weight organic acid and inorganic base; The low molecular weight organic acid is sebacic acid or azelaic acid, and the inorganic base is liquid lithium or lime milk.

6. The wide temperature range fat composition according to claim 5, wherein: The molar ratio of the 12-hydroxystearic acid to the low molecular weight organic acid is 3:1 to 5:

1.

7. The wide temperature range grease composition according to claim 1, wherein: The antioxidant is one of diphenylamine and N-phenyl-α-naphthylamine; The rust inhibitor is at least one of barium petroleum sulfonate, barium polyalkylbenzene sulfonate, and barium dinonylnaphthalene sulfonate.

8. A method for preparing a wide temperature range fat composition, characterized in that: The method comprises the following steps: Mixing waste PAO fully synthetic lubricating oil with mineral oil base oil to obtain a mixed base oil; Adding a thickener and an antioxidant to 1 / 2 of the mixed base oil for saponification reaction, and then adding 1 / 4 of the mixed base oil for dehydration and high-temperature refining to obtain a mixed material; The remaining 1 / 4 of the mixed base oil is added to the mixed material as quenching oil for stirring, and then a rust inhibitor is added, and high-pressure shearing, homogenization and vacuum degassing are performed after continued cooling; In parts by weight, the waste PAO fully synthetic lubricating oil is 60-100 parts, the mineral oil base oil is 6-50 parts, the thickener is 5-18 parts, the antioxidant is 0.5-5 parts, and the rust inhibitor is 1-9 parts.

9. The method according to claim 8, wherein: The saponification reaction temperature is 95-105°C and the time is 80-130min; The dehydration temperature is 130-150°C and the time is 25-35 minutes; The high temperature refining temperature is 180-220°C and the time is 10-15 minutes.

10. The method according to claim 8, wherein: The temperature of the quenching oil is 0°C; the temperature after continued cooling is 100-130°C.