A biodegradable lubricant and its preparation method

Abstract

The present invention discloses a biodegradable lubricant and a preparation method thereof. The raw material composition of the biodegradable lubricant comprises, by weight, 20-30 parts of hydrogenated vegetable oil, 3-5 parts of n-butanol, 1-2 parts of amino acids, 3-5 parts of graphene oxide, and 0.1-0.3 parts of antioxidants. The preparation method comprises the following steps: S1, mixing the hydrogenated vegetable oil and n-butanol to obtain a mixed solution; S2, ball-milling 10%-50% of the mixed solution with 1-2 parts by weight of graphene oxide, mixing the ball-milled product with the remaining mixed solution and performing low-pressure rotary evaporation to obtain a base oil; S3, mixing the base oil with the amino acids, antioxidant, and remaining graphene oxide to obtain a biodegradable lubricant.

Description

Technical Field

[0001] The present invention relates to the technical field of lubricants, and in particular to a biodegradable lubricant and a preparation method thereof. Background Art

[0002] Lubricants have two main functions. On the one hand, they are used in mechanical transmission to reduce the friction resistance of friction pairs and slow down wear. On the other hand, they are used to add organic resins, which can effectively improve the lubricity of resins, improve the color of products, increase gloss, improve antistatic properties, promote melting, avoid degradation, increase product toughness, and effectively reduce energy consumption during processing. Adding internal lubricants can reduce the cohesive force between polymer molecular chains, accelerate melting, reduce melt viscosity, extend processing life, improve fluidity during processing and improve product transparency.

[0003] Current lubricants can be categorized as organic or inorganic based on their materials. The vast majority of organic lubricants use mineral oil as their base oil. Mineral oil, extracted from petroleum, is primarily a mixture of hydrocarbon molecules composed of carbon and hydrogen. Due to its low price and performance, which meets the lubrication needs of most machinery and equipment, it dominates the market. However, after use, this product accumulates in the environment, causing environmental pollution, primarily due to its non-biodegradable composition.

[0004] Patent specification with publication number CN109913300A discloses a biodegradable and environmentally friendly lubricant and a preparation method thereof. The lubricant comprises the following components: vegetable oil, an antioxidant, an emulsifier, sodium carbonate, hydrochloric acid, and an ionic liquid. The preparation method of the lubricant comprises: preparation of vegetable oil fatty acid methyl ester; preparation of primary modified vegetable oil; preparation of epoxidized primary modified vegetable oil; preparation of secondary modified vegetable oil; adding the secondary modified vegetable oil, ionic liquid, antioxidant, emulsifier, sodium carbonate, and hydrochloric acid to a reactor in sequence and stirring to obtain the lubricant; after the primary and secondary modifications of the vegetable oil, the C=C double bonds in the vegetable oil are eliminated and the glycerol in the vegetable oil molecules is replaced, thereby obtaining a modified vegetable oil with good oxidative stability. Experimental results show that the lubricant prepared by this patented technology has good biodegradability and lubricating effect.

[0005] Patent specification CN106367186A discloses a plant-oil-based biodegradable lubricant comprising the following components, by weight: 125-160 parts plant-based synthetic oil, 2-6 parts viscosity index improver, 2-5 parts preservative, 2-5 parts flake graphite, 2-5 parts fungicide, 2-5 parts defoamer, and 180-220 parts water. The plant-based synthetic oil comprises the following components, by weight: 5-10 parts oleic acid, 3-9 parts linoleic acid, 80-90 parts castor oil, 35-55 parts cottonseed oil, 1-3 parts stearic acid, and 1-3 parts dihydroxystearic acid. The plant-oil-based biodegradable lubricant and its preparation method provided by this patented technology significantly improve the maximum no-seizure load, exhibit excellent lubrication performance and stability, and are also biodegradable, contributing to environmental benefits. Summary of the Invention

[0006] The present invention provides a biodegradable lubricant that does not require the introduction of components such as catalysts. It uses hydrogenated vegetable oil as a basic component and is then modified with n-butanol, amino acids, and graphene oxide. While ensuring the biodegradability of the lubricant, it also has excellent lubrication performance.

[0007] A biodegradable lubricant, the raw materials of which are calculated by weight:

[0008]

[0009] Hydrogenated vegetable oil tends to be in a greasy state, which makes the hydrogenated vegetable oil more stable and the lubricant itself has better lubrication properties. The hydrogenated vegetable oil can be hydrogenated rapeseed oil and / or hydrogenated soybean oil, which can be obtained by hydrogenating rapeseed oil and / or soybean oil.

[0010] The amino acid may be isoleucine. Isoleucine has a certain antioxidant capacity and can improve the lubricating performance, maximum non-seizure load, sintering load and degradability of the lubricant after addition.

[0011] The antioxidant may be antioxidant 246 (2,4,6-tri-tert-butylphenol).

[0012] The present invention also provides a method for preparing the biodegradable lubricant, comprising the steps of:

[0013] S1, mixing hydrogenated vegetable oil and n-butanol to obtain a mixed solution;

[0014] S2, mixing 10%-50% of the mixed solution with 1-2 parts by mass of graphene oxide and ball milling, mixing the ball-milled product with the remaining mixed solution and performing low-pressure rotary evaporation to obtain a base oil;

[0015] S3, mixing the base oil with the amino acid, the antioxidant and the remaining graphene oxide to obtain the biodegradable lubricant.

[0016] The preparation method of the present invention divides graphene oxide into two parts. During the reaction process in step S2, a portion of the graphene oxide is used as a reaction medium for hydrogenated vegetable oil and n-butanol to promote the stability of the hydrogenated vegetable oil. In step S3, the remaining graphene oxide is used as an additive to ensure the lubricating properties of the lubricant.

[0017] The first portion of graphene oxide is used in step S2 to modify the hydrogenated vegetable oil and enhance its stability. During the ball-milling of the mixed solution and graphene oxide in step S2, the material becomes more viscous. Therefore, the present invention first ball-mills only 10%-50% of the mixed solution with 1-2 parts by mass of graphene oxide, and then mixes the milled product with the remaining mixed solution. If the entire mixed solution were ball-milled with 1-2 parts by mass, or even all of the graphene oxide, all at once, the material would become very viscous, and the lubricating effect, biodegradability, and other properties of the resulting lubricant would be reduced. The ball-milling process in step S2 also promotes the integration of graphene oxide into the overall system, improving its stability in the lubricant. Furthermore, if too much graphene oxide is added in step S2, the alcoholization and oxidation reaction of the hydrogenated vegetable oil will be excessive, and the resulting lubricant product will also fail to achieve the desired effect. The preparation method of the present invention achieves a lubricant with optimal overall performance by strictly controlling the degree of modification of the hydrogenated vegetable oil.

[0018] In step S1, in order to achieve better mixing, the mixing temperature may be 50-70°C.

[0019] In step S2, the ball milling time may be 0.5-1 h.

[0020] In step S2, low-pressure rotary evaporation can remove light substances from the base oil, thereby ensuring the distribution of the substance mass in the base oil, avoiding the mixing of small molecules, and improving the lubrication stability of the lubricant.

[0021] In step S2, the temperature of the low-pressure rotary evaporation can be 70-80°C, the time can be 20-30 minutes, and the vacuum degree can be 15-20 kPa.

[0022] In step S2, the recovery rate of the light material obtained by the low-pressure rotary evaporation can be controlled at 75wt%-85wt%.

[0023] In step S3, the base oil, amino acid, antioxidant, and remaining graphene oxide can be mixed by vibrating ball milling. The operating temperature can be no higher than 70° C., and the mixing time can be 0.5-1 hour. In step S3, the operating temperature can be no higher than 70° C. to prevent excessive oxidation of the hydrogenated vegetable oil in the presence of graphene oxide.

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

[0025] 1. The present invention uses hydrogenated vegetable oil as a basic component, and then modifies it with n-butanol, amino acid, and graphene oxide. While ensuring the biodegradability of the lubricant, it also has very good lubrication performance.

[0026] 2. The hydrogenated vegetable oil of the present invention can be hydrogenated rapeseed oil and / or soybean oil. The hydrogenated vegetable oil tends to be in a fat-like state, which makes the hydrogenated vegetable oil more stable and the lubricant itself has better lubricating properties.

[0027] 3. In the present invention, graphene oxide is used as a reaction medium for hydrogenated vegetable oil and n-butanol during the reaction process to promote the stability of the hydrogenated vegetable oil. In addition, graphene oxide is used as an additive to ensure the lubricating performance of the lubricant. DETAILED DESCRIPTION

[0028] The present invention will be further described below with reference to specific examples. It should be understood that these examples are only intended to illustrate the present invention and are not intended to limit the scope of the present invention.

[0029] Unless otherwise specified, “parts” in the following examples and comparative examples refer to parts by mass.

[0030] Example 1

[0031] S101 base oil preparation:

[0032] S1011 Hydrogenated vegetable oil and n-butanol mixture

[0033] 20 parts of hydrogenated vegetable oil (hydrogenated rapeseed oil) and 3 parts of n-butanol were mixed and heated to 50° C. to obtain a mixed solution.

[0034] S1012 disperses graphene oxide into the mixed liquid

[0035] A portion of the mixed liquid, generally about 1 / 3 of the total amount, is placed in a ball mill mixer with 1 part of graphene oxide, and then ball milled for 0.5 hours. The ball-milled product is then mixed with the remaining mixed liquid and stirred thoroughly to complete the graphene oxide dispersion treatment and obtain a dispersion.

[0036] S1013 dispersion liquid is evaporated at low pressure to remove light

[0037] The temperature of the low-pressure rotary evaporation was 70° C., the vacuum degree was 20 kPa, the rotary evaporation time was 20 min, and the recovery rate of the light material obtained by the low-pressure rotary evaporation was 80.2 wt %, to obtain the base oil.

[0038] S102 lubricant preparation:

[0039] Base oil, 2 parts of graphene oxide, 0.1 parts of 2,4,6-tri-tert-butylphenol, and 1 part of isoleucine were mixed and placed in a vibration ball mill at an operating temperature of 70° C. for 0.5 h.

[0040] In order to characterize the lubricating performance of the lubricant, the following test was conducted: according to SH / T0204, the wear spot diameter was measured to be 0.14 mm at 392 N for 60 min;

[0041] According to SH / T0202, the four-ball machine test was carried out and the maximum non-seizure load (P B ) is 1215N, sintering load (P D ) is 7130N;

[0042] The biodegradation rate was determined to be 78.0% according to CECL-33-93.

[0043] Example 2

[0044] S201 base oil preparation:

[0045] S2011 Hydrogenated vegetable oil and n-butanol mixture

[0046] 30 parts of hydrogenated vegetable oil (hydrogenated rapeseed oil) and 5 parts of n-butanol were mixed and heated to 70° C. to obtain a mixed solution.

[0047] S2012 disperses graphene oxide into the mixed liquid

[0048] A portion of the mixed liquid, generally about 1 / 3 of the total amount, is placed in a ball mill mixer with 2 parts of graphene oxide, and then ball milled for 1 hour. The ball-milled product is then mixed with the remaining mixed liquid and stirred thoroughly to complete the graphene oxide dispersion treatment and obtain a dispersion.

[0049] S2013 dispersion liquid low pressure rotary evaporation to remove light

[0050] The temperature of the low-pressure rotary evaporation is 80° C., the vacuum degree is 15 kPa, the rotary evaporation time is 30 min, and the recovery rate of the light material obtained by the low-pressure rotary evaporation is 75.9 wt %, to obtain the base oil.

[0051] S202 lubricant preparation:

[0052] Base oil, 3 parts of graphene oxide, 0.3 parts of 2,4,6-tri-tert-butylphenol, and 2 parts of isoleucine were mixed and placed in a vibration ball mill at an operating temperature of 70° C. for 1 hour.

[0053] In order to characterize the lubricating performance of the lubricant, the following test was conducted: according to SH / T0204, the wear spot diameter was measured to be 0.15 mm at 392 N for 60 min;

[0054] According to SH / T0202, the four-ball machine test was carried out and the P B 1220N, P D 7210N;

[0055] The biodegradation rate was determined to be 80.6% according to CECL-33-93.

[0056] Example 3

[0057] S301 base oil preparation:

[0058] S3011 Hydrogenated vegetable oil and n-butanol mixture

[0059] 25 parts of hydrogenated vegetable oil (hydrogenated rapeseed oil) and 4 parts of n-butanol were mixed and heated to 60° C. to obtain a mixed solution.

[0060] S3012 disperses graphene oxide into the mixed liquid

[0061] A portion of the mixed liquid, generally about 1 / 3 of the total amount, is placed in a ball mill mixer with 1.5 parts of graphene oxide, and then ball milled for 0.6 hours. The ball-milled product is then mixed with the remaining mixed liquid and stirred thoroughly to complete the graphene oxide dispersion treatment and obtain a dispersion.

[0062] S3013 dispersion liquid is evaporated at low pressure to remove light

[0063] The temperature of the low-pressure rotary evaporation was 75° C., the vacuum degree was 18 kPa, the rotary evaporation time was 25 min, and the recovery rate of the light material obtained by the low-pressure rotary evaporation was 76.1 wt %, to obtain the base oil.

[0064] S302 lubricant preparation:

[0065] Base oil, 2.5 parts of graphene oxide, 0.2 parts of 2,4,6-tri-tert-butylphenol, and 1.5 parts of isoleucine were mixed and placed in a vibration ball mill at an operating temperature of 70° C. for 0.8 h.

[0066] In order to characterize the lubricating performance of the lubricant, the following test was conducted: according to SH / T0204, the wear spot diameter was measured to be 0.14 mm at 392 N for 60 min;

[0067] According to SH / T0202, the four-ball machine test was carried out and the P B 1250N, P D 7200N;

[0068] The biodegradation rate was determined to be 83.1% according to CECL-33-93.

[0069] Comparative Example 1

[0070] S401 base oil preparation:

[0071] S4011 Hydrogenated vegetable oil and n-butanol mixture

[0072] 20 parts of hydrogenated vegetable oil (hydrogenated rapeseed oil) and 3 parts of n-butanol were mixed and heated to 50° C. to obtain a mixed solution.

[0073] S4012 disperses graphene oxide into the mixed liquid

[0074] The entire mixed solution and 1 part of graphene oxide were placed in a ball mill mixer, and then ball milled for 0.5 h, completing the graphene oxide dispersion treatment to obtain a dispersion.

[0075] S4013 dispersion liquid low pressure rotary evaporation to remove light

[0076] The temperature of the low-pressure rotary evaporation was 70° C., the vacuum degree was 20 kPa, the rotary evaporation time was 20 min, and the recovery rate of the light material obtained by the low-pressure rotary evaporation was 80.2 wt %, to obtain the base oil.

[0077] S402 lubricant preparation:

[0078] Base oil, 2 parts of graphene oxide, 0.1 parts of 2,4,6-tri-tert-butylphenol, and 1 part of isoleucine were mixed and placed in a vibration ball mill at an operating temperature of 70° C. for 0.5 h.

[0079] In order to characterize the lubricating performance of the lubricant, the following test was conducted: according to SH / T0204, the wear spot diameter was measured to be 0.22 mm at 392 N for 60 min;

[0080] According to SH / T0202, the four-ball machine test was carried out and the P B 1107N, P D 6850N;

[0081] The biodegradation rate was determined to be 77.5% according to CECL-33-93.

[0082] Comparative Example 2

[0083] S501 base oil preparation:

[0084] S5011 Hydrogenated vegetable oil and n-butanol mixture

[0085] 20 parts of hydrogenated vegetable oil (hydrogenated rapeseed oil) and 3 parts of n-butanol were mixed and heated to 50° C. to obtain a mixed solution.

[0086] S5012 disperses graphene oxide into the mixed liquid

[0087] A portion of the mixed liquid, generally about 1 / 3 of the total amount, is placed in a ball mill mixer with 3 parts of graphene oxide, and then ball milled for 0.5 hours. The ball-milled product is then mixed with the remaining mixed liquid and stirred thoroughly to complete the graphene oxide dispersion treatment and obtain a dispersion.

[0088] S5013 dispersion liquid is evaporated at low pressure to remove light

[0089] The temperature of the low-pressure rotary evaporation was 70° C., the vacuum degree was 20 kPa, the rotary evaporation time was 20 min, and the recovery rate of the light material obtained by the low-pressure rotary evaporation was 80.2 wt %, to obtain the base oil.

[0090] S502 lubricant preparation:

[0091] Mix the base oil, 0.1 part of 2,4,6-tri-tert-butylphenol and 1 part of isoleucine and put them into a vibration ball mill at an operating temperature of 70°C for 0.5 h.

[0092] In order to characterize the lubricating performance of the lubricant, the following test was conducted: according to SH / T0204, the wear spot diameter was measured at 392N for 60min and was 0.21mm;

[0093] According to SH / T0202, the four-ball machine test was carried out and the P B 1078N, P D 5950N;

[0094] The biodegradation rate was determined to be 76.8% according to CECL-33-93.

[0095] Comparative Example 3

[0096] S601 base oil preparation:

[0097] S6011 rapeseed oil and n-butanol mixture

[0098] 20 parts of rapeseed oil and 3 parts of n-butanol were mixed and heated to 50° C. to obtain a mixed solution.

[0099] S6012 disperses graphene oxide into the mixed liquid

[0100] A portion of the mixed liquid, generally about 1 / 3 of the total amount, is placed in a ball mill mixer with 1 part of graphene oxide, and then ball milled for 0.5 hours. The ball-milled product is then mixed with the remaining mixed liquid and stirred thoroughly to complete the graphene oxide dispersion treatment and obtain a dispersion.

[0101] S6013 dispersion liquid low pressure rotary evaporation to remove light

[0102] The temperature of the low-pressure rotary evaporation was 70° C., the vacuum degree was 20 kPa, the rotary evaporation time was 20 min, and the recovery rate of the light material obtained by the low-pressure rotary evaporation was 63.8 wt %, to obtain the base oil.

[0103] S602 lubricant preparation:

[0104] Base oil, 2 parts of graphene oxide, 0.1 parts of 2,4,6-tri-tert-butylphenol, and 1 part of isoleucine were mixed and placed in a vibration ball mill at an operating temperature of 70° C. for 0.5 h.

[0105] In order to characterize the lubricating performance of the lubricant, the following test was conducted: according to SH / T0204, the wear spot diameter was measured at 392N for 60min and was 0.33mm;

[0106] According to SH / T0202, the four-ball machine test was carried out and the P B 780N, P D 5400N;

[0107] The biodegradation rate was determined to be 80.3% according to CECL-33-93.

[0108] Comparative Example 4

[0109] S701 base oil preparation:

[0110] S7011 Hydrogenated vegetable oil and n-butanol mixture

[0111] 20 parts of hydrogenated vegetable oil (hydrogenated rapeseed oil) and 3 parts of n-butanol were mixed and heated to 50° C. to obtain a mixed solution.

[0112] S7012 disperses graphene oxide into the mixed liquid

[0113] A portion of the mixed liquid, generally about 1 / 3 of the total amount, is placed in a ball mill mixer with 1 part of graphene oxide, and then ball milled for 0.5 hours. The ball-milled product is then mixed with the remaining mixed liquid and stirred thoroughly to complete the graphene oxide dispersion treatment and obtain a dispersion.

[0114] S7013 dispersion liquid low pressure rotary evaporation to remove light

[0115] The temperature of the low-pressure rotary evaporation was 70° C., the vacuum degree was 20 kPa, the rotary evaporation time was 20 min, and the recovery rate of the light material obtained by the low-pressure rotary evaporation was 80.2 wt %, to obtain the base oil.

[0116] S702 lubricant preparation:

[0117] Base oil, 2 parts of graphene oxide, and 0.1 parts of 2,4,6-tri-tert-butylphenol were mixed and placed in a vibration ball mill at an operating temperature of 70° C. for 0.5 h.

[0118] In order to characterize the lubricating performance of the lubricant, the following test was conducted. According to SH / T0204, the wear spot diameter was measured to be 0.15 mm at 392 N for 60 min.

[0119] According to SH / T0202, the four-ball machine test was carried out and the P B 1044N, P D 6508N;

[0120] The biodegradation rate was determined to be 76.7% according to CECL-33-93.

[0121] In addition, it should be understood that after reading the above description of the present invention, those skilled in the art may make various changes or modifications to the present invention, and these equivalent forms also fall within the scope defined by the claims attached to this application.

Claims

1. A biodegradable lubricant, characterized in that In parts by mass, the raw material composition includes: The amino acid is isoleucine; The preparation method of the biodegradable lubricant comprises the steps of: S1, mixing hydrogenated vegetable oil and n-butanol to obtain a mixed solution; S2, mixing 10%-50% of the mixed solution with 1-2 parts by mass of graphene oxide and ball milling, mixing the ball-milled product with the remaining mixed solution and performing low-pressure rotary evaporation to obtain a base oil; S3, mixing the base oil with the amino acid, the antioxidant and the remaining graphene oxide to obtain the biodegradable lubricant.

2. The biodegradable lubricant according to claim 1, characterized in that The hydrogenated vegetable oil is hydrogenated rapeseed oil and / or hydrogenated soybean oil, which is obtained by hydrogenating rapeseed oil and / or soybean oil.

3. The biodegradable lubricant according to claim 1, characterized in that The antioxidant is antioxidant 246.

4. The method for preparing a biodegradable lubricant according to any one of claims 1 to 3, characterized in that: Including steps: S1, mixing hydrogenated vegetable oil and n-butanol to obtain a mixed solution; S2, mixing 10%-50% of the mixed solution with 1-2 parts by mass of graphene oxide and ball milling, mixing the ball-milled product with the remaining mixed solution and performing low-pressure rotary evaporation to obtain a base oil; S3, mixing the base oil with the amino acid, the antioxidant and the remaining graphene oxide to obtain the biodegradable lubricant.

5. The preparation method according to claim 4, characterized in that In step S1, the mixing temperature is 50-70°C.

6. The preparation method according to claim 4, characterized in that In step S2, the ball milling time is 0.5-1 h.

7. The preparation method according to claim 4, characterized in that In step S2, the temperature of the low-pressure rotary evaporation is 70-80°C, the time is 20-30 minutes, and the vacuum degree is 15-20 kPa.

8. The preparation method according to claim 4, characterized in that In step S3, the base oil, amino acid, antioxidant and remaining graphene oxide are mixed by vibration ball milling, the operating temperature does not exceed 70° C., and the time is 0.5-1 hour.

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