A lubricating grease for construction machines and a method for producing the same

Abstract

The application provides a special grease for engineering machinery and a preparation method thereof, and belongs to the technical field of greases. The grease is prepared from the following components in parts by weight: 75-90 parts of composite base oil, 7-10 parts of composite soap, 3-7 parts of composite anti-wear agent, 0.2-1.5 parts of composite antioxidant, 0.2-3 parts of alkaline stabilizer, 0.01-0.05 parts of rust inhibitor, 0.5-5 parts of water separating agent and 5-30PPm of defoaming agent. The self-made composite anti-wear agent and the low-amount rust inhibitor are used, so that the protection of the grease on the friction pair is more comprehensive, and the anti-wear performance is more excellent.

Description

TECHNICAL FIELD

[0001] The present application belongs to the technical field of lubricating grease, and particularly relates to a lubricating grease special for engineering machinery and a preparation method thereof. BACKGROUND

[0002] The lubricating grease is a kind of stable solid or semi-solid product composed of a thickening agent dispersed in a liquid lubricant, which is used for the friction part of machinery to play a role of lubrication and sealing. It is also used for the metal surface to play a role of filling gaps and rust prevention. It is mainly prepared from mineral oil (or synthetic lubricating oil) and a thickening agent, and is used for the lubrication between friction pairs which are not suitable for fluid lubrication. In order to meet different equipment and occasions, various lubricating greases have been produced over time. According to the thickening agent, the lubricating grease can be divided into two types of soap-based grease and non-soap-based grease. The thickening agent of the soap-based grease is commonly metal soaps such as lithium, sodium, calcium, aluminum and zinc, and also metal soaps such as potassium, barium, lead and manganese. The thickening agent of the non-soap-based grease is graphite, carbon black, asbestos and synthetic thickening agents (such as polyurea-based, bentonite). According to the use, the lubricating grease can be divided into two types of general lubricating grease and special lubricating grease, the former is used for general mechanical parts, and the latter is used for tractors, railway locomotives, ship machinery, oil drilling machinery, valves and the like. With the continuous development of equipment, various new requirements for the performance of the lubricating grease are put forward, and the performance of the original lubricating grease is difficult to meet the lubrication needs of new equipment and machinery.

[0003] The indoor equipment or the vehicle running on the road is relatively simple and easy to replace and maintain, while the engineering machinery type equipment working in the wild has frequent load changes and sudden impact load in the working process, so the impact load resistance, i.e. the wear resistance of the lubricating grease is particularly required.

[0004] The Chinese patent with the publication number CN104152219B discloses a lubricating grease special for engineering machinery and a preparation method thereof, which uses phosphoric acid trimethyl phenyl ester as an extreme pressure anti-wear agent. However, the phosphorus agent belongs to a low-load extreme pressure anti-wear agent, and the borate also belongs to an extreme pressure anti-wear agent. However, it needs to use calcium sulfonate as a dispersing aid to play a good effect, and the addition amount of the rust inhibitor is large. The rust inhibitor is preferentially adsorbed to the metal surface, thereby blocking the adsorption of the extreme pressure anti-wear agent and the metal, so that the extreme pressure anti-wear agent loses the effect.

[0005] The Chinese patent with the publication number CN104498137A discloses a lubricating grease special for excavators, which only uses phosphoric acid trimethyl phenyl ester or di-n-butyl phosphite of the phosphorus agent as an extreme pressure anti-wear agent. The single anti-wear agent can only solve the extreme pressure anti-wear under the low-load condition. In the production process of many lubricating greases, a large amount of acidic anti-wear agent is used to increase the wear resistance. Although the acidic anti-wear agent has good extreme pressure anti-wear performance, the acidic substance can seriously damage the alkaline soap in the use process of the lubricating grease, thereby affecting the protection of the lubricating grease to the friction pair. SUMMARY

[0006] To solve the problems in the background art, the application provides a special grease for engineering machinery and a preparation method thereof, which adopts self-made composite anti-wear agent and low-amount rust inhibitor, so as to ensure more comprehensive protection of the grease on the friction pair and more excellent wear resistance.

[0007] To achieve the above-mentioned purpose, in the first aspect, the application provides a special grease for engineering machinery, which adopts the following technical scheme:

[0008] The special grease for engineering machinery is prepared from the following components in parts by weight: 75-90 parts of composite base oil, 7-10 parts of composite soap, 3-7 parts of composite anti-wear agent, 0.2-1.5 parts of composite antioxidant, 0.2-3 parts of alkaline stabilizer, 0.01-0.05 parts of rust inhibitor, 0.5-5 parts of water separating agent and 5-30 ppm of defoaming agent.

[0009] All the components are in parts by weight, and the preparation method of the composite anti-wear agent is as follows: 200 parts of water are added to a reaction kettle, stirring is started, and 40 parts of boric acid are added, and heated to 50-90℃; after complete dissolution, 24 parts of 1,8-diazabicyclo-dicyclo(5,4,0)-7-undecene, 6 parts of triethylamine and 8 parts of N,N-dimethylaniline are sequentially added, and reacted for 1.2 hours; 0.8 parts of titanate is added, and heated to 70-90℃ under stirring, and vacuum dehydration; after complete dehydration, 7.5 parts of trimethylphenyl phosphite, 5 parts of sulfur-phosphorus acid nitrogen derivative, 20 parts of triphenyl phosphite and 30 parts of organic metal framework material are added, and mixed uniformly.

[0010] Preferably, the preparation method of the organic metal framework material is as follows:

[0011] A1, 0.1 mol of SnCl2 is dissolved in 20 ml of deionized water to obtain an aqueous SnCl2 solution, 0.24 mmol of 2,3,6,7,10,11-hexamino triphenyl hexa hydrochloride is dissolved in 40 ml of deionized water to obtain a 2,3,6,7,10,11-hexamino triphenyl hexa hydrochloride solution, and the two are mixed uniformly to obtain a mixed solution;

[0012] A2, 1.2 ml of ammonia water with a concentration of 14 mol / L is added dropwise to the mixed solution obtained in A1, stirring is performed for 3 hours, the reaction product is centrifuged and separated, the solid product is washed with deionized water and ethanol for 2 times respectively, and then dried, to obtain the organic metal framework material.

[0013] Preferably, the preparation method of the rust inhibitor is as follows: 30 parts of barium dinonyl naphthalene sulfonate, 40 parts of alkyl phosphoric acid imidazoline amine and 20 parts of N-oleoyl sarcosine octadecylamine are sequentially put into a reaction kettle, heated to 60℃, and mixed uniformly, to obtain the rust inhibitor.

[0014] Preferably, the water separating agent comprises the following components in parts by weight: polyisobutylene 3.5 parts and perfluoropolyether 0.8 parts.

[0015] Preferably, the composite base oil comprises the following components in parts by weight: naphthenic mineral oil 50 parts, alkyl naphthalene 17.5 parts and polyalphaolefin 20 parts.

[0016] Preferably, the preparation method of the composite soap comprises the following steps in parts by weight: adding water 200 parts into an autoclave, starting stirring, then adding calcium oxide 10-40 parts; after the reaction is completed, heating to 60-90℃, then adding sulfonic acid 15-25 parts, reacting for 20-30 minutes; then adding acetic acid 1-5 parts, sebacic acid 5-10 parts and dodecanol hydroxystearic acid 5-10 parts in sequence, mixing for 10-30 minutes; then adding lithium hydroxide 5-10 parts, closing the autoclave, heating to 130-170℃, reacting for 1-3 hours, opening the exhaust valve, slowly draining water, and dehydrating to obtain the composite soap.

[0017] Preferably, the sulfonic acid is a long-chain alkyl sulfonic acid containing 12 carbons or more.

[0018] Preferably, the preparation method of the composite antioxidant comprises the following steps in parts by weight: adding 2,6-di-tert-butyl-p-cresol 45 parts, diphenylamine 20 parts and benzotriazole 2 parts into a reaction kettle in sequence, heating to 50-70℃, and mixing uniformly to obtain the composite antioxidant.

[0019] Preferably, the basic stabilizer comprises the following components in parts by weight: sulfided calcium alkyl phenate 0.6 parts and polyisobutylene butadiene imine 2 parts.

[0020] In the second aspect, the present application provides a preparation method of the special grease for construction machinery, which adopts the following technical scheme:

[0021] The preparation method of the special grease for construction machinery is used for preparing the special grease for construction machinery, and comprises the following steps:

[0022] S1, first, the composite base oil is put into a reaction kettle, then the composite anti-wear agent, the composite antioxidant, the anti-rust agent and the defoaming agent are added and uniformly mixed to obtain a mixture A;

[0023] S2, the composite soap is put into an autoclave, then 15-25% of the mixture A is added, the temperature is raised to 210-240℃, and the temperature is kept for 5-15 minutes; cooling water is introduced into the autoclave, the temperature of the cooling water is controlled to be between -20℃ and -10℃, and the remaining mixture A is pumped into the autoclave; after the temperature is lowered to 60-90℃ under stirring, the water separating agent and the basic stabilizer are added and uniformly stirred; then the mixture is uniformly filtered and vacuum degassed to obtain the special grease for construction machinery.

[0024] The present application has the following beneficial effects:

[0025] 1. The rust inhibitor is added in the lowest amount to ensure the rust prevention performance, and the occupation of the metal surface by the composite anti-wear agent is avoided.

[0026] The self-made composite anti-wear agent reasonably matches phosphorus, sulfur and nitrogen anti-wear agents, which can meet the needs of low-load extreme pressure and anti-wear, and can also meet the needs of medium-load and heavy-load extreme pressure and anti-wear, and has extremely high anti-sintering load, and can more comprehensively protect the friction pair, so that the anti-wear performance is more excellent.

[0027] The self-made organic metal framework material is a two-dimensional nanomaterial with a layered structure similar to that of graphene. The electrons of tin and nitrogen elements in the material are redistributed between and within the double layers of the organic metal framework material, thereby changing the interaction energy between the layers. This energy change can effectively control the tribological behavior between the layers, reduce the friction force, and improve the anti-wear performance.

[0028] Although the amount of the rust inhibitor is small, it has a very good synergistic effect on the rust prevention of the metal in cooperation with the alkaline stabilizer and the water separating agent. The three components achieve more excellent rust prevention performance.

[0029] 2. The composite soap used in the present application allows long and short fibers to interlace, thereby enhancing the elasticity and strength of the spatial net structure of the soap fibers. The change rate of the working cone penetration is less than 4%, and the stability is better. The addition of the alkaline stabilizer can neutralize the acidic substances generated by the oxidation of the lubricating grease during use. The addition of the composite antioxidant improves the oxidation resistance of the lubricating grease, prolongs the service life of the lubricating grease, and reduces the frequency of lubricating grease injection.

[0030] 3. The composite base oil is composed of naphthenic mineral oil, alkyl naphthalene and poly-alpha olefin. The naphthenic base oil and alkyl naphthalene can swell the rubber parts, while the poly-alpha olefin can shrink the rubber parts. The mutual cooperation of the two can make the swelling and shrinking of the rubber parts reach 1:1, thereby prolonging the service life of the joint rubber sealing parts. The good performance of the sealing parts can reduce the damage of water, dust and harmful gases to the lubricating grease, thereby prolonging the service life of the lubricating grease. BRIEF DESCRIPTION OF DRAWINGS

[0031] Figure 1 Trend graph of rust grade of the lubricating greases of Examples 1-5 and Comparative Examples 1-12;

[0032] Figure 2 Trend graph of wear resistance of the lubricating greases of Examples 1-5 and Comparative Examples 1-12;

[0033] Figure 3Trend chart of grease working cone penetration of Example 1-5 and Comparative Example 13-14;

[0034] Figure 4 Trend chart of prolonged working cone penetration change rate of Example 1-5 and Comparative Example 13-14 grease. DETAILED DESCRIPTION

[0035] The application will be further described in detail below in conjunction with examples.

[0036] The raw materials of the examples and comparative examples of the application are all ordinary commercial products except for special instructions.

[0037] Example 1

[0038] Preparation of the organic metal framework material: A1, 0.1 mol SnCl2 was dissolved in 20 ml of deionized water to obtain a SnCl2 aqueous solution, 0.24 mmol 2,3,6,7,10,11-hexamino triphenyl hexa hydrochloride was dissolved in 40 ml of deionized water to obtain a 2,3,6,7,10,11-hexamino triphenyl hexa hydrochloride solution, and the two were mixed uniformly to obtain a mixed solution; A2, 1.2 ml of ammonia water with a concentration of 14 mol / L was added dropwise into the mixed solution obtained in A1, and stirred for 3 h, the reaction product was centrifuged and separated, the solid product was washed with deionized water and ethanol for 2 times respectively, and then dried, thereby obtaining the organic metal framework material.

[0039] Preparation of the composite anti-wear agent (components are by weight fraction): 200 parts of water was added into a reaction kettle, stirring was started, and 40 parts of boric acid was added, and heated to 70℃; after complete dissolution, 24 parts of 1,8-diazabicyclo-dicyclo(5,4,0)-7-undecene, 6 parts of triethylamine and 8 parts of N,N-dimethyl aniline were sequentially added, and reacted for 1.2 hours; 0.8 parts of titanate was added, and heated to 80℃ under stirring, and vacuum dehydration; after the dehydration was completed, 7.5 parts of trimethyl phenyl phosphite, 5 parts of sulfur phosphorus acid nitrogen derivative, 20 parts of triphenyl phosphite and 30 parts of the organic metal framework material were added, and mixed uniformly, thereby obtaining the composite anti-wear agent.

[0040] Preparation of the rust inhibitor (components are by weight fraction): 30 parts of barium dinonyl naphthalene sulfonate, 40 parts of alkyl imidazoline phosphoric acid amine and 20 parts of N-oleoyl sarcosine octadecylamine were sequentially added into a reaction kettle, heated to 60℃, and mixed uniformly, thereby obtaining the rust inhibitor.

[0041] Preparation of the composite antioxidant (components are by weight fraction): 45 parts of 2,6-di-tert-butyl-p-cresol, 20 parts of diphenylamine and 2 parts of benzotriazole were sequentially added into a reaction kettle, heated to 60℃, and mixed uniformly, thereby obtaining the composite antioxidant.

[0042] Water separator: By weight, it consists of two components: 3.5 parts polyisobutylene and 0.8 parts perfluoropolyether.

[0043] Alkaline stabilizer: by weight, it comprises two components: 0.6 parts of calcium alkylphenol sulfide and 2 parts of polyisobutylene butadiene imide.

[0044] Complex base oil: by weight, it comprises three components: 50 parts naphthenic mineral oil, 17.5 parts alkyl naphthalene, and 20 parts polyalphaolefin.

[0045] Defoamer: Mix dimethyl silicone oil and kerosene in a ratio of 1.5:10 and use evenly.

[0046] Preparation of compound soap (components by weight): Add 200 parts water to a high-pressure reactor, start stirring, then add 25 parts calcium oxide; after the reaction is complete, heat to 75℃, then add 20 parts sulfonic acid and react for 25 minutes; then add 3 parts acetic acid, 7.5 parts sebacic acid, and 7.5 parts dodecyl stearic acid in sequence, mix for 20 minutes; then add 7.5 parts lithium hydroxide, seal the high-pressure reactor, heat to 150℃, react for 2 hours, open the exhaust valve, slowly drain the water, and dehydrate to obtain the compound soap. The sulfonic acid (R-SO3H) is a long-chain alkyl sulfonic acid containing more than 12 carbon atoms, specifically dodecyl sulfonic acid.

[0047] Preparation of special lubricating grease for construction machinery:

[0048] By weight, this grease is prepared from the following components in parts by weight: 82 parts of complex base oil, 8.5 parts of complex soap, 5 parts of complex anti-wear agent, 0.8 parts of complex antioxidant, 1.6 parts of alkaline stabilizer, 0.03 parts of rust inhibitor, 3.5 parts of water separator and 17 ppm of defoamer.

[0049] The specific preparation steps for this lubricating grease are as follows:

[0050] S1. First, add the composite base oil into the reaction vessel, then add the composite anti-wear agent, composite antioxidant, rust inhibitor and defoamer, mix evenly to obtain mixture A;

[0051] S2. Add the compound soap to the autoclave, then add 20% of mixture A, rapidly heat to 225℃, keep warm for 10 minutes, introduce cooling water into the autoclave, and control the temperature of the cooling water at about -15℃. At the same time, pump the remaining mixture A into the autoclave, stir and cool down to 75℃, then add the water separator and alkaline stabilizer, stir evenly, filter homogenize and degas under vacuum to obtain the special lubricating grease for engineering machinery.

[0052] Example 2

[0053] The only difference between this embodiment and Embodiment 1 is that:

[0054] The special grease for engineering machinery is prepared from the following components in parts by weight: 75 parts of the complex base oil, 7 parts of the complex soap, 3 parts of the complex anti-wear agent, 0.2 parts of the complex antioxidant, 0.2 parts of the basic stabilizer, 0.01 parts of the anti-rust agent, 0.5 parts of the water separating agent and 5PPm of the defoaming agent.

[0055] The other raw materials, the preparation method of the grease and the component ratio are the same as those in Example 1.

[0056] Example 3

[0057] The difference between this example and Example 1 is only that:

[0058] The special grease for engineering machinery is prepared from the following components in parts by weight: 90 parts of the complex base oil, 10 parts of the complex soap, 7 parts of the complex anti-wear agent, 1.5 parts of the complex antioxidant, 3 parts of the basic stabilizer, 0.05 parts of the anti-rust agent, 5 parts of the water separating agent and 30PPm of the defoaming agent.

[0059] The other raw materials, the preparation method of the grease and the component ratio are the same as those in Example 1.

[0060] Example 4

[0061] The difference between this example and Example 1 is only that:

[0062] The special grease for engineering machinery is prepared from the following components in parts by weight: 90 parts of the complex base oil, 10 parts of the complex soap, 3 parts of the complex anti-wear agent, 0.2 parts of the complex antioxidant, 0.2 parts of the basic stabilizer, 0.05 parts of the anti-rust agent, 0.5 parts of the water separating agent and 5PPm of the defoaming agent.

[0063] The other raw materials, the preparation method of the grease and the component ratio are the same as those in Example 1.

[0064] Example 5

[0065] The difference between this example and Example 1 is only that:

[0066] The special grease for engineering machinery is prepared from the following components in parts by weight: 75 parts of the complex base oil, 7 parts of the complex soap, 7 parts of the complex anti-wear agent, 1.5 parts of the complex antioxidant, 3 parts of the basic stabilizer, 0.05 parts of the anti-rust agent, 5 parts of the water separating agent and 28PPm of the defoaming agent.

[0067] The other raw materials, the preparation method of the grease and the component ratio are the same as those in Example 1.

[0068] Comparative Example 1

[0069] The difference between the present comparative example and Example 1 is only that:

[0070] The addition amount of the rust preventive exceeds the protection scope of the present application.

[0071] Specifically, the special lubricating grease for engineering machinery is prepared from the following components by weight fraction: 82 parts of composite base oil, 8.5 parts of composite soap, 5 parts of composite anti-wear agent, 0.8 parts of composite antioxidant, 1.6 parts of basic stabilizer, 0.06 parts of rust preventive, 3.5 parts of water separating agent, and 17 PPm of defoaming agent.

[0072] The other raw materials, the preparation method of the lubricating grease, and the component ratio are the same as those of Example 1.

[0073] Comparative Example 2

[0074] The difference between the present comparative example and Example 1 is only that:

[0075] The addition amount of the rust preventive exceeds the protection scope of the present application.

[0076] Specifically, the special lubricating grease for engineering machinery is prepared from the following components by weight fraction: 82 parts of composite base oil, 8.5 parts of composite soap, 5 parts of composite anti-wear agent, 0.8 parts of composite antioxidant, 1.6 parts of basic stabilizer, 0.08 parts of rust preventive, 3.5 parts of water separating agent, and 17 PPm of defoaming agent.

[0077] The other raw materials, the preparation method of the lubricating grease, and the component ratio are the same as those of Example 1.

[0078] Comparative Example 3

[0079] The difference between the present comparative example and Example 1 is only that:

[0080] The addition amount of the rust preventive is lower than the protection scope of the present application.

[0081] Specifically, the special lubricating grease for engineering machinery is prepared from the following components by weight fraction: 82 parts of composite base oil, 8.5 parts of composite soap, 5 parts of composite anti-wear agent, 0.8 parts of composite antioxidant, 1.6 parts of basic stabilizer, 0.009 parts of rust preventive, 3.5 parts of water separating agent, and 17 PPm of defoaming agent.

[0082] The other raw materials, the preparation method of the lubricating grease, and the component ratio are the same as those of Example 1.

[0083] Comparative Example 4

[0084] The difference between the present comparative example and Example 1 is only that:

[0085] The addition amount of the rust preventive is lower than the protection scope of the present application.

[0086] Specifically, the special grease for engineering machinery is prepared from the following components by weight fraction: 82 parts of compound base oil, 8.5 parts of compound soap, 5 parts of compound anti-wear agent, 0.8 parts of compound antioxidant, 1.6 parts of basic stabilizer, 0.007 parts of anti-rust agent, 3.5 parts of water separating agent and 17PPm of defoaming agent.

[0087] The other raw materials, the preparation method of the grease and the component ratio are the same as those in Example 1.

[0088] Comparative Example 5

[0089] The difference between the present comparative example and Example 1 is only that:

[0090] The addition amount of the water separating agent is lower than the protection scope of the present application.

[0091] Specifically, the special grease for engineering machinery is prepared from the following components by weight fraction: 82 parts of compound base oil, 8.5 parts of compound soap, 5 parts of compound anti-wear agent, 0.8 parts of compound antioxidant, 1.6 parts of basic stabilizer, 0.03 parts of anti-rust agent, 0.4 parts of water separating agent and 17PPm of defoaming agent.

[0092] The other raw materials, the preparation method of the grease and the component ratio are the same as those in Example 1.

[0093] Comparative Example 6

[0094] The difference between the present comparative example and Example 1 is only that:

[0095] The water separating agent is not contained in the raw material components.

[0096] Specifically, the special grease for engineering machinery is prepared from the following components by weight fraction: 82 parts of compound base oil, 8.5 parts of compound soap, 5 parts of compound anti-wear agent, 0.8 parts of compound antioxidant, 1.6 parts of basic stabilizer, 0.03 parts of anti-rust agent and 17PPm of defoaming agent.

[0097] The other raw materials, the preparation method of the grease and the component ratio are the same as those in Example 1.

[0098] Comparative Example 7

[0099] The difference between the present comparative example and Example 1 is only that:

[0100] The basic stabilizer is not contained in the raw material components.

[0101] Specifically, the special grease for engineering machinery is prepared from the following components by weight fraction: 82 parts of compound base oil, 8.5 parts of compound soap, 5 parts of compound anti-wear agent, 0.8 parts of compound antioxidant, 0.03 parts of anti-rust agent, 0.4 parts of water separating agent and 17PPm of defoaming agent.

[0102] The other raw materials, the preparation method of the grease and the component ratio are the same as those in Example 1.

[0103] Comparative Example 8

[0104] The difference between the present comparative example and Example 1 is only that:

[0105] The raw material components do not contain a water separating agent and an alkaline stabilizer.

[0106] Specifically, the special grease for engineering machinery is prepared from the following components by weight fraction: 82 parts of composite base oil, 8.5 parts of composite soap, 5 parts of composite anti-wear agent, 0.8 parts of composite antioxidant, 0.03 parts of anti-rust agent, and 17PPm of defoaming agent.

[0107] The other raw materials, the preparation method of the grease and the component ratio are the same as those in Example 1.

[0108] Comparative Example 9

[0109] The difference between the present comparative example and Example 1 is only that:

[0110] The raw material components for preparing the composite anti-wear agent do not contain an organic metal framework material.

[0111] Specifically, the composite anti-wear agent (components by weight fraction) is prepared as follows: 200 parts of water is added to a reaction kettle, stirring is started, and 40 parts of boric acid is added, and heated to 70°C; after complete dissolution, 24 parts of 1,8-diazabicyclo-dicyclo(5,4,0)-7-undecene, 6 parts of triethylamine, and 8 parts of N,N-dimethylaniline are sequentially added, and reacted for 1.2 hours; 0.8 parts of titanate is added, and heated to 80°C under stirring, and vacuum dehydration; after complete dehydration, 7.5 parts of trimethylphenyl phosphite, 5 parts of a nitrogen-containing derivative of sulfur phosphoric acid, and 20 parts of triphenyl phosphite are added, and mixed uniformly, to obtain the composite anti-wear agent.

[0112] The other raw materials, the preparation method of the grease and the component ratio are the same as those in Example 1.

[0113] Comparative Example 10

[0114] The difference between the present comparative example and Example 1 is only that:

[0115] The raw material components for preparing the composite anti-wear agent do not contain a nitrogen-containing derivative of sulfur phosphoric acid and an organic metal framework material.

[0116] Specifically, the composite anti-wear agent is prepared (components are by weight parts) : water 200 parts is added into a reaction kettle, stirring is started, boric acid 40 parts is added, heating to 70 DEG C; after complete dissolution, 1,8-diazabicyclo-dicyclo(5,4,0)-7-undecene 24 parts, triethylamine 6 parts and N,N-dimethyl aniline 8 parts are added in sequence, reaction 1.2 hours; titanium ester 0.8 parts is added, temperature is raised to 80 DEG C under stirring, vacuum dehydration; after complete dehydration, trimethylphenyl phosphite 7.5 parts and triphenyl phosphite 20 parts are added, mixed uniformly, the composite anti-wear agent is obtained.

[0117] The other raw materials, the preparation method and component ratio of the grease are same as those of Example 1.

[0118] Comparative Example 11

[0119] The difference between the present comparative example and Example 1 is only that:

[0120] In the raw material components for preparing the composite anti-wear agent, the sulfur-phosphorus acid nitrogen-containing derivative, triphenyl phosphite and the organic metal framework material are not contained.

[0121] Specifically, the composite anti-wear agent is prepared (components are by weight parts) : water 200 parts is added into a reaction kettle, stirring is started, boric acid 40 parts is added, heating to 70 DEG C; after complete dissolution, 1,8-diazabicyclo-dicyclo(5,4,0)-7-undecene 24 parts, triethylamine 6 parts and N,N-dimethyl aniline 8 parts are added in sequence, reaction 1.2 hours; titanium ester 0.8 parts is added, temperature is raised to 80 DEG C under stirring, vacuum dehydration; after complete dehydration, trimethylphenyl phosphite 7.5 parts and triphenyl phosphite 20 parts are added, mixed uniformly, the composite anti-wear agent is obtained.

[0122] The other raw materials, the preparation method and component ratio of the grease are same as those of Example 1.

[0123] Comparative Example 12

[0124] The difference between the present comparative example and Example 1 is only that:

[0125] A single anti-wear agent is used, specifically trimethylphenyl phosphite.

[0126] The other raw materials, the preparation method and component ratio of the grease are same as those of Example 1.

[0127] Comparative Example 13

[0128] The difference between the present comparative example and Example 1 is only that:

[0129] In the raw material components for preparing the composite soap, the sulfonic acid is specifically selected as methyl sulfonic acid.

[0130] Specifically, the composite soap is prepared (the components are by weight fraction) : in the autoclave, 200 parts of water is added, and stirring is started, then 25 parts of calcium oxide is added; after the reaction is completed, heating is performed to 75 DEG C, then 20 parts of methyl sulfonic acid is added, and the reaction is performed for 25 minutes; then 3 parts of acetic acid, 7.5 parts of sebacic acid and 7.5 parts of dodecanol stearic acid are sequentially added, and mixing is performed for 20 minutes; then 7.5 parts of lithium hydroxide is added, the autoclave is closed, heating is performed to 150 DEG C, and the reaction is performed for 2 hours, then the exhaust valve is opened, and the water is slowly drained, and dehydration is performed, and the composite soap is obtained.

[0131] Comparative Example 14

[0132] The difference between the present comparative example and Example 1 is only that:

[0133] In the raw material components for preparing the composite soap, the sulfonic acid is not contained.

[0134] Specifically, the composite soap is prepared (the components are by weight fraction) : in the autoclave, 200 parts of water is added, and stirring is started, then 25 parts of calcium oxide is added; after the reaction is completed, heating is performed to 75 DEG C, then 20 parts of methyl sulfonic acid is added, and the reaction is performed for 25 minutes; then 3 parts of acetic acid, 7.5 parts of sebacic acid and 7.5 parts of dodecanol stearic acid are sequentially added, and mixing is performed for 20 minutes; then 7.5 parts of lithium hydroxide is added, the autoclave is closed, heating is performed to 150 DEG C, and the reaction is performed for 2 hours, then the exhaust valve is opened, and the water is slowly drained, and dehydration is performed, and the composite soap is obtained.

[0135] Test Example 1

[0136] Test item: 1, determination of the rust-proof performance of the lubricating grease; according to the standard: SH / T 0700-2000;

[0137] 2, determination of the anti-wear performance of the lubricating grease; according to the standard: SH / T 0204-1992 (2004) ;

[0138] Test object: Examples 1-5 and Comparative Examples 1-12;

[0139] Test result: see Table 1.

[0140] Table 1

[0141]

[0142] Result analysis: the data in Table 1 is analyzed, and it can be known from Figures 1-2 that, by using the self-prepared rust-proof agent, under the premise of ensuring the rust-proof performance, the lowest range of the adding amount of the rust-proof agent is selected, the rust-proof agent can avoid affecting the occupation of the composite anti-wear agent on the metal surface, and the anti-wear performance is not affected; the composite anti-wear agent reasonably matches the phosphorus, sulfur and nitrogen agents, the protection of the friction pair is more comprehensive, and the anti-wear performance is more excellent; although the adding amount of the rust-proof agent is small, the rust-proof agent has a very good synergistic effect on the metal under the cooperation of the alkaline stabilizer and the water separating agent, and the three agents synergistically produce more excellent rust-proof effect.

[0143] Test Example 2

[0144] Test item: grease cone penetration determination; according to standard: GB / T 269-1991;

[0145] Test object: examples 1-5 and comparative examples 13-14;

[0146] Test results: see table 2.

[0147] Table 2

[0148] Working cone penetration / 0.1 mm Extended working cone penetration rate of change / % Example 1 277 3.2 Example 2 275 3.1 Example 3 280 3.4 Example 4 278 3.7 Example 5 279 3.2 Comparative Example 13 283 5.1 Comparative Example 14 285 5.7

[0149] Result analysis: analyze table 2 data and combine Figures 3-4 It can be known that, by using the self-made composite soap, the long and short fibers are matched with each other, the elasticity and strength of the space net rack structure of the soap fiber are enhanced, the change rate of the working cone penetration is less than 4%, and the stability is more excellent.

[0150] In addition, it should be noted that each specific technical feature described in the above specific embodiments can be combined in any appropriate manner without contradiction, and in order to avoid unnecessary repetition, various possible combinations are not described again by the present application.

[0151] In addition, various different embodiments of the present application can also be combined in any manner, as long as they do not deviate from the idea of the present application, and they should also be considered as disclosed by the present application.

Claims

1. A grease for construction machines, characterized in that, It is prepared from the following components by weight fraction: 75-90 parts of complex base oil, 7-10 parts of complex soap, 3-7 parts of complex anti-wear agent, 0.2-1.5 parts of complex antioxidant, 0.2-3 parts of basic stabilizer, 0.01-0.05 parts of anti-rust agent, 0.5-5 parts of water separating agent and 5-30PPm of defoaming agent; All components are calculated by weight fraction, and the preparation method of the complex anti-wear agent is as follows: 200 parts of water are added to a reaction kettle, stirring is started, 40 parts of boric acid are added, and heating is started to 50-90℃; After complete dissolution, 24 parts of 1,8-diazabicyclo-dicyclo(5,4,0)-7-undecene, 6 parts of triethylamine and 8 parts of N,N-dimethyl aniline are added in sequence, and the reaction is carried out for 1.2 hours; 0.8 parts of titanate are added, and the temperature is raised to 70-90℃ under stirring, and vacuum dehydration is carried out; After dehydration is completed, 7.5 parts of trimethylphenyl phosphite, 5 parts of sulfur phosphorus acid containing nitrogen derivative, 20 parts of triphenyl phosphite and 30 parts of organic metal framework material are added, and mixing is carried out evenly to obtain the complex anti-wear agent; The water separating agent comprises the following components by weight fraction: 3.5 parts of polyisobutylene and 0.8 parts of perfluoropolyether; All components are calculated by weight fraction, and the preparation method of the complex soap is as follows: 200 parts of water are added to a high-pressure kettle, stirring is started, and 10-40 parts of calcium oxide are added; After the reaction is completed, heating is started to 60-90℃, 15-25 parts of sulfonic acid are added, and the reaction is carried out for 20-30 minutes; 1-5 parts of acetic acid, 5-10 parts of decanedioic acid and 5-10 parts of dodecahydroxystearic acid are added in sequence, and mixing is carried out for 10-30 minutes; 5-10 parts of lithium hydroxide are added, the high-pressure kettle is closed, heating is started to 130-170℃, the reaction is carried out for 1-3 hours, the exhaust valve is opened, and the water is slowly discharged, and dehydration is carried out to obtain the complex soap; The sulfonic acid is a long-chain alkyl sulfonic acid containing 12 carbons or more; The basic stabilizer comprises the following components by weight fraction: 0.6 parts of sulfided alkyl phenol calcium and 2 parts of polyisobutylene butadiene imine.

2. The special grease for construction machinery according to claim 1, characterized by, The preparation method of the organic metal framework material is as follows: A1, 0.1 mol SnCl2 is dissolved in 20 ml of deionized water to obtain a SnCl2 aqueous solution, 0.24 mmol 2,3,6,7,10,11-hexaaminotriphenyl hexa hydrochloride is dissolved in 40 ml of deionized water to obtain a 2,3,6,7,10,11-hexaaminotriphenyl hexa hydrochloride solution, and the two are mixed evenly to obtain a mixed solution; A2, 1.2 ml of ammonia water with a concentration of 14 mol / L is added dropwise to the mixed solution obtained in A1, stirring is carried out for 3 hours, the reaction product is centrifuged and separated, the solid product is washed with deionized water and ethanol for 2 times respectively, and then dried to obtain the organic metal framework material.

3. The special grease for construction machinery according to claim 1, characterized by, The preparation method of the anti-rust agent is as follows: 30 parts of barium dinonylnaphthalene sulfonate, 40 parts of alkyl phosphoric acid imidazoline amine and 20 parts of N-oleoyl sarcosine octadecylamine are sequentially put into a reaction kettle, heating is started to 60℃, and mixing is carried out evenly to obtain the anti-rust agent.

4. The special grease for construction machinery according to claim 1, characterized by, The complex base oil comprises the following components by weight fraction: 50 parts of naphthenic mineral oil, 17.5 parts of alkyl naphthalene and 20 parts of polyalphaolefin.

5. The special grease for construction machinery according to claim 1, characterized by, The composite antioxidant is prepared by adding 45 parts of 2,6-di-tert-butyl-p-cresol, 20 parts of diphenylamine and 2 parts of benzotriazole into a reaction kettle in sequence, and heating to 50-70 DEG C to mix uniformly.

6. A method of preparing a lubricating grease for construction machines, characterized by, The method for preparing the special grease for engineering machinery as claimed in any one of claims 1-5 comprises the following steps: S1, first put the composite base oil into the reaction kettle, then add the composite anti-wear agent, the composite antioxidant, the anti-rust agent and the defoaming agent, mix uniformly to obtain a mixture A; S2, put the composite soap into the autoclave, then add 15-25% of the mixture A, heat to 210-240 DEG C, keep warm for 5-15 minutes, let the cooling water pass through the autoclave, control the temperature of the cooling water at-20 DEG C to-10 DEG C, at the same time, pump the remaining mixture A into the autoclave, stir to cool to 60-90 DEG C, then add the water separating agent and the alkaline stabilizer, stir uniformly, homogenize, filter and vacuum degas to obtain the special grease for engineering machinery.

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