Low-thickening-agent composite calcium sulfonate lubricating grease and preparation method thereof

Abstract

The invention discloses low-thickening-agent composite calcium sulfonate lubricating grease and a preparation method thereof, and relates to the technical field of composite calcium sulfonate lubricating grease preparation, the low-thickening-agent composite calcium sulfonate lubricating grease comprises, by weight, 55-65 parts of base oil, 20-30 parts of a thickening agent and 1-8 parts of an anti-wear reagent at extreme pressure, the base oil is mineral oil and synthetic oil including 150BS, 500N, poly-alpha olefin and mixed oil of 150BS, 500N and poly-alpha olefin; according to the low-thickening-agent composite calcium sulfonate lubricating grease and the preparation method thereof, the proportion of long-chain-line sulfonic acid and heavy alkyl benzene sulfonic acid in high-base-number synthetic calcium sulfonate and the product index are equivalent to those of foreign imported products, special functional additives and high polymer materials are added, and the colloid structure of the system is strictly controlled; in the production process, flammable and explosive phase inversion agents such as isopropanol and n-butyl alcohol which pollute the environment do not need to be added, and the product belongs to an environment-friendly product.

Description

Technical Field

[0001] The invention relates to the technical field of preparation of composite calcium sulfonate grease, and in particular to a low-thickening agent composite calcium sulfonate grease and a preparation method thereof. Background Art

[0002] Composite calcium sulfonate grease combines the performance advantages of composite lithium grease, polyurea grease, composite aluminum grease and composite calcium grease. It is a high-quality grease that integrates excellent properties such as extreme pressure, wear resistance, high and low temperature resistance, mechanical stability, colloid stability, and water resistance. It is called a grease with a new concept; and because it does not contain heavy metals and other functional additives that are harmful to the environment, it is also called an environmentally friendly grease. Composite calcium sulfonate is mostly used in harsh environments such as dusty and water-corrosive equipment in industries such as steel, metallurgy, and seawater transportation. This requires the grease to have multiple properties such as high temperature resistance, water resistance, extreme pressure resistance, and corrosion resistance.

[0003] At present, lithium-based greases are mainly used in the domestic market, and composite calcium sulfonate greases account for 1%. However, with the continuous rise in lithium ore prices, the comprehensive performance of composite calcium sulfonate greases will continue to improve, which will bring composite calcium sulfonate greases a good opportunity for development. The key to the preparation of composite calcium sulfonate greases is to convert non-Newtonian high-base calcium sulfonate into calcium sulfonate with a calcite structure. The mechanism of the conversion process is relatively complex. If the conversion is not complete, the grease will become soft and its performance will be unstable. Therefore, continuous optimization of the conversion method and optimization of the conversion agent are the focus of attention of technicians in this industry. In addition, the addition of suitable calcium borate soap and fatty acid soap cannot be ignored. Due to the immaturity of these raw materials, formulas and production methods, large-scale production has not yet been formed. In relatively harsh environments, the composite calcium sulfonate greases used are mostly imported from abroad.

[0004] At present, there are many technical documents at home and abroad that study the preparation method of composite calcium sulfonate grease. Domestic patents CN101153239A and CN10131964A change different raw material ratios and the order of converter feeding in the traditional process, and can prepare grease of the same consistency with less thickener content, but it has high requirements for raw materials, complex processes, and high conversion temperatures; the grease prepared by patent US4597800 has good high temperature performance and shear stability, but due to the excessively high thickener content, it has poor pumpability and high cost; CN1414076A adds organic urea to improve the grease, but the production process is more complicated, the production time is longer, and the raw materials are toxic, which is not conducive to production. The present invention uses 150BS and PAO6 as base oils, high-base environmentally friendly composite calcium as a thickener, 12-alkylbenzene sulfonic acid, glacial acetic acid and 12-hydroxystearic acid as conversion agents, boric acid, calcium hydroxide and 12-hydroxystearic acid as saponifiers, and additives such as nano calcium carbonate, calcium acetate and dioctyl zinc salt of sulfur and phosphorus. The prepared grease has a dropping point greater than 320°C, and has good low-temperature performance at -40°C, can be used under high temperature conditions and extremely cold conditions, has good water resistance, and has an extreme pressure and anti-wear PD of up to 500kg, which prolongs the life of the equipment, and the preparation process does not cause pollution to the environment. The thickener content required in the preparation process is low, the cost is low, the process is simple, the heating temperature is not high, and the economy is good.

[0005] At the same time, in the current preparation and production process of composite calcium sulfonate-based grease, it is necessary to stir and mix various raw materials. During the preparation reaction process, a stirring rod is usually used for stirring and mixing. During the mixing process, the raw materials cannot be fully fused, resulting in poor mixing reaction effect and long reaction time, resulting in low preparation quality and low preparation efficiency of composite calcium sulfonate-based grease. Summary of the invention

[0006] The object of the present invention is to provide a low-thickening agent composite calcium sulfonate grease and a preparation method thereof, so as to solve the deficiencies in the above-mentioned background technology.

[0007] The purpose of the present invention can be achieved through the following technical solutions:

[0008] A low-thickener composite calcium sulfonate grease, characterized by comprising the following parts by weight:

[0009] The invention comprises 55-65 parts of base oil, 20-30 parts of thickener and 1-8 parts of extreme pressure anti-wear agent. The base oil is mineral oil and synthetic oil, including 150BS, 500N, polyalphaolefin and mixed oil of 150BS, 500N and polyalphaolefin; the thickener comprises high-base calcium sulfonate, a converter and a saponifier, the converter comprises 12-alkylbenzene sulfonic acid, 12-hydroxystearic acid and glacial acetic acid, the saponifier comprises 12-hydroxystearic acid, boric acid and calcium hydroxide; the extreme pressure anti-wear agent comprises nano calcium carbonate and disoctyl zinc sulfate and phosphorus salt, and also comprises adding 3 parts of calcium acetate powder.

[0010] A method for preparing a low-thickening agent composite calcium sulfonate grease comprises the following steps:

[0011] Step 1: Add 2 / 3 of the base oil to the mixing preparation device, then add the overbased calcium sulfonate, heat to 40-50°C, and stir continuously to dissolve;

[0012] Step 2, add 12-alkylbenzene sulfonic acid, control the time for 15 to 20 minutes, stir for 10 minutes, and heat to 50-60°C;

[0013] Step 3, add acetic acid aqueous solution, the addition time is controlled within 20 to 30 minutes, the addition of acetic acid should be kept relatively closed, and stir the reaction for 1 hour;

[0014] Step 4: Raise the temperature to 95°C, add 12-hydroxystearic acid during the heating process to perform composite thickening, check the status of the conversion reaction every half an hour, stir for about 10 seconds until the system no longer thickens, and monitor the product by infrared spectroscopy until 881-884cm-1 appears, and the amorphous calcium carbonate is completely converted into crystalline calcium carbonate;

[0015] Step 5. Add thickened oil in 3 batches, leaving 10 minutes between each batch, or open the lid and let it flow continuously;

[0016] Step 6: Heat to 95-98°C, add calcium hydroxide emulsion slowly, and stir for 30 minutes;

[0017] Step 7: Control the temperature at 95-98°C, add boric acid aqueous solution, and dissolve it with hot water. If boric acid precipitates due to low temperature, reheat and dissolve it, add slowly, and stir for 30 minutes;

[0018] Step 8, add the remaining 12-hydroxystearic acid, control the temperature in the kettle to 95-100°C, and react for 1 hour;

[0019] Step 9: After the reaction is completed, the temperature is raised to 135-140°C and dehydrated at constant temperature for 40 minutes;

[0020] Step 10, raising the temperature in the kettle to 160-165°C for refining and keeping the temperature constant for 10 minutes;

[0021] Step 11: Cool the fat until the temperature drops to 50-60°C, then pass it into a grinder to grind out the fat.

[0022] As a further solution of the present invention: the mixing preparation device comprises:

[0023] A reaction mixing box, wherein a mixing preparation box is fixedly connected to the bottom of the reaction mixing box, and electric heating plates are fixedly connected to the reaction mixing box and the mixing preparation box;

[0024] A reaction mixing mechanism, which is disposed in a reaction mixing box and is used to fully mix and react the liquid raw materials;

[0025] The preparation mixing mechanism is arranged in a mixing preparation box and is used for fully mixing the reacted substances to prepare a thick composite calcium sulfonate grease.

[0026] As a further solution of the present invention: the reaction mixing mechanism comprises two extraction boxes fixedly connected to the reaction mixing box, a first electric telescopic rod is fixedly connected inside the reaction mixing box, one end of the first electric telescopic rod is fixedly connected to a transmission plate, a first transmission pipe is rotatably connected to the transmission plate, an outer surface of the first transmission pipe is rotatably connected to a transmission box slidably connected to the extraction box, a plurality of first stirring pipes are fixedly connected to the outer surface of the first transmission pipe, a plurality of suction pipes are fixedly connected to the extraction box, a one-way valve is arranged on the suction pipe, a hedging pipe is fixedly connected to the extraction box, the outer surface of the first transmission pipe is transmission-connected to a first transmission mechanism connected to the transmission plate, and the first transmission mechanism is used to drive the first transmission pipe to rotate;

[0027] A partition is fixedly connected inside the reaction mixing box, a first discharge pipe is fixedly connected to the partition, an electromagnetic valve is provided on the first discharge pipe, a feed funnel is fixedly connected to the top of the first transmission pipe, and a stirring and mixing mechanism connected to the transmission box is transmission-connected to the outer surface of the first transmission pipe, and the stirring and mixing mechanism is used to stir and mix the sucked materials.

[0028] As a further solution of the present invention: the stirring and mixing mechanism includes a first gear fixedly connected to a first transmission tube, a plurality of second gears are meshingly connected to the outer surface of the first gear, a first transmission shaft rotatably connected to a transmission box is fixedly connected to the middle of the second gear, a stirring blade is fixedly connected to the bottom end of the first transmission shaft, and a plurality of second stirring tubes are fixedly connected to the outer surface of the first transmission tube.

[0029] As a further solution of the present invention: the first transmission mechanism includes a first transmission motor fixedly connected to the transmission plate, the output end of the first transmission motor is fixedly connected to the first rotating shaft through a coupling, the outer surface of the first rotating shaft is fixedly sleeved with a first transmission gear, and the outer surface of the first transmission gear is meshingly connected with a second transmission gear fixedly sleeved with the first transmission tube.

[0030] As a further solution of the present invention: the preparation and mixing mechanism includes a second transmission motor fixedly connected to the mixing and preparing box, the output end of the second transmission motor is fixedly connected to a second rotating shaft rotatably connected to the mixing and preparing box through a coupling, the outer surface of the second rotating shaft is connected to a second transmission pipe rotatably connected to the mixing and preparing box through a transmission wheel and a transmission belt, the outer surface of the second transmission pipe is fixedly connected to a plurality of rubber stirring hoses, one end of the second transmission pipe is connected to a feeding mechanism connected to the mixing and preparing box, and the feeding mechanism is used to feed the second transmission pipe;

[0031] The mixing and preparing box is provided with a discharging mechanism, and the discharging mechanism is used for automatically discharging the prepared materials.

[0032] As a further solution of the present invention: the feeding mechanism includes a connecting pipe rotatably connected to the second transmission pipe, the connecting pipe is fixedly connected to the mixing preparation box, one end of the connecting pipe is fixedly connected to a water pump through a pipeline, an electromagnetic valve is provided on the pipeline, and one end of the water pump is fixedly connected to a feeding box fixedly connected to the mixing preparation box.

[0033] As a further solution of the present invention: the outer surface of the connecting pipe is fixedly connected to a fan fixedly connected to the mixing preparation box through a pipeline, the mixing preparation box is fixedly connected to an exhaust pipe, and the exhaust pipe is provided with an electromagnetic valve.

[0034] As a further solution of the present invention: the discharging mechanism includes a third transmission motor fixedly connected to the mixing preparation box, the output end of the third transmission motor is fixedly connected to the third rotating shaft through a coupling, the outer surface of the third rotating shaft is connected to a threaded rod rotatably connected to the mixing preparation box through a transmission wheel and a transmission belt, the outer surface of the threaded rod is threadedly matched with a push ring plate slidably connected to the mixing preparation box, the outer surface of the second transmission tube is fixedly connected to a push plate, two second discharge pipes are fixedly connected to the bottom of the mixing preparation box, a discharge plate fixedly connected to the mixing preparation box is arranged below the second discharge pipe, the bottom of the discharge plate is fixedly connected to a fourth transmission motor, the output end of the fourth transmission motor is fixedly connected to a spiral rod rotatably connected to the discharge plate through a coupling, the bottom of the mixing preparation box is fixedly connected to a second electric telescopic rod, the bottom end of the second electric telescopic rod is fixedly connected to a sealing plate slidably connected to the third rotating shaft, the bottom of the mixing preparation box is fixedly connected to a second electric telescopic rod, and the bottom end of the second electric telescopic rod is fixedly connected to a sealing plate slidably connected to the third rotating shaft.

[0035] Beneficial effects of the present invention:

[0036] (1) The product indicators are comparable to those of imported products through the ratio of long-chain linear sulfonic acid and heavy alkylbenzene sulfonic acid in the high-alkali synthetic calcium sulfonate provided. Special functional additives and polymer materials are added, and the colloidal structure of the system is strictly controlled. The production process does not require the addition of flammable, explosive and environmentally polluting phase transfer agents such as isopropanol and n-butanol, making it an environmentally friendly product.

[0037] (2) The thickening ability of high-alkalinity calcium sulfonate in the provided process is relatively strong. When 12-alkylbenzene sulfonic acid and calcium hydroxide are added, the main component of high-alkalinity calcium sulfonate is synthesized, which is equivalent to a production process combining a one-step method and a two-step method, and can greatly reduce the components of high-alkalinity calcium sulfonate. The traditional high-alkalinity calcium sulfonate production requires an addition amount of 35% to 40% per ton of grease, while the present process can reduce the components of calcium sulfonate to a minimum of about 20%. In addition, the heating of the present process is gradual and stable, and there is no rapid cooling process. The process control is simple, and the refining temperature is about 160°C, which is lower than the previous process.

[0038] (3) By placing the raw materials into a reaction mixing box and a mixing preparation box, and then cooperating with the reaction mixing mechanism and the preparation mixing mechanism, the raw materials can be fully stirred and mixed, which greatly improves the quality of the grease after production and also improves the reaction efficiency. At the same time, the preparation of the grease is divided into liquid mixing and thick mixing through the reaction mixing box and the mixing preparation box, and the two steps are carried out simultaneously, which greatly saves production time and improves the processing efficiency of the grease.

[0039] (4) The raw materials are introduced into a reaction preparation box, and then sucked into a pumping box through the reaction preparation box, and then ejected through the pumping box and the flushing pipe. At the same time, the stirring blades, the first stirring pipe and the second stirring pipe cooperate to achieve a sufficient mixing reaction between the raw materials, which greatly improves the mixing reaction effect between the raw materials. At the same time, the second transmission scraper drives the rubber stirring rod to stir, so that the raw materials are fully mixed, which greatly improves the quality of the grease after production.

[0040] (5) The push ring plate is moved by the Adi, and the push ring plate pushes the prepared grease to fully discharge the grease on the mixing preparation box and the rubber stirring tube, and then discharges it through the second discharge pipe, thereby realizing sufficient automatic discharge of the grease prepared in the mixing preparation box, which is convenient for the next preparation and use. BRIEF DESCRIPTION OF THE DRAWINGS

[0041] The present invention will be further described below in conjunction with the accompanying drawings.

[0042] Figure 1 is a first stereogram of the external structure of the present invention;

[0043] Figure 2 is a first stereogram of the internal structure of the present invention;

[0044] Figure 3 is a second stereoscopic view of the internal structure of the present invention;

[0045] Figure 4 The present invention Figure 1 A magnified view of middle;

[0046] Figure 5 The present invention Figure 2 Enlarged view of middle B;

[0047] Figure 6 The present invention Figure 2 Enlarged view of middle C;

[0048] Figure 7 The present invention Figure 3 Enlarged view of middle D;

[0049] Figure 8 The present invention Figure 3 Enlarged view of E.

[0050] In the figure: 1, reaction mixing box; 2, mixing preparation box; 3, electric heating plate; 11, extraction box; 12, first electric telescopic rod; 13, transmission plate; 14, first transmission pipe; 15, transmission box; 16, first stirring pipe; 17, suction pipe; 18, hedging pipe; 19, partition; 190, first discharge pipe; 191, feeding funnel; 21, first gear; 22, second gear; 23, first transmission shaft; 24, stirring blade; 25, second stirring pipe; 31, first transmission motor; 32, first rotating shaft; 33, first A transmission gear; 34, a second transmission gear; 41, a second transmission motor; 42, a second rotating shaft; 43, a second transmission pipe; 44, a rubber stirring hose; 51, a connecting pipe; 52, a water pump; 53, a feed box; 54, a fan; 55, an exhaust pipe; 61, a third transmission motor; 62, a third rotating shaft; 63, a threaded rod; 64, a push ring plate; 65, a push plate; 66, a second discharge pipe; 67, a discharge plate; 68, a fourth transmission motor; 69, a screw rod; 690, a second electric telescopic rod; 691, a sealing plate. DETAILED DESCRIPTION

[0051] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0052] Embodiment 1

[0053] The present invention is a low-thickener composite calcium sulfonate grease, characterized in that it comprises the following parts by weight:

[0054] The invention comprises 55-65 parts of base oil, 20-30 parts of thickener and 1-8 parts of extreme pressure anti-wear agent. The base oil is mineral oil and synthetic oil, including 150BS, 500N, polyalphaolefin and mixed oil of 150BS, 500N and polyalphaolefin; the thickener comprises high-base calcium sulfonate, a converter and a saponifier, the converter comprises 12-alkylbenzene sulfonic acid, 12-hydroxystearic acid and glacial acetic acid, the saponifier comprises 12-hydroxystearic acid, boric acid and calcium hydroxide; the extreme pressure anti-wear agent comprises nano calcium carbonate and disoctyl zinc sulfate and phosphorus salt, and also comprises adding 3 parts of calcium acetate powder.

[0055] Implementation Case 2

[0056] A method for preparing a low-thickening agent composite calcium sulfonate grease, characterized in that it comprises the following steps:

[0057] Step 1: Add 38.7 parts of 150BS base oil and 25.8 parts of overbased calcium sulfonate to the reactor, heat to 40-50°C, and stir continuously to dissolve;

[0058] Step 2: linearly add 1.2 parts of 12-alkylbenzenesulfonic acid for 15 to 20 minutes, stir for 10 minutes, and heat to 50-60°C;

[0059] Step 3: Add 0.77 parts of acetic acid (dissolved in 12.5 parts of water) over 20 to 30 minutes. The acetic acid should be added in a relatively closed state and stirred for 1 hour.

[0060] Step 4: Raise the temperature to 95°C, add 1.0 part of 12-hydroxystearic acid during the heating process to perform composite thickening, check the status of the conversion reaction every half an hour, stir for about 10 seconds until the system no longer thickens, and monitor the product by infrared spectroscopy until 881-884cm-1 appears, and the amorphous calcium carbonate is completely converted into crystalline calcium carbonate;

[0061] Step 5: Add thickened oil 150BS and PAO6 in 3 batches, add 8.8 parts of 150BS, 5.9 parts of PAO6, and 5.9 parts of PAO6 respectively, with an interval of 10 minutes between each batch, or open the lid and keep it flowing, and heat until it is completely integrated into the calcium sulfonate system;

[0062] Step 6: Heat to 95-98°C, add 1.1 parts of calcium hydroxide emulsion (dissolved in 2.2 parts of water), add slowly, and stir for 30 minutes;

[0063] Step 7: Control the temperature at 95-98°C, add 1.3 parts of boric acid aqueous solution (dissolved in 2.6 parts of hot water). If the boric acid precipitates due to low temperature, reheat and dissolve it, add slowly, and stir for 30 minutes;

[0064] Step 8, add the remaining 2.0 parts of 12-hydroxystearic acid, control the temperature in the kettle to 95-100°C, and react for 1 hour;

[0065] Step 9: After the reaction is completed, the temperature is raised to 135-140°C and dehydrated at constant temperature for 40 minutes;

[0066] Step 10, raising the temperature in the kettle to 160-165°C for refining and keeping the temperature constant for 10 minutes;

[0067] Step 11: Cooling: When the temperature of the fat drops to 60-80°C, add 3.7 parts of nano calcium carbonate and 3.7 parts of dioctyl zinc thiophosphate, heat to about 100°C, and completely blend into the system.

[0068] Step 12: Cool down the fat until the temperature drops to 50-60℃, then grind out the fat.

[0069] Implementation Case 3

[0070] Step 1: Add 37.6 parts of 150BS base oil and 25.1 parts of overbased calcium sulfonate to the reactor, heat to 40-50°C, and stir continuously to dissolve;

[0071] Step 2: linearly add 1.2 parts of 12-alkylbenzenesulfonic acid for 15 to 20 minutes, stir for 10 minutes, and heat to 50-60°C;

[0072] Step 3: Add 0.75 parts of acetic acid (0.025 parts dissolved in water), the addition time is controlled within 20 to 30 minutes, the addition of acetic acid should be kept relatively closed, and stir the reaction for 1 hour;

[0073] Step 4: Raise the temperature to 95°C, add 1 part of 12-hydroxystearic acid during the heating process to perform composite thickening, check the status of the conversion reaction every half an hour, stir for about 10 seconds until the system no longer thickens, and monitor the product by infrared spectroscopy until 881-884cm-1 appears, and the amorphous calcium carbonate is completely converted into crystalline calcium carbonate;

[0074] Step 5: Add thickened oil 150BS and PAO6 in 3 batches, add 8.5 parts of 150BS, 5.75 parts of PAO6, and 5.75 parts of PAO6 respectively, with an interval of 10 minutes between each batch, or open the lid and keep it flowing, and heat until it is completely integrated into the calcium sulfonate system;

[0075] Step 6: Heat to 95-98°C, add 1.1 parts of calcium hydroxide emulsion (dissolved in 2.2 parts of water), add slowly, and stir for 30 minutes;

[0076] Step 7: Control the temperature at 95-98°C, add 1.25 parts of boric acid aqueous solution (dissolved in 2.5 parts of hot water). If the boric acid precipitates due to low temperature, reheat and dissolve it, add slowly, and stir for 30 minutes;

[0077] Step 8, add the remaining 2 parts of 12-hydroxystearic acid, control the temperature in the kettle at 95-100°C, and react for 1 hour;

[0078] Step 9: Keep the temperature at about 95-100°C, add 2.7 parts of calcium acetate powder, and continue heating to dissolve;

[0079] Step 10, heating to 135-140°C, constant temperature dehydration for 40 minutes;

[0080] Step 11, raising the temperature in the kettle to 160-165°C for refining and keeping the temperature constant for 10 minutes;

[0081] Step 12: Cooling: When the temperature of the fat drops to 60-80°C, add 3.6 parts of nano calcium carbonate and 3.6 parts of dioctyl zinc thiophosphate, heat to about 100°C, and completely integrate into the system.

[0082] (13) Cool the fat until the temperature drops to 50-60°C, then grind the fat.

[0083] Implementation Case 4

[0084] Step 1: Add 37.6 parts of 150BS base oil and 25.1 parts of overbased calcium sulfonate to the reactor, heat to 40-50°C, and stir continuously to dissolve;

[0085] Step 2: linearly add 1.2 parts of 12-alkylbenzenesulfonic acid for 15 to 20 minutes, stir for 10 minutes, and heat to 50-60°C;

[0086] Step 3: Add 0.75 parts of acetic acid (0.025 parts dissolved in water), the addition time is controlled within 20 to 30 minutes, the addition of acetic acid should be kept relatively closed, and stir the reaction for 1 hour;

[0087] Step 4: Raise the temperature to 95°C, add 1 part of 12-hydroxystearic acid during the heating process to perform composite thickening, check the status of the conversion reaction every half an hour, stir for about 10 seconds until the system no longer thickens, and monitor the product by infrared spectroscopy until 881-884cm-1 appears, and the amorphous calcium carbonate is completely converted into crystalline calcium carbonate;

[0088] Step 5: Add thickened oil 150BS and PAO6 in 3 batches, add 8.5 parts of 150BS, 5.75 parts of PAO6, and 5.75 parts of PAO6 respectively, with an interval of 10 minutes between each batch, or open the lid and keep it flowing, and heat until it is completely integrated into the calcium sulfonate system;

[0089] Step 6: Heat to 95-98°C, add 1.1 parts of calcium hydroxide emulsion (dissolved in 2.2 parts of water), add slowly, and stir for 30 minutes;

[0090] Step 7: Control the temperature at 95-98°C, add 1.25 parts of boric acid aqueous solution (dissolved in 2.5 parts of hot water). If the boric acid precipitates due to low temperature, reheat and dissolve it, add slowly, and stir for 30 minutes;

[0091] Step 8, add the remaining 2 parts of 12-hydroxystearic acid, control the temperature in the kettle at 95-100°C, and react for 1 hour;

[0092] Step 9, heating to 135-140°C, constant temperature dehydration for 40 minutes;

[0093] Step 10, raising the temperature in the kettle to 160-165°C for refining and keeping the temperature constant for 10 minutes;

[0094] Step 11: Cooling: When the temperature of the fat drops to 60-80°C, add 2.7 parts of calcium acetate powder, 3.6 parts of nano calcium carbonate and 3.6 parts of dioctyl zinc thiophosphate, heat to about 100°C, and completely blend into the system;

[0095] Step 12: Cool down the fat until the temperature drops to 50-60℃, then grind out the fat.

[0096] Implementation Case 5

[0097] Step 1: Add 37.6 parts of 150BS base oil and 25.1 parts of overbased calcium sulfonate to the reactor, heat to 40-50°C, and stir continuously to dissolve;

[0098] Step 2: linearly add 1.2 parts of 12-alkylbenzenesulfonic acid for 15 to 20 minutes, stir for 10 minutes, and heat to 50-60°C;

[0099] Step 3: Add 3.45 parts of acetic acid (dissolved in 12.5 parts of water) over 20 to 30 minutes. The acetic acid should be added in a relatively closed container and stirred for 1 hour.

[0100] Step 4: Raise the temperature to 95°C, add 1 part of 12-hydroxystearic acid during the heating process to perform composite thickening, check the status of the conversion reaction every half an hour, stir for about 10 seconds until the system no longer thickens, and monitor the product by infrared spectroscopy until 881-884cm-1 appears, and the amorphous calcium carbonate is completely converted into crystalline calcium carbonate;

[0101] Step 5: Add thickened oil 150BS and PAO6 in 3 batches, add 8.5 parts of 150BS, 5.75 parts of PAO6, and 5.75 parts of PAO6 respectively, with an interval of 10 minutes between each batch, or open the lid and keep it flowing, and heat until it is completely integrated into the calcium sulfonate system;

[0102] Step 6: Heat to 95-98°C, add 1.1 parts of calcium hydroxide emulsion (dissolved in 2.2 parts of water), add slowly, and stir for 30 minutes;

[0103] Step 7: Control the temperature at 95-98°C, add 1.25 parts of boric acid aqueous solution (dissolved in 2.5 parts of hot water). If the boric acid precipitates due to low temperature, reheat and dissolve it, add slowly, and stir for 30 minutes;

[0104] Step 8, add the remaining 2 parts of 12-hydroxystearic acid, control the temperature in the kettle at 95-100°C, and react for 1 hour;

[0105] Step 9, heating to 135-140°C, constant temperature dehydration for 40 minutes;

[0106] Step 10, raising the temperature in the kettle to 160-165°C for refining and keeping the temperature constant for 10 minutes;

[0107] Step 11: Cooling: When the temperature of the fat drops to 60-80°C, add 3.6 parts of nano calcium carbonate and 3.6 parts of dioctyl zinc thiophosphate, heat to about 100°C, and completely integrate into the system;

[0108] Step 12: Cool down the fat until the temperature drops to 50-60℃, then grind the fat.

[0109] Implementation Case 6

[0110] Step 1: Add 36.6 parts of 150BS base oil and 24.4 parts of overbased calcium sulfonate to the reactor, heat to 40-50°C, and stir continuously to dissolve;

[0111] Step 2: linearly add 1.2 parts of 12-alkylbenzenesulfonic acid for 15 to 20 minutes, stir for 10 minutes, and heat to 50-60°C;

[0112] Step 3: Add 0.75 parts of acetic acid (dissolved in 2.5 parts of water) for 20 to 30 minutes. The acetic acid should be added in a relatively closed state and stirred for 1 hour.

[0113] Step 4: Raise the temperature to 95°C, add 1 part of 12-hydroxystearic acid during the heating process to perform composite thickening, check the status of the conversion reaction every half an hour, stir for about 10 seconds until the system no longer thickens, and monitor the product by infrared spectroscopy until 881-884cm-1 appears, and the amorphous calcium carbonate is completely converted into crystalline calcium carbonate;

[0114] Step 5: Add thickened oil 150BS and PAO6 in 3 batches, add 8.5 parts of 150BS, 5.75 parts of PAO6, and 5.75 parts of PAO6 respectively, with an interval of 10 minutes between each batch, or open the lid and keep it flowing, and heat until it is completely integrated into the calcium sulfonate system;

[0115] Step 6: Heat to 95-98°C, add 1.1 parts of calcium hydroxide emulsion (dissolved in 2.2 parts of water), add slowly, and stir for 30 minutes;

[0116] Step 7: Control the temperature at 95-98°C, add 1.25 parts of boric acid aqueous solution (dissolved in 2.5 parts of hot water). If the boric acid precipitates due to low temperature, reheat and dissolve it, add slowly, and stir for 30 minutes;

[0117] Step 8, add the remaining 2 parts of 12-hydroxystearic acid, control the temperature in the kettle at 95-100°C, and react for 1 hour;

[0118] Step 9: Keep the temperature at about 95-100°C, add 5.3 parts of calcium acetate powder, and continue heating to dissolve;

[0119] Step 10, heating to 135-140°C, constant temperature dehydration for 40 minutes;

[0120] Step 11, raising the temperature in the kettle to 160-165°C for refining and keeping the temperature constant for 10 minutes;

[0121] Step 12: Cooling: When the temperature of the fat drops to 60-80°C, add 3.5 parts of nano calcium carbonate and 3.5 parts of dioctyl zinc thiophosphate, heat to about 100°C, and completely integrate into the system;

[0122] Step 13: Cool down the fat until the temperature drops to 50-60℃, then grind the fat.

[0123] Implementation Case 7

[0124] Step 1: Add 35.7 parts of 150BS base oil and 23.8 parts of overbased calcium sulfonate to the reactor, heat to 40-50°C, and stir continuously to dissolve;

[0125] Step 2: linearly add 1.2 parts of 12-alkylbenzenesulfonic acid for 15 to 20 minutes, stir for 10 minutes, and heat to 50-60°C;

[0126] Step 3: Add 0.75 parts of acetic acid (dissolved in 2.5 parts of water) for 20 to 30 minutes. The acetic acid should be added in a relatively closed state and stirred for 1 hour.

[0127] Step 4: Raise the temperature to 95°C, add 1 part of 12-hydroxystearic acid during the heating process to perform composite thickening, check the status of the conversion reaction every half an hour, stir for about 10 seconds until the system no longer thickens, and monitor the product by infrared spectroscopy until 881-884cm-1 appears, and the amorphous calcium carbonate is completely converted into crystalline calcium carbonate;

[0128] Step 5: Add thickened oil 150BS and PAO6 in 3 batches, add 8.5 parts of 150BS, 5.75 parts of PAO6, and 5.75 parts of PAO6 respectively, with an interval of 10 minutes between each batch, or open the lid and keep it flowing, and heat until it is completely integrated into the calcium sulfonate system;

[0129] Step 6: Heat to 95-98°C, add 1.1 parts of calcium hydroxide emulsion (dissolved in 2.2 parts of water), add slowly, and stir for 30 minutes;

[0130] Step 7: Control the temperature at 95-98°C, add 1.25 parts of boric acid aqueous solution (dissolved in 2.5 parts of hot water). If the boric acid precipitates due to low temperature, reheat and dissolve it, add slowly, and stir for 30 minutes;

[0131] Step 8, add the remaining 2 parts of 12-hydroxystearic acid, control the temperature in the kettle at 95-100°C, and react for 1 hour;

[0132] Step 9: Keep the temperature at about 95-100°C, add 7.7 parts of calcium acetate powder, and continue heating to dissolve;

[0133] Step 10, heating to 135-140°C, constant temperature dehydration for 40 minutes;

[0134] Step 11, raising the temperature in the kettle to 160-165°C for refining and keeping the temperature constant for 10 minutes;

[0135] Step 12: Cooling: When the temperature of the fat drops to 60-80°C, add 3.4 parts of nano calcium carbonate and 3.4 parts of dioctyl zinc thiophosphate, heat to about 100°C, and completely integrate into the system;

[0136] Step 13: Cool down the fat until the temperature drops to 50-60℃, then grind the fat.

[0137] Its performance is shown in Table 1.

[0138] Table 1 Comparison of the impact of the process for preparing calcium acetate grease in the implementation case of the present invention

[0139]

[0140]

[0141] From the analysis results in the above table, we can see that:

[0142] 1) Comparison between Example 2 and Example 3: Under the same conditions of thickener and additives, the process of adding calcium acetate has an important influence on the performance of composite calcium sulfonate. The performance of adding calcium acetate powder before refining is better than adding calcium acetate after refining. Adding calcium acetate powder before refining can heat up to a higher temperature, calcium acetate is better integrated into the system, and its consistency and steel mesh oil separation ability are improved;

[0143] 2) Comparison between Example 2, Example 3 and Example 4: Under the same conditions of base oil and thickener, adding too much acetic acid will result in the conversion process not forming fat, not converting into calcite structure, and the conversion process fails;

[0144] 3) Comparison of Example 1 with Example 2, Example 5 and Example 6: Under the same conditions of base oil and additives, the addition of calcium acetate will improve the dropping point, steel mesh oil separation performance and consistency of the grease, but the continuous addition of calcium acetate will lead to a decrease in the proportion of high-base calcium sulfonate in the system, reduce extreme pressure and anti-wear properties, and reduce water resistance. According to experimental results, it is better to be around 3%-5%;

[0145] 4) In summary, the composite calcium sulfonate grease provided by the present invention not only has excellent high and low temperature performance and water resistance, but is also environmentally friendly and economical, and has controllable process operation. It is a grease with excellent comprehensive performance.

[0146] Through the ratio of long-chain linear sulfonic acid and heavy alkylbenzene sulfonic acid in the high-alkali synthetic calcium sulfonate provided, the product indicators are equivalent to those of imported products. Special functional additives and polymer materials are added, and the colloid structure of the system is strictly controlled. The production process does not require the addition of flammable, explosive and environmentally polluting phase transfer agents such as isopropanol and n-butanol, making it an environmentally friendly product.

[0147] The high-alkalinity calcium sulfonate has a strong thickening ability through the provided process. When 12-alkylbenzene sulfonic acid and calcium hydroxide are added, the main components of the high-alkalinity calcium sulfonate are synthesized, which is equivalent to a production process combining a one-step method and a core two-step method, and can greatly reduce the components of the high-alkalinity calcium sulfonate. The traditional high-alkalinity calcium sulfonate production requires an addition amount of 35% to 40% per ton of grease, while the process can reduce the components of calcium sulfonate to a minimum of about 20%. In addition, the heating of the process is gradual and steadily rising, without a rapid cooling process, and the process control is simple. The refining temperature is about 160°C, which is lower than the previous process.

[0148] Embodiment 8

[0149] See also Figure 1 - Figure 8 As shown, the mixing and preparing device includes a reaction mixing box 1, a mixing and preparing box 2 is fixedly connected to the bottom of the reaction mixing box 1, electric heating plates 3 are fixedly connected to the reaction mixing box 1 and the mixing and preparing box 2, the electric heating plate 3 is connected to the temperature controller, and the heating temperature of the heating plate can be adjusted according to the temperature in the reaction mixing box 1 and the mixing and preparing box 2, a transparent observation glass window is fixedly connected to the reaction mixing box 1, a reaction mixing mechanism is arranged in the reaction mixing box 1, the reaction mixing mechanism is used for fully mixing the liquid raw materials, and a preparation mixing mechanism is arranged in the mixing and preparing box 2, the preparation mixing mechanism is used for re-adding and fully mixing the reacted substances to prepare thick composite calcium sulfate grease.

[0150] 2 / 3 of the base oil is added into the reaction mixing box 1, and then high base calcium sulfonate is added, and then the solution is heated to 40-50°C by the electric heating plate 3, and then the solution is fully stirred and mixed by the reaction mixing mechanism in the reaction mixing box 1, and the temperature is raised to 50-60°C, and then 12-alkylbenzene sulfonic acid is added, and then the solution is stirred and mixed again by the reaction mixing mechanism, and then an acetic acid aqueous solution is added, and then the solution is stirred and mixed, and then the temperature is raised to 95°C again, and 12-hydroxystearic acid is added during the heating process, and the solution is stirred and mixed at the same time to accelerate the reaction and perform composite thickening. The conversion reaction is checked every half an hour, and the solution is stirred for about 10 seconds until the system no longer thickens. The product is monitored by infrared spectroscopy until 881-884cm-1 appears, and the amorphous calcium carbonate is completely converted into crystalline calcium carbonate.

[0151] After the above reaction is completed, the above solution is passed into the mixing preparation box 2. When the raw materials in the reaction mixing box 1 are completely introduced into the mixing preparation box 2, the reaction mixing box 1 then repeats the above feeding and mixing reaction, and then thickened oil is added to the mixing preparation box 2, and then stirred and mixed by the mixing preparation box 2, and then heated to 95-98° C. by the heating plate in the mixing preparation box 2, and then calcium hydroxide emulsion is added, stirred and mixed, and then boric acid aqueous solution is added for stirring and mixing, and finally the remaining 12-hydroxystearic acid is added for mixing, and when the reaction is completed After that, the mixing preparation box 2 is heated to 135-140°C, dehydrated at a constant temperature for 40 minutes, the temperature in the kettle is heated to 160-165°C for refining, kept at a constant temperature for 10 minutes, cooled, and the grease is discharged after the temperature drops to 50-60°C, thereby achieving sufficient stirring and mixing reaction of the raw materials, greatly improving the quality of the grease after production, and also improving the reaction efficiency. At the same time, the preparation of the grease is divided into liquid mixing and thick mixing through the reaction mixing box 1 and the mixing preparation box 2, and the two steps are carried out simultaneously, which greatly saves production time and improves the processing efficiency of the grease.

[0152] Embodiment 9

[0153] Based on Example 8, please refer to Figure 2 - Figure 7As shown, the reaction mixing mechanism includes two extraction boxes 11 fixedly connected to the reaction mixing box 1, a first electric telescopic rod 12 is fixedly connected inside the reaction mixing box 1, one end of the first electric telescopic rod 12 is fixedly connected to a transmission plate 13, a first transmission pipe 14 is rotatably connected to the transmission plate 13, the outer surface of the first transmission pipe 14 is rotatably connected to a transmission box 15 slidably connected to the extraction box 11, a plurality of first stirring pipes 16 are fixedly connected to the outer surface of the first transmission pipe 14, the lengths of the plurality of first stirring pipes 16 are different, and the raw materials can be discharged into different radii during discharge, a plurality of suction pipes 17 are fixedly connected to the extraction box 11, a one-way valve is arranged on the suction pipe 17, a hedging pipe 18 is fixedly connected to the extraction box 11, and the outer surface of the first transmission pipe 14 is transmission-connected to the transmission box 15. The first transmission mechanism connected to the plate 13 is used to drive the first transmission tube 14 to rotate. The first transmission mechanism includes a first transmission motor 31 fixedly connected to the transmission plate 13. The first transmission motor 31 is controlled by a PLC programming program to control the first transmission motor 31 to rotate forward and reverse and rotate at an angle. The output end of the first transmission motor 31 is fixedly connected to a first rotating shaft 32 through a coupling. A first transmission gear 33 is fixedly sleeved on the outer surface of the first rotating shaft 32. The outer surface of the first transmission gear 33 is meshedly connected to a second transmission gear 34 fixedly sleeved with the first transmission tube 14. The first rotating shaft 32 is driven to rotate by the first transmission motor 31, and the first rotating shaft 32 drives the first transmission tube 14 to rotate through the first transmission gear 33 and the second transmission gear 34;

[0154] A partition 19 is fixedly connected inside the reaction mixing box 1, and a first discharge pipe 190 is fixedly connected to the partition 19. The first discharge pipe 190 is provided with an electromagnetic valve, and a feed funnel 191 is fixedly connected to the top of the first transmission pipe 14. The outer surface of the first transmission pipe 14 is transmission-connected with a stirring and mixing mechanism connected to the transmission box 15, and the stirring and mixing mechanism is used to stir and mix the sucked material. The stirring and mixing mechanism includes a first gear 21 fixedly sleeved with the first transmission pipe 14, and the outer surface of the first gear 21 is meshingly connected with a plurality of second gears 22, and the middle of the second gear 22 is fixedly sleeved with a first transmission shaft 23 rotatably connected to the transmission box 15, and the bottom end of the first transmission shaft 23 is fixedly connected with a stirring blade 24, and the outer surface of the first transmission pipe 14 is fixedly connected with a plurality of second stirring pipes 25, and the lengths of the plurality of second stirring pipes 25 are different, so that the raw materials can be discharged into different radius ranges during discharge.

[0155] By adding the raw materials into the reaction mixing box 1, the transmission plate 13 is driven downward by the first electric telescopic rod 12, the transmission plate 13 drives the first transmission tube 14 to move downward, and then drives the transmission box 15 to move downward, and then the first electric telescopic rod 12 drives the transmission box 15 to move upward, and then the extraction box 11 draws the raw materials in the reaction mixing box 1 into the extraction box 11 through the suction tube 17. In the process of extracting materials, the first transmission tube 14 is driven to rotate by the first transmission mechanism at the same time, and the first transmission tube 14 drives the first transmission shaft 23 to rotate through the first gear 21 and the second gear 22, and the first transmission shaft 23 drives the stirring blade 24 to rotate, and the stirring blade 24 stirs and mixes the sucked raw materials. When the suction is completed, the transmission plate 13 is then driven downward by the first electric telescopic rod 12, the transmission plate 13 drives the first transmission tube 14 to move downward, the first transmission tube 14 drives the transmission box 15 to move downward, and at the same time, the first transmission mechanism drives the first transmission tube 14 to rotate, thereby driving the stirring blade 24 to rotate, and the raw materials are stirred again, and then the transmission box 15 pushes out the raw materials in the extraction box 11, and then the extraction box 11 is sprayed out through the hedging pipe 18, so that the raw materials in the two extraction boxes 11 are collided to the middle position in the reaction mixing box 1 through the hedging pipe 18, so as to realize the hedging fusion between the raw materials. At the same time, in the symmetrical process, the first transmission pipe 14 drives the first stirring pipe 16 to rotate and move downward to stir and mix the raw materials, which greatly improves the mitigation effect on the raw materials and further improves the reaction effect between the raw materials. At the same time, in the raw material feeding process, the raw materials are passed into the first transmission pipe 14, and then the first transmission pipe 14 discharges the raw materials through the first stirring pipe 16 and the second stirring pipe 25. At the same time, the first transmission pipe 14 drives the first stirring pipe 16 and the second stirring pipe 25 to rotate. At the same time, each of the multiple first stirring pipes 16 and the second stirring pipes 25 has a different length, and the raw materials can be evenly sprinkled into the reaction mixing box 1, which further improves the mixing effect between the raw materials. After being completely mixed, the raw materials after the mixed reaction are then passed into the mixing preparation box 2 through the first discharge pipe 190 on the partition 19.

[0156] Embodiment 10

[0157] Based on Example 9, please refer to Figure 2 , Figure 3 , Figure 4 and Figure 8As shown, the preparation and mixing mechanism includes a second transmission motor 41 fixedly connected to the mixing preparation box 2, the second transmission motor 41 is controlled by a PLC programming program, and the second transmission motor 41 can be controlled to rotate forward and reverse and rotate at an angle, the output end of the second transmission motor 41 is fixedly connected to a second rotating shaft 42 rotatably connected to the mixing preparation box 2 through a coupling, the outer surface of the second rotating shaft 42 is connected to a second transmission tube 43 rotatably connected to the mixing preparation box 2 through a transmission wheel and a transmission belt, the outer surface of the second transmission tube 43 is fixedly connected to a plurality of rubber stirring hoses 44, the plurality of rubber stirring hoses 44 have different lengths, and the raw materials can be discharged into different radius ranges when discharging. , one end of the second transmission pipe 43 is drivingly connected to a feeding mechanism connected to the mixing preparation box 2, the feeding mechanism is used to feed the second transmission pipe 43, the feeding mechanism includes a connecting pipe 51 rotatably connected to the second transmission pipe 43, the connecting pipe 51 is fixedly connected to the mixing preparation box 2, one end of the connecting pipe 51 is fixedly connected to a water pump 52 through a pipeline, an electromagnetic valve is provided on the pipeline, one end of the water pump 52 is fixedly connected to a feed box 53 fixedly connected to the mixing preparation box 2, the outer surface of the connecting pipe 51 is fixedly connected to a fan 54 fixedly connected to the mixing preparation box 2 through a pipeline, the mixing preparation box 2 is fixedly connected to an exhaust pipe 55, and the exhaust pipe 55 is provided with an electromagnetic valve;

[0158] The mixing and preparing box 2 is provided with a discharging mechanism, which is used to automatically discharge the prepared materials.

[0159] The raw materials mixed in the reaction mixing box 1 are introduced into the mixing preparation box 2, and then the raw materials are put into the feed box 53, and then the raw materials are pumped into the second transmission pipe 43 through the pipeline and the connecting pipe 51 by the water pump 52, and then the second transmission pipe 43 discharges the raw materials through multiple rubber stirring hoses 44. At the same time, the second transmission motor 41 drives the second rotating shaft 42 to rotate, and the second rotating shaft 42 drives the second transmission pipe 43 to rotate through the transmission belt and the transmission wheel. The second transmission pipe 43 drives multiple rubber stirring hoses 44 to rotate, and the rubber stirring hose 44 sprinkles the raw materials into various positions in the mixing preparation box 2. At the same time, the rubber stirring hose 44 fully stirs and mixes the raw materials. When the mixing reaction is completed, the fan 54 is then operated, and the fan 54 blows cold air into the connecting pipe 51 through the pipeline, and then the cold air enters the second transmission pipe 43, and the second transmission pipe 43 blows the cold air out through the rubber stirring hose 44 to cool the mixing preparation box 2, so that thick grease is generated, and then discharged through the discharge mechanism.

[0160] Embodiment 11

[0161] Based on Example 10, please refer to Figure 3 and Figure 8As shown, the discharging mechanism includes a third transmission motor 61 fixedly connected to the mixing preparation box 2, the third transmission motor 61 is controlled by a PLC programming program, and the third transmission motor 61 can be controlled to rotate forward and reverse and rotate at an angle, the output end of the third transmission motor 61 is fixedly connected to a third rotating shaft 62 through a coupling, the outer surface of the third rotating shaft 62 is connected to a threaded rod 63 rotatably connected to the mixing preparation box 2 through a transmission wheel and a transmission belt, the outer surface of the threaded rod 63 is threadedly matched with a push ring plate 64 slidably connected to the mixing preparation box 2, and the outer surface of the second transmission tube 43 is fixedly connected to a push plate 65. Two second discharge pipes 66 are fixedly connected to the bottom of the mixing preparation box 2, and an electromagnetic valve is arranged on the second discharge pipe 66. A discharge plate 67 fixedly connected to the mixing preparation box 2 is arranged below the second discharge pipe 66. A fourth transmission motor 68 is fixedly connected to the bottom of the discharge plate 67, and an output end of the fourth transmission motor 68 is fixedly connected to a screw rod 69 rotatably connected to the discharge plate 67 through a coupling. A second electric telescopic rod 690 is fixedly connected to the bottom of the mixing preparation box 2, and a sealing plate 691 slidably connected to the third rotating shaft 62 is fixedly connected to the bottom of the second electric telescopic rod 690.

[0162] The third rotating shaft 62 is driven to rotate by the third transmission motor 61, and the third rotating shaft 62 drives the threaded rod 63 to rotate through the transmission wheel and the transmission belt, and the threaded rod 63 drives the push ring plate 64 to move, and the push ring plate 64 pushes the grease to the second discharge pipe 66 position. At this time, the sealing plate 691 is driven downward by the second electric telescopic rod 690 to open the bottom of the second discharge pipe 66, and then the fourth transmission motor 68 drives the threaded rod 63 to rotate, and the threaded rod 63 transports the grease downward into the second discharge pipe 66 for discharge. The rubber stirring hose 44 scrapes the material in the inner hole of the push ring plate 64, and the grease on the rubber stirring hose 44 is scraped off, and then it moves to one side, and then the push plate 65 is driven to rotate through the second transmission tube 43, and the push plate 65 scrapes the grease on the push ring plate 64, so that it enters the position of the screw rod 69, and then it is spirally transported to the second discharge pipe 66, and then discharged to the discharge plate 67 through the second discharge pipe 66 for discharge, thereby achieving sufficient discharge of the grease prepared in the mixing preparation box 2, which is convenient for preparation and use next time.

[0163] The above is a detailed description of an embodiment of the present invention, but the content is only a preferred embodiment of the present invention and cannot be considered to limit the scope of implementation of the present invention. All equivalent changes and improvements made within the scope of the present invention should still fall within the scope of the patent coverage of the present invention.

Claims

1. A low-thickener composite calcium sulfonate grease, characterized in that: The invention comprises the following parts by weight: 55-65 parts of base oil, 20-30 parts of thickener, and 1-8 parts of extreme pressure anti-wear agent, wherein the base oil is mineral oil and synthetic oil, including 150BS, 500N, polyalphaolefin, and mixed oil of 150BS, 500N and polyalphaolefin; the thickener comprises high-base calcium sulfonate, a converter and a saponifier, the converter comprises 12-alkylbenzene sulfonic acid, 12-hydroxystearic acid and glacial acetic acid, the saponifier comprises 12-hydroxystearic acid, boric acid and calcium hydroxide; the extreme pressure anti-wear agent comprises nano calcium carbonate and disoctyl zinc sulfate and phosphorus salt, and further comprises adding 3 parts of calcium acetate powder.

2. The method for preparing a low-thickening agent composite calcium sulfonate grease according to claim 1, characterized in that: The following steps are involved: Step 1: Add 2 / 3 of the base oil to the mixing preparation device, then add the overbased calcium sulfonate, heat to 40-50°C, and stir continuously to dissolve; Step 2: Add 12-alkylbenzenesulfonic acid for 15-20 minutes, stir for 10 minutes, and heat to 50-60°C; Step 3, add acetic acid aqueous solution, the adding time is controlled within 20-30 minutes, the addition of acetic acid should be kept relatively closed, and stir the reaction for 1 hour; Step 4: Raise the temperature to 95°C, add 12-hydroxystearic acid during the heating process to perform composite thickening, check the status of the conversion reaction every half an hour, stir for about 10 seconds until the system no longer thickens, and monitor the product by infrared spectroscopy until 881-884cm-1 appears, and the amorphous calcium carbonate is completely converted into crystalline calcium carbonate; Step 5. Add thickened oil in 3 batches, leaving 10 minutes between each batch, or open the lid and let it flow continuously; Step 6: Heat to 95-98°C, add calcium hydroxide emulsion slowly, and stir for 30 minutes; Step 7: Control the temperature at 95-98°C, add boric acid aqueous solution, and dissolve it with hot water. If boric acid precipitates due to low temperature, reheat and dissolve it, add slowly, and stir for 30 minutes; Step 8, add the remaining 12-hydroxystearic acid, control the temperature in the kettle to 95-100°C, and react for 1 hour; Step 9: After the reaction is completed, the temperature is raised to 135-140°C and dehydrated at constant temperature for 40 minutes; Step 10, raising the temperature in the kettle to 160-165°C for refining and keeping the temperature constant for 10 minutes; Step 11: Cool the fat until the temperature drops to 50-60°C, then pass it into a grinder to grind out the fat.

3. A low-thickener composite calcium sulfonate grease and a preparation method thereof according to claim 2, characterized in that: The mixing preparation device comprises: A reaction mixing box (1), wherein the bottom of the reaction mixing box (1) is fixedly connected to a mixing preparation box (2), and the reaction mixing box (1) and the mixing preparation box (2) are both fixedly connected to electric heating plates (3); A reaction mixing mechanism, the reaction mixing mechanism being arranged in the reaction mixing box (1), and the reaction mixing mechanism being used to fully mix the liquid raw materials; The preparation mixing mechanism is arranged in the mixing preparation box (2), and is used to add materials again to the reacted substances for sufficient mixing to prepare a thick composite calcium sulfonate grease.

4. A low-thickener composite calcium sulfonate grease and a preparation method thereof according to claim 3, characterized in that: The reaction mixing mechanism comprises two material extraction boxes (11) fixedly connected to the reaction mixing box (1), a first electric telescopic rod (12) fixedly connected inside the reaction mixing box (1), one end of the first electric telescopic rod (12) fixedly connected to a transmission plate (13), a first transmission pipe (14) rotatably connected to the transmission plate (13), an outer surface of the first transmission pipe (14) rotatably connected to a transmission box (15) slidably connected to the material extraction box (11), a plurality of first stirring pipes (16) fixedly connected to the outer surface of the first transmission pipe (14), a plurality of suction pipes (17) fixedly connected to the material extraction box (11), a one-way valve provided on the suction pipe (17), a hedging pipe (18) fixedly connected to the material extraction box (11), a first transmission mechanism connected to the transmission plate (13) rotatably connected to the outer surface of the first transmission pipe (14), the first transmission mechanism being used to drive the first transmission pipe (14) to rotate; A partition (19) is fixedly connected inside the reaction mixing box (1), a first discharge pipe (190) is fixedly connected to the partition (19), an electromagnetic valve is provided on the first discharge pipe (190), a feed hopper (191) is fixedly connected to the top of the first transmission pipe (14), a stirring and mixing mechanism connected to the transmission box (15) is transmission-connected to the outer surface of the first transmission pipe (14), and the stirring and mixing mechanism is used to stir and mix the sucked materials.

5. A low-thickener composite calcium sulfonate grease and a preparation method thereof according to claim 4, characterized in that: The stirring and mixing mechanism comprises a first gear (21) fixedly sleeved with a first transmission tube (14); a plurality of second gears (22) are meshingly connected to the outer surface of the first gear (21); a first transmission shaft (23) rotatably connected to a transmission box (15) is fixedly sleeved in the middle of the second gear (22); a stirring blade (24) is fixedly connected to the bottom end of the first transmission shaft (23); and a plurality of second stirring tubes (25) are fixedly connected to the outer surface of the first transmission tube (14).

6. A low-thickener composite calcium sulfonate grease and a preparation method thereof according to claim 4, characterized in that: The first transmission mechanism comprises a first transmission motor (31) fixedly connected to a transmission plate (13); an output end of the first transmission motor (31) is fixedly connected to a first rotating shaft (32) via a coupling; a first transmission gear (33) is fixedly sleeved on an outer surface of the first rotating shaft (32); and a second transmission gear (34) fixedly sleeved on an outer surface of the first transmission gear (33) is meshingly connected to a second transmission gear (34) fixedly sleeved on a first transmission tube (14).

7. A low-thickener composite calcium sulfonate grease and a preparation method thereof according to claim 3, characterized in that: The preparation and mixing mechanism comprises a second transmission motor (41) fixedly connected to the mixing and preparing box (2); the output end of the second transmission motor (41) is fixedly connected to a second rotating shaft (42) rotatably connected to the mixing and preparing box (2) via a coupling; the outer surface of the second rotating shaft (42) is connected to a second transmission pipe (43) rotatably connected to the mixing and preparing box (2) via a transmission wheel and a transmission belt; the outer surface of the second transmission pipe (43) is fixedly connected to a plurality of rubber stirring hoses (44); one end of the second transmission pipe (43) is connected to a feeding mechanism connected to the mixing and preparing box (2); the feeding mechanism is used to feed the second transmission pipe (43); The mixing and preparation box (2) is provided with a discharge mechanism, and the discharge mechanism is used to automatically discharge the prepared materials.

8. A low-thickener composite calcium sulfonate grease and a preparation method thereof according to claim 7, characterized in that: The feeding mechanism comprises a connecting pipe (51) rotatably connected to the second transmission pipe (43), the connecting pipe (51) being fixedly connected to the mixing preparation box (2), one end of the connecting pipe (51) being fixedly connected to a water pump (52) via a pipeline, an electromagnetic valve being provided on the pipeline, and one end of the water pump (52) being fixedly connected to a feeding box (53) fixedly connected to the mixing preparation box (2).

9. A low-thickener composite calcium sulfonate grease and a preparation method thereof according to claim 8, characterized in that: The outer surface of the connecting pipe (51) is fixedly connected to a fan (54) fixedly connected to the mixing preparation box (2) through a pipeline, and the mixing preparation box (2) is fixedly connected to an exhaust pipe (55), and the exhaust pipe (55) is provided with an electromagnetic valve.

10. A low-thickener composite calcium sulfonate grease and a preparation method thereof according to claim 7, characterized in that: The discharging mechanism comprises a third transmission motor (61) fixedly connected to the mixing preparation box (2); the output end of the third transmission motor (61) is fixedly connected to a third rotating shaft (62) via a coupling; the outer surface of the third rotating shaft (62) is connected to a threaded rod (63) rotatably connected to the mixing preparation box (2) via a transmission wheel and a transmission belt; the outer surface of the threaded rod (63) is threadedly matched with a pusher ring plate (64) slidably connected to the mixing preparation box (2); the outer surface of the second transmission pipe (43) is fixedly connected to a pusher plate (65); two second discharging pipes (66) are fixedly connected to the bottom of the mixing preparation box (2); a discharging plate (67) fixedly connected to the mixing preparation box (2) is arranged below the second discharging pipe (66); the bottom of the discharging plate (67) is fixedly connected to a fourth transmission motor (68); the output end of the fourth transmission motor (68) is fixedly connected to a screw rod (69) rotatably connected to the discharging plate (67) via a coupling.

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