CN103122266A - Composite calcium-sulfonate-base lubricating grease and preparation method thereof - Google Patents
Composite calcium-sulfonate-base lubricating grease and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the technical field of a composite calcium-sulfonate-base grease and preparation thereof, particularly a composite calcium-sulfonate-base lubricating grease and a preparation method thereof. The preparation method of the composite calcium-sulfonate-base lubricating grease comprises the following step: 1. respectively weighing 20-30 parts by weight of high-base-number petroleum calcium sulfonate with the total base number of 200-400 mg KOH/g, and 44-55 parts by weight of high-viscosity-index base oil with the viscosity index of 90-120. The invention has the advantages of simple technique, accessible raw materials and safe working environment, is convenient for operation, and effectively lowers the energy consumption; the product obtained by the method provided by the invention has excellent properties, and can satisfy the product index requirements without adding any additive, and thus, the production input cost of the product is lower than that of any other high temperature grease; no harmful substance is generated in the product production and use process, so the composite calcium-sulfonate-base grease is harmless to the human body; and the composite calcium-sulfonate-base grease can be recycled and reutilized to maximize the use of energy sources, thereby completely satisfying the requirements of energy saving and environmental protection.
Description
Technical field
The present invention relates to the technical field of calcium sulfonate complex grease and preparation thereof, is a kind of complex calcium sulfonate grease and preparation method thereof.
Background technology
A kind of new and effective grease product of complex calcium sulfonate grease.It is by the sulfonic acid calcium soap of high base number and lipid acid calcium soap and the compound multiviscosisty base oil of inorganic calcium salt and a class that makes has the grease product of premium properties.But, still exist following problem:
1. the high base number viscosifying agent is to the thickening ability of base oil and condition each other with other Additive Properties.To consider and the consistency of base oil and the compatibleness of viscosifying agent and additive when producing;
2. the synthesis under normal pressure temperature is more than 100 degree, and long reaction time consumes energy high;
3. transforming agent methyl alcohol commonly used can evaporate with vapor form, has reduced transformation efficiency, and methanol steam is poisonous has simultaneously caused unsafe production environment;
4. during reaction with pressure, strict to the sealing requirements of the equipment such as autoclave pressure, and increased the later stage saponification, reinforced difficulty during the high temperature refining, also inconvenient observing response phenomenon simultaneously, bad control of time, energy consumption is also high;
5. high base number viscosifying agent addition is many, and low conversion rate makes production cost higher, directly affects economic benefit;
Summary of the invention
The invention provides a kind of complex calcium sulfonate grease and preparation method thereof, overcome the deficiency of above-mentioned prior art, it can effectively solve the existing complex calcium sulfonate grease method of producing and have that restriction, long reaction time, power consumption are high, the problem of low conversion rate.
One of technical scheme of the present invention realizes by following measures: a kind of complex calcium sulfonate grease, obtain as follows: the first step, raw material is the mark meter by weight, and 20 parts to 30 parts of the high base number calcium mahogany sulfonates, the viscosity index that take respectively total basicnumber and be 200mgKOH/g to 400mgKOH/g are 90 to 120 3 parts to 6 parts of 2 parts to 5 parts of 2 parts to 5 parts, 2 parts to 5 parts of 44 parts to 55 parts of high viscosity index (HVI) base oils, ten dihydroxystearic acids, calcium hydroxide, acetic acid, boric acid, 10 parts to 20 parts, water; Second step, after high base number calcium mahogany sulfonate and acetic acid are mixed, adding wherein weight is the water of the first step Raw gross weight 0.1%, then be that 60 rpms to 100 rpms, temperature are reaction 40 minutes to 60 minutes under the condition of 90 degrees centigrade to 100 degrees centigrade in stir speed (S.S.), continue to be heated to 110 degrees centigrade after reaction is completed and dewater and obtain the mixture I; The 3rd step obtained emulsion by load weighted calcium hydroxide in the first step being joined in the hot water that weight is 49 times of calcium hydroxide weight after dissolving, and the emulsion of then inciting somebody to action while hot joins and obtains the mixture II in the mixture I; The 4th step obtained boric acid solution after the boric acid that takes in the first step is joined in the hot water that weight is 19 times of boric acid weight dissolving, then while hot the boric acid solution at this temperature was joined to obtain the mixture III in the mixture II; The 5th step, ten dihydroxystearic acids that take in the first step are joined in the mixture III, and to add wherein weight be the water of the first step Raw gross weight 0.1%, then be that 80 rpms to 100 rpms, temperature are that 110 degrees centigrade to 120 degrees centigrade, time are to carry out saponification reaction under the condition of 40 minutes to 60 minutes in stir speed (S.S.), saponification reaction obtains agranular solid paste after finishing; The 6th step, be to dewater under the condition of 125 degrees centigrade to 130 degrees centigrade in temperature with the solid paste, then add the high viscosity index (HVI) base oil that takes in the first step to obtain mixing paste, the add-on of high viscosity index (HVI) base oil is 3% to 5% of the high viscosity index (HVI) base oil weight that takes in the first step, then will mix paste and carry out expanded reaction and obtain semi-solid paste, the temperature of expanded reaction is that 180 degrees centigrade, time are 40 minutes to 50 minutes; The 7th step, semi-solid paste is carried out the high temperature refining obtain refining product, the temperature of high temperature refining is that 225 degrees centigrade to 235 degrees centigrade, time are 20 minutes to 30 minutes, after the high temperature refining finishes, add the high viscosity index (HVI) base oil that takes in the first step to obtain thick liquid in the refining product, the add-on of high viscosity index (HVI) base oil is 95% to 97% of the high viscosity index (HVI) base oil weight that takes in the first step, thick liquid is stirred be cooled to 120 degrees centigrade to 130 degrees centigrade; The 8th step, adding wear preventive additive and anticorrosive additive to carry out homogenizing in thick liquid after the cooling processes, then obtain complex calcium sulfonate grease after naturally cooling to normal temperature, the add-on of anti-wear agent is 0.01 % to 0.02% of the first step Raw gross weight, and the add-on of sanitas is 0.005 % to 0.01% of the first step Raw gross weight.
Two of technical scheme of the present invention realizes by following measures: a kind of preparation method of complex calcium sulfonate grease, carry out in the steps below: the first step, raw material is the mark meter by weight, and 20 parts to 30 parts of the high base number calcium mahogany sulfonates, the viscosity index that take respectively total basicnumber and be 200mgKOH/g to 400mgKOH/g are 90 to 120 3 parts to 6 parts of 2 parts to 5 parts of 2 parts to 5 parts, 2 parts to 5 parts of 44 parts to 55 parts of high viscosity index (HVI) base oils, ten dihydroxystearic acids, calcium hydroxide, acetic acid, boric acid, 10 parts to 20 parts, water; Second step, after high base number calcium mahogany sulfonate and acetic acid are mixed, adding wherein weight is the water of the first step Raw gross weight 0.1%, then be that 60 rpms to 100 rpms, temperature are reaction 40 minutes to 60 minutes under the condition of 90 degrees centigrade to 100 degrees centigrade in stir speed (S.S.), continue to be heated to 110 degrees centigrade after reaction is completed and dewater and obtain the mixture I; The 3rd step obtained emulsion by load weighted calcium hydroxide in the first step being joined in the hot water that weight is 49 times of calcium hydroxide weight after dissolving, and the emulsion of then inciting somebody to action while hot joins and obtains the mixture II in the mixture I; The 4th step obtained boric acid solution after the boric acid that takes in the first step is joined in the hot water that weight is 19 times of boric acid weight dissolving, then while hot the boric acid solution at this temperature was joined to obtain the mixture III in the mixture II; The 5th step, ten dihydroxystearic acids that take in the first step are joined in the mixture III, and to add wherein weight be the water of the first step Raw gross weight 0.1%, then be that 80 rpms to 100 rpms, temperature are that 110 degrees centigrade to 120 degrees centigrade, time are to carry out saponification reaction under the condition of 40 minutes to 60 minutes in stir speed (S.S.), saponification reaction obtains agranular solid paste after finishing; The 6th step, be to dewater under the condition of 125 degrees centigrade to 130 degrees centigrade in temperature with the solid paste, then add the high viscosity index (HVI) base oil that takes in the first step to obtain mixing paste, the add-on of high viscosity index (HVI) base oil is 3% to 5% of the high viscosity index (HVI) base oil weight that takes in the first step, then will mix paste and carry out expanded reaction and obtain semi-solid paste, the temperature of expanded reaction is that 180 degrees centigrade, time are 40 minutes to 50 minutes; The 7th step, semi-solid paste is carried out the high temperature refining obtain refining product, the temperature of high temperature refining is that 225 degrees centigrade to 235 degrees centigrade, time are 20 minutes to 30 minutes, after the high temperature refining finishes, add the high viscosity index (HVI) base oil that takes in the first step to obtain thick liquid in the refining product, the add-on of high viscosity index (HVI) base oil is 95% to 97% of the high viscosity index (HVI) base oil weight that takes in the first step, thick liquid is stirred be cooled to 120 degrees centigrade to 130 degrees centigrade; The 8th step, adding wear preventive additive and anticorrosive additive to carry out homogenizing in thick liquid after the cooling processes, then obtain complex calcium sulfonate grease after naturally cooling to normal temperature, the add-on of anti-wear agent is 0.01 % to 0.02% of the first step Raw gross weight, and the add-on of sanitas is 0.005 % to 0.01% of the first step Raw gross weight.
The below is the further optimization and/or improvements to the foregoing invention technical scheme:
In the above-mentioned the first step, the 6th step and the 7th step, the sticking model that refers to that base oil can be oil product of height used is the mixture of the mineral oil of deep refining of the mixture of the mineral oil of deep refining of the mixture of the mineral oil of deep refining of 150BS and synthetic oil or 150N and synthetic oil or 200N and synthetic oil or is the synthetic oil of PAO series.
In above-mentioned the 8th step anti-wear agent used can be T362 without sulphur phosphorus chlorine extreme pressure anti-wear additives or T366 without sulphur phosphorus chlorine extreme pressure anti-wear additives, sanitas is dialkyl dithiocarbamate series sanitas.
When above-mentioned second step adds water, can add water one time in 5 minutes clockwise high base number calcium mahogany sulfonates and acetic acid, adding water inventory is the first step Raw gross weight 0.1%.
Above-mentioned the 5th step, added water was that temperature can be the hot water of 50 degrees centigrade to 80 degrees centigrade when adding water, and added hot water in 5 minutes clockwise contains the mixture III of ten dihydroxystearic acids, and the total amount that adds of hot water is the first step Raw gross weight 0.1%.
Processing method of the present invention is simple, handled easily, and raw material is easy to get, and effectively reduces energy consumption, Working environment safety; And the excellent product performance that the inventive method obtains does not need to add additive can satisfy the product index requirement, so relative other high temperature greases of products production input cost are lower; Products production, use procedure unharmful substance produce simultaneously, to not injury of human body, can reclaim cycling and reutilization, the energy are used maximize, and meet the energy-saving and environmental protection requirement fully.
Embodiment
The present invention is not subjected to the restriction of following embodiment, can determine concrete embodiment according to technical scheme of the present invention and practical situation.
The invention will be further described below in conjunction with embodiment:
Embodiment 1, this complex calcium sulfonate grease obtains by following preparation method: the first step, raw material is the mark meter by weight, and 20 parts to 30 parts of the high base number calcium mahogany sulfonates, the viscosity index that take respectively total basicnumber and be 200mgKOH/g to 400mgKOH/g are 90 to 120 3 parts to 6 parts of 2 parts to 5 parts of 2 parts to 5 parts, 2 parts to 5 parts of 44 parts to 55 parts of high viscosity index (HVI) base oils, ten dihydroxystearic acids, calcium hydroxide, acetic acid, boric acid, 10 parts to 20 parts, water; Second step, after high base number calcium mahogany sulfonate and acetic acid are mixed, adding wherein weight is the water of the first step Raw gross weight 0.1%, then be that 60 rpms to 100 rpms, temperature are reaction 40 minutes to 60 minutes under the condition of 90 degrees centigrade to 100 degrees centigrade in stir speed (S.S.), continue to be heated to 110 degrees centigrade after reaction is completed and dewater and obtain the mixture I; The 3rd step obtained emulsion by load weighted calcium hydroxide in the first step being joined in the hot water that weight is 49 times of calcium hydroxide weight after dissolving, and the emulsion of then inciting somebody to action while hot joins and obtains the mixture II in the mixture I; The 4th step obtained boric acid solution after the boric acid that takes in the first step is joined in the hot water that weight is 19 times of boric acid weight dissolving, then while hot the boric acid solution at this temperature was joined to obtain the mixture III in the mixture II; The 5th step, ten dihydroxystearic acids that take in the first step are joined in the mixture III, and to add wherein weight be the water of the first step Raw gross weight 0.1%, then be that 80 rpms to 100 rpms, temperature are that 110 degrees centigrade to 120 degrees centigrade, time are to carry out saponification reaction under the condition of 40 minutes to 60 minutes in stir speed (S.S.), saponification reaction obtains agranular solid paste after finishing; The 6th step, be to dewater under the condition of 125 degrees centigrade to 130 degrees centigrade in temperature with the solid paste, then add the high viscosity index (HVI) base oil that takes in the first step to obtain mixing paste, the add-on of high viscosity index (HVI) base oil is 3% to 5% of the high viscosity index (HVI) base oil weight that takes in the first step, then will mix paste and carry out expanded reaction and obtain semi-solid paste, the temperature of expanded reaction is that 180 degrees centigrade, time are 40 minutes to 50 minutes; The 7th step, semi-solid paste is carried out the high temperature refining obtain refining product, the temperature of high temperature refining is that 225 degrees centigrade to 235 degrees centigrade, time are 20 minutes to 30 minutes, after the high temperature refining finishes, add the high viscosity index (HVI) base oil that takes in the first step to obtain thick liquid in the refining product, the add-on of high viscosity index (HVI) base oil is 95% to 97% of the high viscosity index (HVI) base oil weight that takes in the first step, thick liquid is stirred be cooled to 120 degrees centigrade to 130 degrees centigrade; The 8th step, adding wear preventive additive and anticorrosive additive to carry out homogenizing in thick liquid after the cooling processes, then obtain complex calcium sulfonate grease after naturally cooling to normal temperature, the add-on of anti-wear agent is 0.01 % to 0.02% of the first step Raw gross weight, and the add-on of sanitas is 0.005 % to 0.01% of the first step Raw gross weight.Acetic acid in second step can replace with other lower fat classes such as propionic acid, calcium hydroxide in the 3rd step can replace with lime, second step dewaters and the 6th step when dewatering to 130 degrees celsius at 125 degrees centigrade at 110 degrees centigrade, because at this temperature, water does not exist substantially, therefore as long as temperature reaches this value, namely be considered as dewatering complete.
Embodiment 2, this complex calcium sulfonate grease obtains by following preparation method: the first step, raw material is the mark meter by weight, and 20 parts to 30 parts of high base number calcium mahogany sulfonates, the viscosity index that takes respectively total basicnumber and be 200mgKOH/g to 400mgKOH/g is 3 parts of 2 parts of 2 parts, 2 parts of 90 to 120 44 parts to 55 parts of high viscosity index (HVI) base oils, ten dihydroxystearic acids or 5 parts, calcium hydroxide or 5 parts, acetic acid or 5 parts, boric acid or 6 parts, 10 parts or 20 parts, water; Second step, after high base number calcium mahogany sulfonate and acetic acid are mixed, adding wherein weight is the water of the first step Raw gross weight 0.1%, then be that 60 rpms or 100 rpms, temperature are reaction 40 minutes or 60 minutes under the condition of 90 degrees centigrade or 100 degrees centigrade in stir speed (S.S.), continue to be heated to 110 degrees centigrade after reaction is completed and dewater and obtain the mixture I; The 3rd step obtained emulsion by load weighted calcium hydroxide in the first step being joined in the hot water that weight is 49 times of calcium hydroxide weight after dissolving, and the emulsion of then inciting somebody to action while hot joins and obtains the mixture II in the mixture I; The 4th step obtained boric acid solution after the boric acid that takes in the first step is joined in the hot water that weight is 19 times of boric acid weight dissolving, then while hot the boric acid solution at this temperature was joined to obtain the mixture III in the mixture II; The 5th step, ten dihydroxystearic acids that take in the first step are joined in the mixture III, and to add wherein weight be the water of the first step Raw gross weight 0.1%, then be that 80 rpms or 100 rpms, temperature are 110 degrees centigrade or 120 degrees centigrade, time to be to carry out saponification reaction under the condition of 40 minutes or 60 minutes in stir speed (S.S.), saponification reaction obtains agranular solid paste after finishing; The 6th step, be to dewater under the condition of 125 degrees centigrade or 130 degrees centigrade in temperature with the solid paste, then add the high viscosity index (HVI) base oil that takes in the first step to obtain mixing paste, the add-on of high viscosity index (HVI) base oil is 3% or 5% of the high viscosity index (HVI) base oil weight that takes in the first step, then will mix paste and carry out expanded reaction and obtain semi-solid paste, the temperature of expanded reaction is that 180 degrees centigrade, time are 40 minutes or 50 minutes; The 7th step, semi-solid paste is carried out the high temperature refining obtain refining product, the temperature of high temperature refining is that 225 degrees centigrade or 235 degrees centigrade, time are 20 minutes or 30 minutes, after the high temperature refining finishes, add the high viscosity index (HVI) base oil that takes in the first step to obtain thick liquid in the refining product, the add-on of high viscosity index (HVI) base oil is 95% or 97% of the high viscosity index (HVI) base oil weight that takes in the first step, thick liquid is stirred be cooled to 120 degrees centigrade or 130 degrees centigrade; The 8th step, adding wear preventive additive and anticorrosive additive to carry out homogenizing in thick liquid after the cooling processes, then obtain complex calcium sulfonate grease after naturally cooling to normal temperature, the add-on of anti-wear agent is 0.01 % or 0.02% of the first step Raw gross weight, and the add-on of sanitas is 0.005 % or 0.01% of the first step Raw gross weight.
Embodiment 3, preferred as above-described embodiment, in the first step, the 6th step and the 7th step, height used is sticking refers to that base oil is the mixture of the mineral oil of deep refining of the mixture of the mineral oil of deep refining of the mixture of the mineral oil of the model of the oil product deep refining that is 150BS and synthetic oil or 150N and synthetic oil or 200N and synthetic oil or is the synthetic oil of PAO series.
Embodiment 4, preferred as above-described embodiment, and in the 8th step, anti-wear agent used is T362 without sulphur phosphorus chlorine extreme pressure anti-wear additives or T366 without sulphur phosphorus chlorine extreme pressure anti-wear additives, sanitas is dialkyl dithiocarbamate series sanitas.
Embodiment 5, and preferred as above-described embodiment when second step adds water, adds water one time in 5 minutes clockwise high base number calcium mahogany sulfonates and acetic acid, and adding water inventory is the first step Raw gross weight 0.1%.
Embodiment 6, preferred as above-described embodiment, the 5th step, when adding water, added water was that temperature can be the hot water of 50 degrees centigrade to 80 degrees centigrade, and add hot water in 5 minutes clockwise contains the mixture III of ten dihydroxystearic acids, the total amount that adds of hot water is the first step Raw gross weight 0.1%.
With existing complex calcium sulfonate grease as a control group, the complex calcium sulfonate grease that obtains according to the above embodiment of the present invention as experimental group from the Drawing cone in-degree, extend Drawing cone in-degree, anti-water drenching energy (water pouring number of dropouts), Stencil oil-dividing, dropping point, rustless property (rust protection), non-corrosibility (copper corrosion) and abrasion resistance etc. compare analysis as detecting index, result is as shown in table 1, and in table 1, data are mean value.
By to the data analysis in form, Drawing cone in-degree under 25 degrees centigrade, experimental group is better than control group, the mobility of illustrative experiment group is better than the mobility of control group, and extending Drawing cone in-degree (10,000 times)/0.1mm and extending Drawing cone in-degree (100,000 times)/0.1mm proves that further the mobility of experimental group is better than the mobility of control group; Water drenches the number of dropouts experimental group and is better than control group, the water absorbing properties of illustrative experiment group is less than the control group water absorbing properties, this has determined lubricating oil consistency change in use, and the hydrolysis ability that water absorbing properties is little is little, consistency change is little, can effectively guarantee lubricant effect; Stencil oil-dividing can show that minute speed oil of the complex calcium sulfonate grease that the above embodiment of the present invention obtains is not more than 2%, illustrates that the stability of the complex calcium sulfonate grease that the above embodiment of the present invention obtains is good; The dropping point of experimental group is greater than the dropping point of control group, and the illustrative experiment group has the range of application wider than control group; The copper corrosion of experimental group detects as qualified, illustrates in use, need not additionally add rut preventives, therefore, in use, can reduce use cost; The rust protection detection of experimental group is 1 grade, illustrates in use, need not additionally add rust-inhibiting additive, therefore, in use, can reduce use cost; Extreme pressure and antiwear behavior PB value experimental group is less than control group, and the illustrative experiment group less than control group, therefore, is used the time of utilizing that experimental group can extension device to the wearing and tearing ability of equipment; Extreme pressure and antiwear behavior PD value experimental group is greater than control group, and the maximal work ability of illustrative experiment group is better than control group; The resistance to abrasion experimental group is less than control group, and the wear intensity the when lubricating grease that uses experimental group is described between equipment is the wear intensity between equipment during less than the lubricating grease that uses control group.
Above analytic explanation is the grease product that a class has premium properties according to the complex calcium sulfonate grease that the above embodiment of the present invention obtains.
Table 1
| Project | Control group | Experimental group | Detection method |
| The Drawing cone in-degree, 25 ℃, 0.1mm | 230 | 235 | GB/T269 |
| Extend Drawing cone in-degree (10,000 times)/0.1mm | 235 | 238 | GB/T269 |
| Extend Drawing cone in-degree (100,000 times)/0.1mm | 239 | 241 | GB/T269 |
| Water pouring number of dropouts (38 ℃, 1h)/%＜= | 0.69 | 0.5 | SH/T0109 |
| Stencil oil-dividing (100 ℃ * 24h), %＜= | 2 | 2 | SH/T0324 |
| Dropping point ， ℃＞= | 290 | 320 | GB/T4929 |
| Copper corrosion (T2,100 ℃ * 24h) | The copper sheet color is constant | Qualified | GB/T7326B |
| Rust protection (52 ℃ * 48h), level | 1 | 1 | GB/T5018 |
| Extreme pressure and antiwear behavior PB value N＞= | 638 | 650 | GB/T3142 |
| Extreme pressure and antiwear behavior PD value N＞= | 4905 | 5000 | GB/T3142 |
| Resistance to abrasion (392N, 1h, 1200r/min)/mm＜= | 0.39 | 0.37 | GB/T3142 |
Claims (10)
1. complex calcium sulfonate grease, it is characterized in that obtaining as follows: the first step, raw material is the mark meter by weight, and 20 parts to 30 parts of the high base number calcium mahogany sulfonates, the viscosity index that take respectively total basicnumber and be 200mgKOH/g to 400mgKOH/g are 90 to 120 3 parts to 6 parts of 2 parts to 5 parts of 2 parts to 5 parts, 2 parts to 5 parts of 44 parts to 55 parts of high viscosity index (HVI) base oils, ten dihydroxystearic acids, calcium hydroxide, acetic acid, boric acid, 10 parts to 20 parts, water; Second step, after high base number calcium mahogany sulfonate and acetic acid are mixed, adding wherein weight is the water of the first step Raw gross weight 0.1%, then be that 60 rpms to 100 rpms, temperature are reaction 40 minutes to 60 minutes under the condition of 90 degrees centigrade to 100 degrees centigrade in stir speed (S.S.), continue to be heated to 110 degrees centigrade after reaction is completed and dewater and obtain the mixture I; The 3rd step obtained emulsion by load weighted calcium hydroxide in the first step being joined in the hot water that weight is 49 times of calcium hydroxide weight after dissolving, and the emulsion of then inciting somebody to action while hot joins and obtains the mixture II in the mixture I; The 4th step obtained boric acid solution after the boric acid that takes in the first step is joined in the hot water that weight is 19 times of boric acid weight dissolving, then while hot the boric acid solution at this temperature was joined to obtain the mixture III in the mixture II; The 5th step, ten dihydroxystearic acids that take in the first step are joined in the mixture III, and to add wherein weight be the water of the first step Raw gross weight 0.1%, then be that 80 rpms to 100 rpms, temperature are that 110 degrees centigrade to 120 degrees centigrade, time are to carry out saponification reaction under the condition of 40 minutes to 60 minutes in stir speed (S.S.), saponification reaction obtains agranular solid paste after finishing; The 6th step, be to dewater under the condition of 125 degrees centigrade to 130 degrees centigrade in temperature with the solid paste, then add the high viscosity index (HVI) base oil that takes in the first step to obtain mixing paste, the add-on of high viscosity index (HVI) base oil is 3% to 5% of the high viscosity index (HVI) base oil weight that takes in the first step, then will mix paste and carry out expanded reaction and obtain semi-solid paste, the temperature of expanded reaction is that 180 degrees centigrade, time are 40 minutes to 50 minutes; The 7th step, semi-solid paste is carried out the high temperature refining obtain refining product, the temperature of high temperature refining is that 225 degrees centigrade to 235 degrees centigrade, time are 20 minutes to 30 minutes, after the high temperature refining finishes, add the high viscosity index (HVI) base oil that takes in the first step to obtain thick liquid in the refining product, the add-on of high viscosity index (HVI) base oil is 95% to 97% of the high viscosity index (HVI) base oil weight that takes in the first step, thick liquid is stirred be cooled to 120 degrees centigrade to 130 degrees centigrade; The 8th step, adding wear preventive additive and anticorrosive additive to carry out homogenizing in thick liquid after the cooling processes, then obtain complex calcium sulfonate grease after naturally cooling to normal temperature, the add-on of anti-wear agent is 0.01 % to 0.02% of the first step Raw gross weight, and the add-on of sanitas is 0.005 % to 0.01% of the first step Raw gross weight.
2. complex calcium sulfonate grease according to claim 1 is characterized in that height used in the first step, the 6th step and the 7th step is sticking and refers to that base oil is the mixture of the mineral oil of deep refining of the mixture of the mineral oil of deep refining of the mixture of the mineral oil of the model of the oil product deep refining that is 150BS and synthetic oil or 150N and synthetic oil or 200N and synthetic oil or is the synthetic oil of PAO series.
3. complex calcium sulfonate grease according to claim 1 and 2, it is characterized in that in the 8th step that anti-wear agent used is T362 without sulphur phosphorus chlorine extreme pressure anti-wear additives or T366 without sulphur phosphorus chlorine extreme pressure anti-wear additives, sanitas is dialkyl dithiocarbamate series sanitas.
4. according to claim 1 and 2 or 3 described complex calcium sulfonate greases when it is characterized in that second step adds water, add water one time in 5 minutes clockwise high base number calcium mahogany sulfonates and acetic acid, adding water inventory is the first step Raw gross weight 0.1%.
5. according to claim 1 and 2 or 3 or 4 described complex calcium sulfonate greases, when it is characterized in that the 5th step added water, added water is that temperature is the hot water of 50 degrees centigrade to 80 degrees centigrade, and add hot water in 5 minutes clockwise contains the mixture III of ten dihydroxystearic acids, the total amount that adds of hot water is the first step Raw gross weight 0.1%.
6. the preparation method of a complex calcium sulfonate grease, it is characterized in that carrying out in the steps below: the first step, raw material is the mark meter by weight, and 20 parts to 30 parts of the high base number calcium mahogany sulfonates, the viscosity index that take respectively total basicnumber and be 200mgKOH/g to 400mgKOH/g are 90 to 120 3 parts to 6 parts of 2 parts to 5 parts of 2 parts to 5 parts, 2 parts to 5 parts of 44 parts to 55 parts of high viscosity index (HVI) base oils, ten dihydroxystearic acids, calcium hydroxide, acetic acid, boric acid, 10 parts to 20 parts, water; Second step, after high base number calcium mahogany sulfonate and acetic acid are mixed, adding wherein weight is the water of the first step Raw gross weight 0.1%, then be that 60 rpms to 100 rpms, temperature are reaction 40 minutes to 60 minutes under the condition of 90 degrees centigrade to 100 degrees centigrade in stir speed (S.S.), continue to be heated to 110 degrees centigrade after reaction is completed and dewater and obtain the mixture I; The 3rd step obtained emulsion by load weighted calcium hydroxide in the first step being joined in the hot water that weight is 49 times of calcium hydroxide weight after dissolving, and the emulsion of then inciting somebody to action while hot joins and obtains the mixture II in the mixture I; The 4th step obtained boric acid solution after the boric acid that takes in the first step is joined in the hot water that weight is 19 times of boric acid weight dissolving, then while hot the boric acid solution at this temperature was joined to obtain the mixture III in the mixture II; The 5th step, ten dihydroxystearic acids that take in the first step are joined in the mixture III, and to add wherein weight be the water of the first step Raw gross weight 0.1%, then be that 80 rpms to 100 rpms, temperature are that 110 degrees centigrade to 120 degrees centigrade, time are to carry out saponification reaction under the condition of 40 minutes to 60 minutes in stir speed (S.S.), saponification reaction obtains agranular solid paste after finishing; The 6th step, be to dewater under the condition of 125 degrees centigrade to 130 degrees centigrade in temperature with the solid paste, then add the high viscosity index (HVI) base oil that takes in the first step to obtain mixing paste, the add-on of high viscosity index (HVI) base oil is 3% to 5% of the high viscosity index (HVI) base oil weight that takes in the first step, then will mix paste and carry out expanded reaction and obtain semi-solid paste, the temperature of expanded reaction is that 180 degrees centigrade, time are 40 minutes to 50 minutes; The 7th step, semi-solid paste is carried out the high temperature refining obtain refining product, the temperature of high temperature refining is that 225 degrees centigrade to 235 degrees centigrade, time are 20 minutes to 30 minutes, after the high temperature refining finishes, add the high viscosity index (HVI) base oil that takes in the first step to obtain thick liquid in the refining product, the add-on of high viscosity index (HVI) base oil is 95% to 97% of the high viscosity index (HVI) base oil weight that takes in the first step, thick liquid is stirred be cooled to 120 degrees centigrade to 130 degrees centigrade; The 8th step, adding wear preventive additive and anticorrosive additive to carry out homogenizing in thick liquid after the cooling processes, then obtain complex calcium sulfonate grease after naturally cooling to normal temperature, the add-on of anti-wear agent is 0.01 % to 0.02% of the first step Raw gross weight, and the add-on of sanitas is 0.005 % to 0.01% of the first step Raw gross weight.
7. the preparation method of complex calcium sulfonate grease according to claim 6 is characterized in that height used in the first step, the 6th step and the 7th step is sticking and refers to that base oil is the mixture of the mineral oil of deep refining of the mixture of the mineral oil of deep refining of the mixture of the mineral oil of the model of the oil product deep refining that is 150BS and synthetic oil or 150N and synthetic oil or 200N and synthetic oil or is the synthetic oil of PAO series.
8. the preparation method of according to claim 6 or 7 described complex calcium sulfonate greases, it is characterized in that in the 8th step that anti-wear agent used is T362 without sulphur phosphorus chlorine extreme pressure anti-wear additives or T366 without sulphur phosphorus chlorine extreme pressure anti-wear additives, sanitas is dialkyl dithiocarbamate series sanitas.
9. the preparation method of according to claim 6 or 7 or 8 described complex calcium sulfonate greases when it is characterized in that second step adds water, adds water one time in 5 minutes clockwise high base number calcium mahogany sulfonates and acetic acid, adding water inventory is the first step Raw gross weight 0.1%.
10. the preparation method of according to claim 6 or 7 or 8 or 9 described complex calcium sulfonate greases, when it is characterized in that the 5th step added water, added water is that temperature is the hot water of 50 degrees centigrade to 80 degrees centigrade, and add hot water in 5 minutes clockwise contains the mixture III of ten dihydroxystearic acids, the total amount that adds of hot water is the first step Raw gross weight 0.1%.
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| CN104450116A (en) * | 2013-09-13 | 2015-03-25 | 中国石油化工股份有限公司 | Calcium sulfonate-calcium naphthenate-based urea octamer grease and preparation method thereof |
| CN104449959A (en) * | 2013-09-13 | 2015-03-25 | 中国石油化工股份有限公司 | High-base number composite calcium-based grease and preparation method thereof |
| CN106118819A (en) * | 2016-06-24 | 2016-11-16 | 沈阳理工大学 | Neopentyl polyol ester contains the octadecane epoxide nitrogen lubricating oil for Calcium pyroborate |
| CN106147960A (en) * | 2016-06-24 | 2016-11-23 | 沈阳理工大学 | Neopentyl polyol ester adds the environment-protective lubricant oil of the multiple additives such as nitrogen-containing borate |
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