CN113186015B - High-base-number magnesium sulfonate detergent and preparation method thereof - Google Patents
High-base-number magnesium sulfonate detergent and preparation method thereof Download PDFInfo
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- CN113186015B CN113186015B CN202110142660.3A CN202110142660A CN113186015B CN 113186015 B CN113186015 B CN 113186015B CN 202110142660 A CN202110142660 A CN 202110142660A CN 113186015 B CN113186015 B CN 113186015B
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- 239000011777 magnesium Substances 0.000 title claims abstract description 27
- 229910052749 magnesium Inorganic materials 0.000 title claims abstract description 27
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 title claims abstract description 26
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000003599 detergent Substances 0.000 title claims abstract description 19
- 239000002904 solvent Substances 0.000 claims abstract description 41
- 238000006243 chemical reaction Methods 0.000 claims abstract description 20
- 238000003756 stirring Methods 0.000 claims abstract description 20
- 239000000395 magnesium oxide Substances 0.000 claims abstract description 16
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 16
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000002253 acid Substances 0.000 claims abstract description 14
- 239000002199 base oil Substances 0.000 claims abstract description 10
- 150000007524 organic acids Chemical class 0.000 claims abstract description 9
- LJKQIQSBHFNMDV-UHFFFAOYSA-N 7-thiabicyclo[4.1.0]hepta-2,4-dien-6-ol Chemical compound C1=CC=CC2(O)C1S2 LJKQIQSBHFNMDV-UHFFFAOYSA-N 0.000 claims abstract description 6
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims abstract description 6
- 125000000217 alkyl group Chemical group 0.000 claims abstract description 6
- 239000011575 calcium Substances 0.000 claims abstract description 6
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 238000003825 pressing Methods 0.000 claims abstract description 5
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 14
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 12
- -1 alkylene anhydride Chemical class 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 9
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 8
- 239000001569 carbon dioxide Substances 0.000 claims description 7
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 5
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical group COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 4
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- 238000004821 distillation Methods 0.000 claims description 4
- 235000019253 formic acid Nutrition 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 239000005909 Kieselgur Substances 0.000 claims 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims 1
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 abstract description 8
- 239000001095 magnesium carbonate Substances 0.000 abstract description 8
- 229910000021 magnesium carbonate Inorganic materials 0.000 abstract description 8
- 239000002994 raw material Substances 0.000 abstract description 4
- 239000006185 dispersion Substances 0.000 abstract description 3
- 239000002585 base Substances 0.000 description 15
- 239000007789 gas Substances 0.000 description 10
- 239000003921 oil Substances 0.000 description 7
- 239000000654 additive Substances 0.000 description 5
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 4
- 230000000996 additive effect Effects 0.000 description 4
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 description 3
- 150000004996 alkyl benzenes Chemical class 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 239000000295 fuel oil Substances 0.000 description 3
- 238000002329 infrared spectrum Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 229960000583 acetic acid Drugs 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000012362 glacial acetic acid Substances 0.000 description 2
- 239000010763 heavy fuel oil Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000006386 neutralization reaction Methods 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 239000003973 paint Substances 0.000 description 2
- 229940014800 succinic anhydride Drugs 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- 239000004032 superbase Substances 0.000 description 2
- 150000007525 superbases Chemical class 0.000 description 2
- 229920002554 vinyl polymer Polymers 0.000 description 2
- 238000005299 abrasion Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 239000010687 lubricating oil Substances 0.000 description 1
- 239000010705 motor oil Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M135/00—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing sulfur, selenium or tellurium
- C10M135/08—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing sulfur, selenium or tellurium containing a sulfur-to-oxygen bond
- C10M135/10—Sulfonic acids or derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M177/00—Special methods of preparation of lubricating compositions; Chemical modification by after-treatment of components or of the whole of a lubricating composition, not covered by other classes
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2203/00—Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions
- C10M2203/10—Petroleum or coal fractions, e.g. tars, solvents, bitumen
- C10M2203/102—Aliphatic fractions
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2219/00—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
- C10M2219/04—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions containing sulfur-to-oxygen bonds, i.e. sulfones, sulfoxides
- C10M2219/046—Overbasedsulfonic acid salts
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2219/00—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
- C10M2219/08—Thiols; Sulfides; Polysulfides; Mercaptals
- C10M2219/082—Thiols; Sulfides; Polysulfides; Mercaptals containing sulfur atoms bound to acyclic or cycloaliphatic carbon atoms
- C10M2219/087—Thiols; Sulfides; Polysulfides; Mercaptals containing sulfur atoms bound to acyclic or cycloaliphatic carbon atoms containing hydroxy groups; Derivatives thereof, e.g. sulfurised phenols
- C10M2219/089—Overbased salts
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Lubricants (AREA)
Abstract
The invention discloses a preparation method of a high base number magnesium sulfonate detergent, which comprises the following steps: adding the solvent accelerator and the base oil into the reaction kettle at one time, and starting stirring at the stirring speed of 500r/min; adding organic acid at one time, and heating the reaction kettle to 40-45 ℃; adding magnesium oxide in four times with equal quantity, stirring for 3-5 min, stirring at constant temperature, and introducing acid gas, wherein the gas quantity is matched with the mass of the magnesium oxide, and the gas is introduced for 1.5-2 h each time; after the introduction of acid gas, the temperature of the reaction kettle is raised to 150 ℃, the pressure is reduced, all solvents are removed, the pressure is reduced until the flash point is qualified, the pressure is stopped, and a proper amount of filter aid is added for filter pressing, so that the magnesium sulfonate detergent with high base number is obtained. The magnesium sulfonate detergent with high base number is prepared by adding calcium alkyl phenol sulfide with high base number. The high-base-number calcium alkyl phenol sulfide has good dispersibility, can promote the uniform dispersion of magnesium carbonate in a system, promote the continuous progress of the reaction, increase the reaction probability of organic acid and magnesium carbonate, improve the utilization rate of magnesium carbonate, reduce the consumption of raw materials and the residual raw materials, and improve the productivity and the yield.
Description
Technical Field
The invention belongs to the technical field of lubricating oil additives, and particularly relates to a magnesium sulfonate detergent with a high base number and a preparation method thereof.
Background
Along with the continuous development of the industry in China, the large-scale heavy oil generator and turbine are widely applied, and the used raw oil, i.e. residual oil, heavy fuel oil, high sulfur-containing fuel oil and other oil products are also used more and more. However, corrosion caused by vanadium in heavy fuel oil, acid corrosion caused by sulfur and nitrogen combustibles and pollution to the environment have become an urgent task which must be solved at present, and have attracted extensive attention from all communities.
The high-base-number magnesium sulfonate has strong neutralization capability and excellent rust resistance. The paint film and carbon deposit generated by the engine are adsorbed very strongly, and the paint film and carbon deposit is mainly used for regulating high-grade internal combustion engine oil, slowing down the oxidation of the oil product, reducing the abrasion and corrosion of the engine and prolonging the service life of the oil product and the engine.
There are related disclosures in the prior art concerning the preparation of high base number magnesium sulfonates. For example, chinese patent application No. CN201410538924.7 discloses a magnesium sulfonate additive with super base number and a preparation method thereof, wherein the magnesium sulfonate additive with super base number is mainly prepared from organic solvent, base oil, methanol, alkenyl succinic anhydride, magnesium oxide, heavy alkylbenzene sulfonic acid, water, glacial acetic acid and fuel oil, and carbon dioxide is introduced in the preparation process. The magnesium sulfonate additive with ultrahigh base number has base number (TBN) up to 600mgKOH/g, magnesium content up to 14.0wt% and viscosity of 40-200cSt at 100deg.C, and has the advantages of stable structure, small viscosity, good oil solubility, and convenient use. The preparation method comprises the following steps: in an organic solvent, under the combined action of methanol, glacial acetic acid and alkenyl succinic anhydride, magnesium oxide and alkylbenzenesulfonic acid are subjected to a neutralization reaction, then carbonation reaction is carried out, an ultrahigh-base-number magnesium alkylbenzenesulfonate colloid is generated, and finally the ultrahigh-base-number magnesium sulfonate additive is obtained through filtration and distillation.
The existing preparation method has low magnesium oxide utilization rate, low productivity and low yield.
Disclosure of Invention
Aiming at the problems, the invention provides a magnesium sulfonate detergent with high base number and a preparation method thereof. The high base number magnesium sulfonate detergent contains high base number vulcanized alkyl phenol calcium, and the high dispersion property of the high base number vulcanized alkyl phenol calcium is utilized to improve the utilization rate of magnesium oxide, thereby improving the productivity and the yield.
The aim and the technical problems of the invention are realized by adopting the following technical proposal.
The invention provides a preparation method of a high base number magnesium sulfonate detergent, which comprises the following steps:
adding the solvent accelerator and the base oil into the reaction kettle at one time, and starting stirring at the stirring speed of 500r/min;
adding organic acid at one time, and heating the reaction kettle to 40-45 ℃;
adding magnesium oxide in four times with equal quantity, stirring for 3-5 min, stirring at constant temperature, and introducing acid gas, wherein the gas quantity is matched with the mass of the magnesium oxide, and the gas is introduced for 1.5-2 h each time;
after the introduction of acid gas, the temperature of the reaction kettle is raised to 150 ℃, the pressure is reduced, all solvents are removed, the pressure is reduced until the flash point is qualified, the pressure is stopped, and a proper amount of filter aid is added for filter pressing, so that the magnesium sulfonate detergent with high base number is obtained.
The preparation method is characterized in that the addition amount of the solvent accelerator is 49% by weight, the addition amount of the base oil is 19% by weight, the addition amount of the magnesium oxide is 9% by weight, the addition amount of the acid gas is 7% by weight, and the addition amount of the organic acid is 16% by weight.
The preparation method comprises the steps of preparing the solvent accelerator by using a solvent accelerator, wherein the solvent accelerator consists of a first solvent accelerator, a second solvent accelerator, a third solvent accelerator and a fourth solvent accelerator, and the mass ratio of the first solvent accelerator to the second solvent accelerator to the third solvent accelerator to the fourth solvent accelerator is 39:7:1:2.
The preparation method comprises the step of preparing the first solvent accelerator, wherein the first solvent accelerator is selected from one or two of toluene, butanol, solvent oil, ethylene glycol, methanol and ethanol; the second solvent accelerator is an alkylene anhydride; the third solvent accelerator is calcium alkyl phenol sulfide; the fourth solvent accelerator is formic acid.
The preparation method, wherein the base oil comprises 150SN or 150N.
The preparation method, wherein the organic acid is alkylbenzenesulfonic acid.
The preparation method, wherein the acid gas is carbon dioxide.
The preparation method, wherein the filter aid is diatomite filter aid.
By means of the technical scheme, the invention has at least the following advantages: the magnesium sulfonate detergent with high base number is prepared by adding the accelerator into the magnesium sulfonate detergent with high base number. The high-base-number calcium alkyl phenol sulfide has good dispersibility, can promote the uniform dispersion of magnesium carbonate in a system, promote the continuous progress of the reaction, increase the reaction probability of organic acid and magnesium carbonate, improve the utilization rate of magnesium carbonate, reduce the consumption of raw materials and the residual raw materials, and improve the productivity and the yield. The utilization rate of magnesium carbonate in the original production technology is 70-80%, and the product yield is 70-76%. The utilization rate of magnesium carbonate in the process is 76-85%, the product yield is more than or equal to 85%, and the original process is obvious.
The foregoing description is only an overview of the present invention, and is intended to provide a better understanding of the present invention, as it is embodied in the following description, with reference to the preferred embodiments of the present invention and the accompanying drawings.
Drawings
FIG. 1 is an infrared spectrum of a high base number magnesium sulfonate detergent obtained according to the preparation method of example 1 of the present invention.
Detailed Description
In order to make the technical means, the creation characteristics, the achievement of the purposes and the effects of the present invention easy to understand, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention and the accompanying drawings, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
All of the features disclosed in this specification, or all of the steps in a method or process disclosed, may be combined in any combination, except for mutually exclusive features and/or steps.
Any feature disclosed in this specification (including any accompanying claims, abstract) may be replaced by alternative features serving the same, equivalent or similar purpose, unless expressly stated otherwise. That is, each feature is one example only of a generic series of equivalent or similar features, unless expressly stated otherwise.
Example 1
According to parts by weight, 39 parts of toluene, 7 parts of vinyl anhydride, 1 part of high-base number calcium alkyl phenol sulfide, 2 parts of formic acid and 150SN 19 parts of base oil are added into a reaction kettle at one time, stirring is started, the stirring speed is 500r/min, 16 parts of alkylbenzene sulfonic acid is added at one time, and the temperature of the reaction kettle is raised to 43 ℃; adding 9 parts of magnesium oxide in four times with equal quantity, stirring for 3-5 min, stirring at constant temperature, introducing carbon dioxide, matching the gas quantity with the mass of the magnesium oxide, and introducing gas for 1.5h each time; and after the introduction of carbon dioxide, heating the reaction kettle to 150 ℃, carrying out reduced pressure distillation, removing all solvents, reducing the pressure until the flash point is qualified, stopping reducing the pressure, adding a proper amount of diatomite filter aid for filter pressing, and obtaining the magnesium sulfonate detergent with high base number.
Comparative example 1
39 parts of toluene, 7 parts of vinyl anhydride, 2 parts of formic acid and 150SN 18 parts of base oil are added into a reaction kettle at one time, stirring is started, the stirring speed is 500r/min, 15 parts of alkylbenzene sulfonic acid is added at one time, and the temperature of the reaction kettle is raised to 43 ℃; adding 9 parts of magnesium oxide in four times with equal quantity, stirring for 3-5 min, stirring at constant temperature, introducing carbon dioxide, matching the gas quantity with the mass of the magnesium oxide, and introducing gas for 1.5h each time; and after the introduction of carbon dioxide, heating the reaction kettle to 150 ℃, carrying out reduced pressure distillation, removing all solvents, reducing the pressure until the flash point is qualified, stopping reducing the pressure, adding a proper amount of diatomite filter aid for filter pressing, and obtaining the magnesium sulfonate detergent.
Test example 1 comparison of product Properties
The magnesium sulfonate detergents obtained in example 1 and comparative example 1 were tested for performance, wherein the determination of TBN (mg/g) was referenced to ASTM D2896, V100 ℃ (mm) 2 S) reference ASTM D445, turbidity (NTU) reference Q/THS-23, S (%) reference SH/T0303, the results are shown in Table 1.
Table 1 comparison of the properties of the products
Note that: samples 1 to 3 in table 1 refer to three batches of product obtained according to the method of comparative example 1; runs 1-3 are three batches of product obtained according to the method of example 1.
Test example 2 infrared spectrogram analysis
The magnesium sulfonate detergent finished product obtained in example 1 was subjected to infrared spectrum analysis, and the result is shown in fig. 1. As can be seen from the analysis of the results of FIG. 1, the infrared spectrum of the productThe graph is at wave number of 850cm -1 And 720cm -1 There is a characteristic absorption in the vicinity. The new and improved process can reach the technical index of the original process.
While the invention has been described with respect to preferred embodiments, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention, and that any such changes and modifications as described in the above embodiments are intended to be within the scope of the invention.
Claims (3)
1. The preparation method of the high base number magnesium sulfonate detergent is characterized by comprising the following steps of:
adding the solvent accelerator and the base oil into the reaction kettle at one time, and starting stirring at the stirring speed of 500r/min;
adding organic acid at one time, and heating the reaction kettle to 40-45 ℃;
adding magnesium oxide in four times with equal quantity, stirring for 3-5 min, stirring at constant temperature, and introducing acid gas, wherein the gas quantity is matched with the mass of the magnesium oxide, and the gas is introduced for 1.5-2 h each time;
after the introduction of acid gas, heating the reaction kettle to 150 ℃, carrying out reduced pressure distillation, removing all solvents, reducing the pressure until the flash point is qualified, stopping reducing the pressure, adding a proper amount of filter aid for filter pressing, and obtaining the magnesium sulfonate detergent with high base number;
the solvent accelerator consists of a first solvent accelerator, a second solvent accelerator, a third solvent accelerator and a fourth solvent accelerator, wherein the mass ratio of the first solvent accelerator to the second solvent accelerator to the third solvent accelerator to the fourth solvent accelerator is 39:7:1:2;
the first solvent accelerator is selected from one or two of toluene, butanol, solvent naphtha, glycol, methanol and ethanol; the second solvent accelerator is an alkylene anhydride; the third solvent accelerator is calcium alkyl phenol sulfide; the fourth solvent accelerator is formic acid;
the addition amount of the solvent accelerator is 49% by weight, the addition amount of the base oil is 19% by weight, the addition amount of the magnesium oxide is 9% by weight, the addition amount of the acid gas is 7% by weight, and the addition amount of the organic acid is 16% by weight;
the organic acid is alkylbenzenesulfonic acid;
the acid gas is carbon dioxide.
2. The method of claim 1, wherein the base oil comprises 150SN or 150N.
3. The method of making according to claim 1, wherein the filter aid is a diatomaceous earth filter aid.
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| CN202110142660.3A CN113186015B (en) | 2021-02-02 | 2021-02-02 | High-base-number magnesium sulfonate detergent and preparation method thereof |
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| CN202110142660.3A CN113186015B (en) | 2021-02-02 | 2021-02-02 | High-base-number magnesium sulfonate detergent and preparation method thereof |
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| CN113186015B true CN113186015B (en) | 2024-02-06 |
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| CN104403722A (en) * | 2014-10-13 | 2015-03-11 | 锦州康泰润滑油添加剂股份有限公司 | Ultrahigh-base-number magnesium sulphonate additive and preparation method thereof |
| CN106675699A (en) * | 2016-12-23 | 2017-05-17 | 新乡市瑞丰新材料股份有限公司 | Preparation method of ultra-overbased synthetic magnesium sulfonate |
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2021
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Patent Citations (9)
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