CN101928239B - Method for preparing calcium sulfonate with high base number - Google Patents
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Abstract
The invention relates to a method for preparing calcium sulfonate with high base number. In the method, alkyl benzene sulfonic acid and/or petroleum sulfonic acid serve as raw materials, low molecular alcohol serves as accelerating agent, calcium oxide and/or calcium hydroxide serve as calcifying agent; firstly, neutralization reaction is carried out to generate calcium sulfonate; then carbonation reaction is carried out for twice, post-treating agent is added for reaction; finally, alcohol, water, solvent and solid residue are removed to obtain the calcium sulfonate with high base number. The product of the invention is especially suitable for preparing lubricating grease, can shorten conversion time of calcium sulfonate crystal form, improve high-temperature bproperty and anti-moisture performance of the lubricating grease and satisfy the demands of high-performance lubricating grease.
Description
Technical field
The present invention relates to a kind of preparation method of calcium sulfonate with high base number.
Background technology
Complex calcium sulfonate grease is the novel lubricating grease of a class, have excellent extreme pressure property, abrasion resistance, water repelling property, salt fog resistance performance and Corrosion Protection, and dropping point is high, Heat stability is good, is widely used in the industries such as automobile, iron and steel, mine, papermaking.
For a long time, it is raw material that complex calcium sulfonate grease all directly adopts newton's body calcium sulphonate, calcium carbonate in newton's body calcium sulphonate is unbodied, and the calcium sulphonate in the complex calcium sulfonate grease is the non-newtonian fluid calcium sulphonate, calcium carbonate wherein is calcite type, therefore in the preparation process of complex calcium sulfonate grease, newton's body calcium sulphonate need to be converted into the non-newtonian fluid calcium sulphonate.
Patent about the calcium sulfonate with high base number of newton's body and overbased calcium sulphonate is very many, such as US4427559, US4604219, US4879053, US4879053, US4929373, US4810396, US51086309, EP0515062, EP0949322, US6015778, US4560489 etc., its preparation method is generally: take sulfonic acid or calcium sulphonate as raw material, adopting all kinds of low mass molecule alcohols is promotor, pass into carbonic acid gas and carry out carbonation reaction, heat up after reaction finishes and dewater, obtain calcium sulfonate with high base number through aftertreatment.The calcium sulfonate with high base number of above-mentioned patent (base number is greater than 300mgKOH/g) and overbased calcium sulphonate (base number is greater than 395mgKOH/g) are mainly used in I. C. engine oil and the technical oils, play solubilising, dispersion, neutralization, the effect such as antirust.
Lubricating grease requires calcium sulphonate to have preferably extreme pressure anti-wear, and requires calcium sulphonate to have in excellent detergency, dispersiveness and the acid and performance in the lubricating oil.Prepare lubricating grease with existing newton's body calcium sulphonate and can have some problems, for example: newton's body calcium sulphonate conversion rate is slow or changing effect is bad, the properties of the lubricating grease after the conversion is not good etc., has so just limited the further application of calcium sulphonate in lubricating grease.
Summary of the invention
The invention provides a kind of preparation method of calcium sulfonate with high base number, the resulting product of the method is particularly useful for making lubricating grease.The present invention also provides the method resulting product.
Among the present invention, except specifying, all raw material consumptions are all take sulfonic acid weight as 100 parts.
Method provided by the present invention comprises:
(1) varsol, neutral oil, C1～C4 alcohol, calcium oxide and/or calcium hydroxide, water are mixed with sulfonic acid, carry out neutralization reaction;
(2) pass into carbonic acid gas, carry out the carbonation reaction first time;
(3) add calcium oxide and/or calcium hydroxide, pass into carbonic acid gas, carry out the carbonation reaction second time;
(4) adding concentration is the inorganic salt solution of 10～60wt%, consumption is 5～100 parts, react 30～120mi n between 40～60 ℃, wherein inorganic salt are selected from one or more in alkali metal chloride, alkaline carbonate, alkali metal sulfates, alkaline earth metal chloride, alkaline earth metal sulphate, ammonium chloride, volatile salt, the ammonium sulfate;
(5) remove alcohol, water, solvent, promotor and solid residue after, obtain product.
Described varsol both can be alkane, and also aromatic hydrocarbon is preferably one or more in 60～180 ℃ straight-run spirit, octane, benzene, toluene and dimethylbenzene of boiling range.The effect of solvent is to provide a reacting environment to neutralization reaction and carbonation reaction.
Described neutral oil is that 100 ℃ of kinematic viscosity are 2～6mm
2The lubricant base of/S is preferably the oil of the old three cover art breading of 100SN, 150SN, lubricating oil and in the hydrofined oil one or more.The effect of neutral oil is the place that a stable dispersion is provided to calcium sulfonate with high base number.
Described C1～C4 alcohol is preferably one or more in methyl alcohol, ethanol, propyl alcohol, butanols and the ethylene glycol.The Main Function of alcohol is the carrier of inorganic phase and organic phase, so that the rate of mass transfer between the gas, liquid, solid three-phase is faster in the reaction mixture, oil phase and water mix, and makes reaction be easy to carry out.The prior effect of alcohol is to help to form the additive colloidal particle, and is therefore essential in reaction.
The content of the impurity in calcium oxide and/or the calcium hydroxide should be low as far as possible, the purity of preferential oxidation calcium and/or calcium hydroxide 〉=95%.
Described sulfonic acid is alkyl benzene sulphonate (ABS) and/or mahogany acid.In the alkyl benzene sulphonate (ABS), the alkyl carbon number is 8～30.Described alkyl benzene sulphonate (ABS) comprises the prepared sulfonic acid of by product-high boiling material of producing dodecylbenzene, mainly be dialkyl benzene, monoalkylated benzenes in this alkylbenzene, also has indane, hexichol alkyl etc. is difficult for the material of sulfonation, the character of high boiling material sulfonic acid is inferior to linear alkyl benzene sulphonic acid, but still can prepare the product of this patent.Described mahogany acid is obtained behind oversulfonate by petroleum fractions, and petroleum fractions generally is the cut of underpressure distillation, the two wires oil that for example reduces pressure, decompression third fractional oil, or the four lines oil of reducing pressure, wherein contain can sulfonation aromatic component.
Described alkyl benzene sulphonate (ABS) or mahogany acid can make by traditional oleum sulfonation, also can obtain by SO 3 sulfonated.
In the step (1), the consumption of C1～C4 alcohol is 20～200 parts, is preferably 50～150 parts; The consumption of varsol is 200～800 parts, is preferably 300～600 parts; The consumption of neutral oil is 50～300 parts, is preferably 120～250 parts; The consumption of calcium oxide and/or calcium hydroxide is 15～150 parts, is preferably 50～100 parts; The consumption of water is 10～50 parts, is preferably 20～40 parts; Temperature of reaction is 40～60 ℃, is preferably 45～55 ℃, and the reaction times is 20～60min.
In step (2) and (3), the intake of carbonic acid gas is 60～140% of theoretical value; The speed that passes into of carbonic acid gas is preferably 0.001～0.004ml/ming; The temperature of carbonation reaction is 40～60 ℃, is preferably 45～55 ℃.
In the step (3), the consumption of calcium oxide and/or calcium hydroxide is 50～300 parts, is preferably 100～150 parts.
In the step (4), the consumption of inorganic salt solution is preferably 10～50 parts; Inorganic salt are preferably one or more in calcium chloride, sodium-chlor, yellow soda ash, salt of wormwood, sodium sulfate and the ammonium sulfate; Temperature of reaction is preferably 45～55 ℃.
The secondary accelerator that also can add 2～50 parts in the step (1) preferably adds 10～30 parts secondary accelerator; Wherein, secondary accelerator is one or more in alcohol, phenol, carboxylic acid, carboxylicesters, carboxylic acid anhydride, the acid amides, and its carbon number is 9～200.Add secondary accelerator, can further improve product performance.
In the step (1), water can replace with alkaline aqueous solution, and described alkaline aqueous solution is selected from one or more in ammonia soln, alkali metal hydroxide aqueous solution and the alkaline earth metal hydroxides aqueous solution.Use alkaline aqueous solution to be conducive to neutralization reaction, can further improve the performance of product.
The concentration of described alkaline aqueous solution is preferably 5wt%～35wt%.
The present invention also provides the sulfonate with high base number that obtains with aforesaid method calcium product, and this product is in preparation during lubricating grease, and the time that is converted into calcite type calcium carbonate by amorphous calcium carbonate in the time of 80 ℃ is 20～100min.
Calcium sulfonate with high base number of the prior art, be mainly used in I. C. engine oil and the technical oils, play solubilising, dispersion, neutralization, the effect such as antirust, can there be some problems during with its synthetic grease, slow or changing effect is bad such as newton's body calcium sulphonate conversion rate, the properties of the lubricating grease after the conversion is not good etc.The resulting calcium sulfonate with high base number of the present invention is particularly useful for making lubricating grease.When preparation lubricating grease, it is fast that amorphous calcium carbonate is converted into the speed of crystal type calcium carbonate, and the crystal of calcium carbonate transforms fully, and the grease of calcium sulfonic acid after the conversion has excellent extreme pressure property, high-temperature behavior and water repelling property.
Embodiment
Further specify by the following examples the present invention.
Embodiment 1
In with 500 milliliters of there-necked flasks of motor agitators and prolong, add 150 milliliters in gasoline (industrial goods), add methyl alcohol 23.7 grams, distilled water 6 grams, 150SN neutral oil 43 grams (production of Sinopec Yanshan Petrochemical company), 4-dodecylphenol 4 grams, calcium oxide 16.5 grams, dodecylbenzene high boiling material sulfonic acid 21.6 grams, the control temperature of reaction is at 45～50 ℃, behind the neutralization reaction 30mi n after adding, pass into carbonic acid gas, Ventilation Rate between 0.062L/min, intake reach theoretical value 85% the time, add remaining 25 the gram calcium oxide, continue to pass into carbonic acid gas and carry out carbonation reaction, when carbonic acid gas reach theoretical value 85% the time, stop ventilation, add sal volatile 5 grams of 20wt%, at 45～50 ℃ of reaction 30min, then be warmed up to 120 ℃ of dealcoholysis, water.Add 100 milliliters of gasoline in the material that obtains, then put into medical centrifuge, 4000rpm is centrifugal with rotating speed, flash distillation thing after centrifugal is put into matrass with decompression facility, at first be warmed up to 120 ℃ of air distillations, then carry out underpressure distillation to system, obtain at last 135 gram additives of tan thickness.Base number=the 385mgKOH/g of product, turbidity=152, product viscosity=133.72mm
2/ s.Infrared analysis calcium carbonate absorption peak position; 863.2cm
-1
Embodiment 2
In with 500 milliliters of there-necked flasks of motor agitators and prolong, add 150 milliliters of dimethylbenzene (chemical pure), 150SN neutral oil 38 grams (production of Sinopec Yanshan Petrochemical company), dodecyl Whitfield's ointment 4 grams, methyl alcohol 8.2 grams, propyl carbinol 20 grams, calcium hydroxide 18 grams, C
20-28Alkyl benzene sulphonate (ABS) 25 grams, add 3 gram ammoniacal liquor, the control temperature of reaction is at 45～50 ℃ after adding, neutralization reaction 30min, pass into carbonic acid gas, Ventilation Rate is between 0.065L/min, intake reach theoretical value 90% the time, add remaining 32.5 the gram calcium hydroxides, continue to pass into carbonic acid gas and carry out carbonation reaction, when carbonic acid gas reach theoretical value 90% the time, stop ventilation, add yellow soda ash and 20wt% sodium chloride solution 8 grams of 30wt%, at 45～50 ℃ of reaction 45min, then be warmed up to 120 ℃ of dealcoholysis, water.Add 100 milliliters of gasoline in the material that obtains, then put into medical centrifuge, 4000rpm is centrifugal with rotating speed, flash distillation thing after centrifugal is put into matrass with decompression facility, at first be warmed up to 120 ℃ of air distillations, then carry out underpressure distillation to system, obtain at last 127 gram additives of tan thickness.Base number=the 392mgKOH/g of product, turbidity=68JTU, product viscosity=109.62mm
2/ s.Infrared analysis calcium carbonate absorption peak position; 863.3cm
-1
Comparative Examples 1,2 repeats respectively embodiment 1,2 operation, and difference is to finish not add inorganic salt solution after the carbonic acid gas ventilation; Comparative Examples 3 repeats Comparative Examples 1, and difference is that secondary accelerator adopts quadrol.
Comparative Examples 1
In with 500 milliliters of there-necked flasks of motor agitators and prolong, add 150 milliliters in gasoline (industrial goods), add methyl alcohol 23.7 grams, distilled water 6 grams, 150SN neutral oil 43 grams (production of Sinopec Yanshan Petrochemical company), 4-dodecylphenol 4 grams, calcium oxide 16.5 grams, dodecylbenzene high boiling material sulfonic acid 21.6 grams, the control temperature of reaction is at 45～50 ℃ after adding, behind the neutralization reaction 30mi n, pass into carbonic acid gas, Ventilation Rate is between 0.062L/min, intake reach theoretical value 85% the time, add remaining 25 the gram calcium oxide, continue to pass into carbonic acid gas and carry out carbonation reaction, when carbonic acid gas reach theoretical value 85% the time, stop ventilation, then be warmed up at once 120 ℃ of dealcoholysis, water.Add 100 milliliters of gasoline in the material that obtains, then put into medical centrifuge, 4000rpm is centrifugal with rotating speed, flash distillation thing after centrifugal is put into matrass with decompression facility, at first be warmed up to 120 ℃ of air distillations, then carry out underpressure distillation to system, obtain at last 135 gram additives of tan thickness.Base number=the 383mgKOH/g of product, turbidity=96, product viscosity=151.18mm
2/ s.Infrared analysis calcium carbonate absorption peak position; 863.6cm
-1
Comparative Examples 2
In with 500 milliliters of there-necked flasks of motor agitators and prolong, add 150 milliliters of dimethylbenzene (chemical pure), 150SN neutral oil 38 grams (production of Sinopec Yanshan Petrochemical company), dodecyl Whitfield's ointment 4 grams, methyl alcohol 8.2 grams, propyl carbinol 20 grams, calcium hydroxide 18 grams, C
20-28Alkyl benzene sulphonate (ABS) 25 grams, add 3 gram ammoniacal liquor, control temperature of reaction at 45～50 ℃ after adding, neutralization reaction 30min, pass into carbonic acid gas, Ventilation Rate between 0.065L/min, intake reach theoretical value 90% the time, add remaining 32.5 the gram calcium hydroxides, continue to pass into carbonic acid gas and carry out carbonation reaction, when carbonic acid gas reach theoretical value 90% the time, stop the ventilation, then be warmed up at once 120 ℃ of dealcoholysis, water.Add 100 milliliters of gasoline in the material that obtains, then put into medical centrifuge, 4000rpm is centrifugal with rotating speed, flash distillation thing after centrifugal is put into matrass with decompression facility, at first be warmed up to 120 ℃ of air distillations, then underpressure distillation obtains at last 129 of tan thickness and restrains additives.Base number=the 395mgKOH/g of product, turbidity=63JTU, product viscosity=125.23mm
2/ s.Infrared analysis calcium carbonate absorption peak position; 863.5cm
-1
Comparative Examples 3
In with 500 milliliters of there-necked flasks of motor agitators and prolong, add 150 milliliters in gasoline (industrial goods), add methyl alcohol 23.7 grams, distilled water 6 grams, 150SN neutral oil 43 grams (production of Sinopec Yanshan Petrochemical company), quadrol 3 grams, calcium oxide 16.5 grams, dodecylbenzene high boiling material sulfonic acid 21.6 grams, the control temperature of reaction is at 45～50 ℃ after adding, behind the neutralization reaction 30min, pass into carbonic acid gas, Ventilation Rate is between 0.062L/min, intake reach theoretical value 85% the time, add remaining 25 the gram calcium oxide, continue to pass into carbonic acid gas and carry out carbonation reaction, when carbonic acid gas reach theoretical value 85% the time, stop ventilation, then be warmed up at once 120 ℃ of dealcoholysis, water.Add 100 milliliters of gasoline in the material that obtains, then put into medical centrifuge, 4000rpm is centrifugal with rotating speed, flash distillation thing after centrifugal is put into matrass with decompression facility, at first be warmed up to 120 ℃ of air distillations, then carry out underpressure distillation to system, obtain at last 135 gram additives of tan thickness.Base number=the 379mgKOH/g of product, turbidity=87, product viscosity=128.9mm
2/ s.Infrared analysis calcium carbonate absorption peak position; 863.6cm
-1
Embodiment 3
Present embodiment is used for illustrating effect of the present invention.
Adopt embodiment 1,2 and Comparative Examples 1,2 synthetic calcium sulfonate with high base number, according to the lubricating grease preparation procedure, add respectively thinning oil, low mass molecule alcohol and water, the calcium viscosifying agent, mixture is heated to 80 ℃ of conversions of carrying out the calcium sulphonate crystal formation, when the infrared absorption peak of newton's body calcium sulphonate calcium carbonate by 863.1cm
-1Transfer to gradually 881.5cm
-1The time, can think to transform and finish.Above synthetic lubricating grease is carried out the properties test, the results are shown in Table 1.
Table 1
Claims (19)
1. the preparation method of a calcium sulfonate with high base number comprises:
(1) varsol, neutral oil, C1～C4 alcohol, calcium oxide and/or calcium hydroxide, water are mixed with sulfonic acid, carry out neutralization reaction;
(2) pass into carbonic acid gas, carry out the carbonation reaction first time;
(3) add calcium oxide and/or calcium hydroxide, pass into carbonic acid gas, carry out the carbonation reaction second time;
(4) adding concentration is the inorganic salt solution of 10～60wt%, take sulfonic acid weight as 100 parts, consumption is 5～100 parts, react 30～120min between 40～60 ℃, wherein inorganic salt are selected from one or more in alkali metal chloride, alkaline carbonate, alkali metal sulfates, alkaline earth metal chloride, alkaline earth metal sulphate, ammonium chloride, volatile salt, the ammonium sulfate;
(5) remove alcohol, water, solvent and solid residue after, obtain product.
2. in accordance with the method for claim 1, it is characterized in that varsol is one or more in 60～180 ℃ straight-run spirit, octane, benzene, toluene and dimethylbenzene of boiling range.
3. in accordance with the method for claim 1, it is characterized in that neutral oil is oil and in the hydrofined oil one or more of the old three cover art breading of 100SN, 150SN, lubricating oil.
4. in accordance with the method for claim 1, it is characterized in that described C1～C4 alcohol is one or more in methyl alcohol, ethanol, propyl alcohol, butanols and the ethylene glycol.
5. in accordance with the method for claim 1, it is characterized in that described sulfonic acid is alkyl benzene sulphonate (ABS) and/or mahogany acid, the alkyl carbon number in the alkyl benzene sulphonate (ABS) is 8～30.
6. in accordance with the method for claim 1, it is characterized in that in the step (1), the consumption of C1～C4 alcohol is 20～200 parts; The consumption of varsol is 200～800 parts; The consumption of neutral oil is 50～300 parts; The consumption of calcium oxide and/or calcium hydroxide is 15～150 parts; The consumption of water is 10～50 parts.
7. in accordance with the method for claim 6, it is characterized in that in the step (1), the consumption of C1～C4 alcohol is 50～150 parts; The consumption of varsol is 300～600 parts; The consumption of neutral oil is 120～250 parts; The consumption of calcium oxide and/or calcium hydroxide is 50～100 parts; The consumption of water is 20～40 parts.
8. in accordance with the method for claim 1, it is characterized in that in the step (1), temperature of reaction is 40～60 ℃, the reaction times is 20～60mi n.
9. in accordance with the method for claim 1, it is characterized in that in step (2) and (3), the intake of carbonic acid gas is 60～140% of theoretical value.
10. in accordance with the method for claim 1, it is characterized in that in step (2) and (3), the temperature of carbonation reaction is 40～60 ℃.
11. in accordance with the method for claim 1, it is characterized in that in the step (3), the consumption of calcium oxide and/or calcium hydroxide is 50～300 parts.
12. in accordance with the method for claim 11, it is characterized in that in the step (3), the consumption of calcium oxide and/or calcium hydroxide is 100～150 parts.
13. in accordance with the method for claim 1, it is characterized in that in the step (4), inorganic salt are one or more in calcium chloride, sodium-chlor, yellow soda ash, salt of wormwood, sodium sulfate and the ammonium sulfate.
14. in accordance with the method for claim 1, it is characterized in that in the step (4), the consumption of inorganic salt solution is 10～50 parts.
15. in accordance with the method for claim 1, it is characterized in that also add 2～50 parts secondary accelerator in the step (1), secondary accelerator is one or more in alcohol, phenol, carboxylic acid, carboxylicesters, carboxylic acid anhydride, the acid amides, its carbon number is 9～200.
16. in accordance with the method for claim 15, it is characterized in that in the step (1), the add-on of secondary accelerator is 10～30 parts.
17. in accordance with the method for claim 1, it is characterized in that in the step (1), replace water with alkaline aqueous solution, alkaline aqueous solution is selected from one or more in ammonia soln, alkali metal hydroxide aqueous solution and the alkaline earth metal hydroxides aqueous solution.
18. in accordance with the method for claim 17, it is characterized in that the concentration of alkaline aqueous solution is 5wt%～35wt%.
19., it is characterized in that this product is in preparation during lubricating grease according to the resulting product of either method in the claim 1～18, to be converted into the time of calcite type calcium carbonate be 20～100min to amorphous calcium carbonate in the time of 80 ℃.
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| CN102070493B (en) * | 2011-01-04 | 2013-07-31 | 锦州惠发天合化学有限公司 | Method for preparing fluorine-containing lubricating oil additive |
| FR3013056B1 (en) * | 2013-11-13 | 2018-01-19 | Total Marketing Services | PROCESS FOR THE PREPARATION OF A COMPLEX CALCIUM SULFONATE GREASE |
| CN113528215B (en) * | 2021-07-09 | 2023-03-10 | 新乡市瑞丰新材料股份有限公司 | Preparation method of high-DBN calcium sulfonate for lubricating grease |
| CN113831267A (en) * | 2021-09-08 | 2021-12-24 | 江苏澳润新材料有限公司 | Production process capable of improving purity of sulfonate |
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| GB1139172A (en) * | 1966-01-28 | 1969-01-08 | Monsanto Chemicals | Process for the production of oil solutions of sulphonate/carbonate complexes |
| US6015778A (en) * | 1998-03-27 | 2000-01-18 | The Lubrizol Corporation | Process for making overbased calcium sulfonate detergents using calcium oxide and a less than stoichiometric amount of water |
| CN1523087A (en) * | 2003-02-20 | 2004-08-25 | 中国石油天然气股份有限公司 | Low-turbidity high-base number calcium petroleum sulfonate additive and preparation method thereof |
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2009
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1139172A (en) * | 1966-01-28 | 1969-01-08 | Monsanto Chemicals | Process for the production of oil solutions of sulphonate/carbonate complexes |
| US6015778A (en) * | 1998-03-27 | 2000-01-18 | The Lubrizol Corporation | Process for making overbased calcium sulfonate detergents using calcium oxide and a less than stoichiometric amount of water |
| CN1523087A (en) * | 2003-02-20 | 2004-08-25 | 中国石油天然气股份有限公司 | Low-turbidity high-base number calcium petroleum sulfonate additive and preparation method thereof |
Non-Patent Citations (2)
| Title |
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| 曲江.高碱值烷基苯磺酸钙合成工艺研究.《石油炼制与化工》.2009,第40卷(第10期),第46－50页. |
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