CN102875798A - Synthetic method of water insoluble polyether synthetic base oil - Google Patents
Synthetic method of water insoluble polyether synthetic base oil Download PDFInfo
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- CN102875798A CN102875798A CN2012103984728A CN201210398472A CN102875798A CN 102875798 A CN102875798 A CN 102875798A CN 2012103984728 A CN2012103984728 A CN 2012103984728A CN 201210398472 A CN201210398472 A CN 201210398472A CN 102875798 A CN102875798 A CN 102875798A
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Abstract
The invention provides a synthetic method of water insoluble polyether synthetic base oil and relates to a synthetic method of a chemical industry product. The synthetic method comprises the following steps of: firstly preprocessing n-butyl alcohol, throwing 10-20g of 3A molecular sieve into per kg of n-butyl alcohol, stirring to be uniform, placing for 24 hours, filtering out the molecular sieve, then throwing into the same fresh molecular sieve, and repeating the steps for three times for later use; then sequentially throwing the n-butyl alcohol and a multi-metal catalyst in a reaction kettle, carrying out an initiation reaction, slowly dropwise adding epoxypropane into the reaction kettle, after dropwise adding is finished, discharging when the temperature of the reaction kettle is reduced to 60 DEG C, thus obtaining an intermediate; and finally throwing the intermediate into the reaction kettle, slowly dropwise adding mixture of the epoxypropane and ethylene oxide into the reaction kettle, after dropwise adding is finished, discharging when the temperature of the reaction kettle is reduced to 60 DEG C, and filtering, thus obtaining a finished product. The polyether synthetic base oil prepared by the synthetic method disclosed by the invention has the advantages of high viscosity property, high viscosity index, small variation along with temperature, low flow point and freezing point, stronger lipophilicity, good intermiscibility with various penetrants, better oxidation stability and emulsion performance and certain water-retaining property.
Description
Technical field
The present invention relates to a kind of synthetic method, more particularly, relate to a kind of synthetic method of water-insoluble polyethers synthetic base oil.
Background technology
Existing water-insoluble polyethers synthetic oil adopts traditional alkali to do the synthetic low-molecular-weight dibasic alcohol of catalyzer, the trivalent alcohol polyethers is initiator, as intermediate again with the insoluble polyethers synthetic base oil of propylene oxide synthetic water.The viscosity characteristics of polyethers synthetic oil is not high in the prior art, and on the low side at corresponding viscosity products medium viscosity index, lipophilicity is strong not, and good not with the intermiscibility of mineral oil and various permeate agents, emulsifying property is not strong, does not have water-retentivity.
The present invention's use is the propyl carbinol in the monohydroxy-alcohol, divides for two steps be polymerized take a certain proportion of propylene oxide, oxyethane mixture as main raw material.The development of this synthetic oil, can make oil product have splendid thermo-oxidative stability, have good viscosity-temperature characteristics and supporting capacity, stable, nontoxic, the high flash point, very little to the effect of metal and rubber of cold property and oxidative stability, the anti-rotten resistant to hydrolysis of anti-combustion preferably, greatly reduced the generation of the objectionable impuritiess such as greasy filth, carbon distribution.Following dibasic alcohol, trivalent alcohol polyethers is that the synthetic water-insoluble polyethers of initiator is compared, even under the operating mode of harshness, synthetic oil also can guarantee preferably stability, greatly reduces friction, reduces and wear and tear; Under low temperature condition, also can reach better flowability.In addition, so that the drain period is compared and prolongs manyly, this also can reduce the waste oil discharging to the superior resistance of oxidation of synthetic oil with high-temperature stability.And synthetic oil is objectionable impuritiess such as sulfur-bearing, nitrogen, phosphorus not fully, and oil product is very little to the infringement of human body, and these all embody its environment protection significance.At present successfully as high temperature grease, gear oil, compressor oil, hydraulic liquid, braking fluid, water-based total synthesis metal processing liquid and special greases base oil.
Summary of the invention
In order to solve above-mentioned problems of the prior art, the object of the invention provides a kind of synthetic method of water-insoluble polyethers synthetic base oil, use the propyl carbinol in the monohydroxy-alcohol, take a certain proportion of propylene oxide, oxyethane mixture as main raw material, under the effect of multimetallic catalyst, be polymerized in two steps.This synthetic oil, can make oil product have fabulous thermo-oxidative stability, have good viscosity-temperature characteristics and supporting capacity, preferably cold property and oxidative stability, anti-combustion, anti-corruption, resistant to hydrolysis are stablized, nontoxic, high flash point, very little to the effect of metal and rubber have greatly reduced the generation of the objectionable impuritiess such as greasy filth, carbon distribution.
In order to realize the foregoing invention purpose, the technical scheme that the present invention takes is: a kind of synthetic method of water-insoluble polyethers synthetic base oil, its characteristics are that described synthetic method step is as follows:
(1), propyl carbinol is carried out pre-treatment
In the molten device of reaction, per 1 kilogram of propyl carbinol drops into 10-20g 3A molecular sieve, and the rear placement that stirs leached molecular sieve in 24 hours, dropped into same fresh molecular sieve again, and is repeatedly for subsequent use after three times like this.
(2), the preparation of intermediate
(a), in reactor, drop into a certain amount of propyl carbinol and micro-multimetallic catalyst, vacuumize pressure reached
To-0.092MPa.
(b) be no more than 40 ℃ in temperature, pass into nitrogen to reactor and make pressure rise to 0.1Mpa, vacuumize again and make Pressure Drop to-0.092MPa, three times repeatedly, make reactor be warming up to 120-130 ℃ and carry out initiation reaction.
(c), after the reaction, slowly drip a small amount of propylene oxide to reactor, the control temperature of reaction is no more than 0.2 Mpa, reaction times at 1-2 hour at 140～160 ℃, pressure.
(d), drip to finish after, be incubated 30 minutes, the question response still cools to 60 ℃ of dischargings, can make intermediate.
(3), the preparation of finished product
(a), drop into a certain amount of above-mentioned synthetic intermediate to reactor, vacuumize pressure is reached-0.092MPa;
(b), pass into nitrogen to reactor, make pressure rise to 0.1MPa, vacuumize again and make Pressure Drop to-0.092MPa.
(c), reactor is warming up to 120 ℃, slowly drips a certain proportion of propylene oxide and oxyethane mixture to reactor, the control temperature of reaction is at 110～130 ℃, pressure is no more than 0.15 Mpa, the reaction times is controlled at 3-4 hour.
(d), drip to finish after, be incubated 30 minutes, the question response still is cooled to 60 ℃ of dischargings, can make finished product after filtration.
Described multimetallic catalyst input amount is 60～80ppm of total inventory.
Described in the preparation process of intermediate, the weight ratio of propyl carbinol and propylene oxide is 1:3-4.
Described in whole reaction process, the weight ratio of propyl carbinol and propylene oxide, oxyethane is 1:10-70:1-7.
Described propylene oxide and oxyethane fully mix in above-mentioned definite ratio.
Described multimetallic catalyst is selected from the multi-metal cyanide complex catalyst.
Beneficial effect of the present invention is: the present invention compared with the prior art, (1), adopt multimetallic catalyst to carry out polyreaction, and through optimization design and repetition test research, pretreatment process, proportioning raw materials, catalyst levels have rationally been determined, the processing parameter such as polymeric reaction temperature, time and condition, reaction conditions is gentle, easily control, with short production cycle, the scope of the regulatable 40 ℃ of kinetic viscosities of polyethers synthetic base oil that make is at 40-700mm
2/ s.(2), employed catalyzer has good catalytic activity, the second step reaction can add catalyzer again, can obtain different viscosity the atactic polyether synthetic base oil.(3), the high molecular polyether synthetic base oil that makes of polyreaction treatment process after filtration again, the product moisture content that obtains is low, acid number is low, has no irritating odor, metal ion content is low.(4), make the polyethers synthetic base oil by the method for the invention and have high viscosity characteristics, viscosity index is high, vary with temperature little, yield point and zero pour are low, lipophilicity is stronger, good with the intermiscibility of mineral oil and various permeate agents, preferably oxidative stability and emulsifying property are arranged, certain water-retentivity is arranged.
Embodiment
Embodiment 1
The first step is carried out pre-treatment to propyl carbinol.In the molten device of reaction, per 1 kilogram of propyl carbinol drops into 10-20g 3A molecular sieve, and the rear placement that stirs leached molecular sieve in 24 hours, dropped into same fresh molecular sieve again, and is repeatedly for subsequent use after three times like this.
Second step, the preparation of intermediate.In reactor, drop into the propyl carbinol 2Kg handle well, drop into multimetallic catalyst 1.75g, vacuumize pressure is reached-0.092MPa; Be no more than 40 ℃ in temperature, pass into nitrogen to reactor and make pressure rise to 0.1Mpa, vacuumize again and make Pressure Drop to-0.092MPa, three times repeatedly, make reactor be warming up to 120-130 ℃ and carry out initiation reaction; After the reaction, slowly drip the 7Kg propylene oxide to reactor, the control temperature of reaction is no more than 0.2 Mpa, reaction times at 140～160 ℃, pressure and is controlled at 1.5 hours; After dripping end, be incubated 30 minutes, the question response still cools to 60 ℃ of dischargings, can make intermediate.
The 3rd step, the preparation of finished product.Drop into the above-mentioned synthetic intermediate of 0.6Kg to reactor, vacuumize pressure is reached-0.092MPa; Pass into nitrogen to reactor, make pressure rise to 0.1MPa, vacuumize again and make Pressure Drop to-0.092MPa; Reactor is warming up to 120 ℃, slowly drips propylene oxide 13K g, oxyethane 2Kg mixture to reactor, and the control temperature of reaction is at 110～130 ℃, and pressure is no more than 0.15 Mpa, and the reaction times is controlled at 3.5 hours; After dripping end, be incubated 30 minutes, the question response still is cooled to 60 ℃ of dischargings, can make finished product after filtration.
Embodiment 2
The first step is carried out pre-treatment to propyl carbinol.In the molten device of reaction, per 1 kilogram of propyl carbinol drops into 10-20g 3A molecular sieve, and the rear placement that stirs leached molecular sieve in 24 hours, dropped into same fresh molecular sieve again, and is repeatedly for subsequent use after three times like this.
Second step, the preparation of intermediate.In reactor, drop into the propyl carbinol 2.5Kg handle well, drop into multimetallic catalyst 2.2g, vacuumize pressure is reached-0.092MPa; Be no more than 40 ℃ in temperature, pass into nitrogen to reactor and make pressure rise to 0.1Mpa, vacuumize again and make Pressure Drop to-0.092MPa, three times repeatedly, make reactor be warming up to 120-130 ℃ and carry out initiation reaction; After the reaction, slowly drip the 7.5Kg propylene oxide to reactor, the control temperature of reaction is no more than 0.2 Mpa, reaction times at 140～160 ℃, pressure and is controlled at 1.5 hours; After dripping end, be incubated 30 minutes, the question response still cools to 60 ℃ of dischargings, can make intermediate.
The 3rd step, the preparation of finished product.Drop into the above-mentioned synthetic intermediate of 0.45Kg to reactor, vacuumize pressure is reached-0.092MPa; Pass into nitrogen to reactor, make pressure rise to 0.1MPa, vacuumize again and make Pressure Drop to-0.092MPa; Reactor is warming up to 120 ℃, slowly drips propylene oxide 17.5K g, oxyethane 5Kg mixture to reactor, and the control temperature of reaction is at 110～130 ℃, and pressure is no more than 0.15 Mpa, and the reaction times is controlled at 3.5 hours; After dripping end, be incubated 30 minutes, the question response still is cooled to 60 ℃ of dischargings, can make finished product after filtration.
Embodiment 3
The first step is carried out pre-treatment to propyl carbinol.In the molten device of reaction, per 1 kilogram of propyl carbinol drops into 10-20g 3A molecular sieve, and the rear placement that stirs leached molecular sieve in 24 hours, dropped into same fresh molecular sieve again, and is repeatedly for subsequent use after three times like this.
Second step, the preparation of intermediate.In reactor, drop into the propyl carbinol 3Kg handle well, drop into multimetallic catalyst 3.0g, vacuumize pressure is reached-0.092MPa; Be no more than 40 ℃ in temperature, pass into nitrogen to reactor and make pressure rise to 0.1Mpa, vacuumize again and make Pressure Drop to-0.092MPa, three times repeatedly, make reactor be warming up to 120-130 ℃ and carry out initiation reaction; After the reaction, slowly drip the 9Kg propylene oxide to reactor, the control temperature of reaction is no more than 0.2 Mpa, reaction times at 140～160 ℃, pressure and is controlled at 1.5 hours; After dripping end, be incubated 30 minutes, the question response still cools to 60 ℃ of dischargings, can make intermediate.
The 3rd step, the preparation of finished product.Drop into the above-mentioned synthetic intermediate of 0.3Kg to reactor, vacuumize pressure is reached-0.092MPa; Pass into nitrogen to reactor, make pressure rise to 0.1MPa, vacuumize again and make Pressure Drop to-0.092MPa; Reactor is warming up to 120 ℃, slowly drips propylene oxide 24K g, oxyethane 7.5Kg mixture to reactor, and the control temperature of reaction is at 110～130 ℃, and pressure is no more than 0.15 Mpa, and the reaction times is controlled at 3.5 hours; After dripping end, be incubated 30 minutes, the question response still is cooled to 60 ℃ of dischargings, can make finished product after filtration.
Embodiment 4
The first step is carried out pre-treatment to propyl carbinol.In the molten device of reaction, per 1 kilogram of propyl carbinol drops into 10-20g 3A molecular sieve, and the rear placement that stirs leached molecular sieve in 24 hours, dropped into same fresh molecular sieve again, and is repeatedly for subsequent use after three times like this.
Second step, the preparation of intermediate.In reactor, drop into the propyl carbinol 3.5Kg handle well, drop into multimetallic catalyst 4.0g, vacuumize pressure is reached-0.092MPa; Be no more than 40 ℃ in temperature, pass into nitrogen to reactor and make pressure rise to 0.1Mpa, vacuumize again and make Pressure Drop to-0.092MPa, three times repeatedly, make reactor be warming up to 120-130 ℃ and carry out initiation reaction; After the reaction, slowly drip the 10.5Kg propylene oxide to reactor, the control temperature of reaction is no more than 0.2 Mpa, reaction times at 140～160 ℃, pressure and is controlled at 1.5 hours; After dripping end, be incubated 30 minutes, the question response still cools to 60 ℃ of dischargings, can make intermediate.
The 3rd step, the preparation of finished product.Drop into the above-mentioned synthetic intermediate of 0.1Kg to reactor, vacuumize pressure is reached-0.092MPa; Pass into nitrogen to reactor, make pressure rise to 0.1MPa, vacuumize again and make Pressure Drop to-0.092MPa; Reactor is warming up to 120 ℃, slowly drips propylene oxide 31.5Kg, oxyethane 10.5Kg mixture to reactor, and the control temperature of reaction is at 110～130 ℃, and pressure is no more than 0.15 Mpa, and the reaction times is controlled at 3.5 hours; After dripping end, be incubated 30 minutes, the question response still is cooled to 60 ℃ of dischargings, can make finished product after filtration.
In above-mentioned each example obtained polyethers synthetic base oil after tested, index is as follows:
Claims (5)
1. a kind of synthetic method of water-insoluble polyethers synthetic base oil is characterized in that described synthetic method step is as follows:
(1), propyl carbinol is carried out pre-treatment:
In the molten device of reaction, per 1 kilogram of propyl carbinol drops into 10-20g 3A molecular sieve, and the rear placement that stirs leached molecular sieve in 24 hours, dropped into same fresh molecular sieve again, and is repeatedly for subsequent use after three times like this;
(2), the preparation of intermediate
(a), in reactor, drop into a certain amount of propyl carbinol and micro-multimetallic catalyst, vacuumize pressure reached
To-0.092MPa;
(b) be no more than 40 ℃ in temperature, pass into nitrogen to reactor and make pressure rise to 0.1Mpa, vacuumize again and make Pressure Drop to-0.092MPa, three times repeatedly, make reactor be warming up to 120-130 ℃ and carry out initiation reaction;
(c), after the reaction, slowly drip a small amount of propylene oxide to reactor, the control temperature of reaction is no more than 0.2 Mpa, reaction times at 1-2 hour at 140～160 ℃, pressure;
(d), drip to finish after, be incubated 30 minutes, the question response still cools to 60 ℃ of dischargings, can make intermediate;
(3), the preparation of finished product
(a), drop into a certain amount ofly by above-mentioned synthetic intermediate to reactor, vacuumize pressure reached-0.092MPa;
(b), pass into nitrogen to reactor, make pressure rise to 0.1MPa, vacuumize again and make Pressure Drop to-0.092MPa;
(c), reactor is warming up to 120 ℃, slowly drips a certain proportion of propylene oxide and oxyethane mixture to reactor, the control temperature of reaction is at 110～130 ℃, pressure is no more than 0.15 Mpa, the reaction times is controlled at 3-4 hour;
(d), drip to finish after, be incubated 30 minutes, the question response still is cooled to 60 ℃ of dischargings, can make finished product after filtration.
2. a kind of synthetic method of described water-insoluble polyethers synthetic base oil according to claim 1, it is characterized in that: described multimetallic catalyst input amount is 60～80ppm of total inventory.
3. a kind of synthetic method of described water-insoluble polyethers synthetic base oil according to claim 1, it is characterized in that: described in the preparation process of intermediate, the weight ratio of propyl carbinol and propylene oxide is 1:3-4.
4. a kind of synthetic method of described water-insoluble polyethers synthetic base oil according to claim 1, it is characterized in that: described in whole reaction process, the weight ratio of propyl carbinol and propylene oxide, oxyethane is 1:10-70:1-7.
5. a kind of synthetic method of described water-insoluble polyethers synthetic base oil according to claim 1, it is characterized in that: described multimetallic catalyst is selected from the multi-metal cyanide complex catalyst.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105189856A (en) * | 2013-07-19 | 2015-12-23 | 松本油脂制药株式会社 | Synthetic fiber treatment agent and use of same |
| CN111171926A (en) * | 2019-12-31 | 2020-05-19 | 南京尚勤新材料科技有限公司 | Synthesis method of graphene oxide modified fatty acid amide for metal cutting fluid |
| CN113956910A (en) * | 2020-07-21 | 2022-01-21 | 中国石油天然气股份有限公司 | Synthetic lubricating oil composition |
| CN114164035A (en) * | 2021-12-15 | 2022-03-11 | 上海东大化学有限公司 | Turbine worm lubricating oil and preparation method thereof |
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| CN101045784A (en) * | 2006-03-27 | 2007-10-03 | 中国石油化工股份有限公司 | Preparation method of atactic polyether |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105189856A (en) * | 2013-07-19 | 2015-12-23 | 松本油脂制药株式会社 | Synthetic fiber treatment agent and use of same |
| CN111171926A (en) * | 2019-12-31 | 2020-05-19 | 南京尚勤新材料科技有限公司 | Synthesis method of graphene oxide modified fatty acid amide for metal cutting fluid |
| CN111171926B (en) * | 2019-12-31 | 2022-07-12 | 南京尚勤新材料科技有限公司 | Synthesis method of graphene oxide modified fatty acid amide for metal cutting fluid |
| CN113956910A (en) * | 2020-07-21 | 2022-01-21 | 中国石油天然气股份有限公司 | Synthetic lubricating oil composition |
| CN114164035A (en) * | 2021-12-15 | 2022-03-11 | 上海东大化学有限公司 | Turbine worm lubricating oil and preparation method thereof |
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