CN113087891B - Oil-soluble polyether and preparation method and application thereof - Google Patents
Oil-soluble polyether and preparation method and application thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
- C08G65/04—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers only
- C08G65/06—Cyclic ethers having no atoms other than carbon and hydrogen outside the ring
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- 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
- C10M107/00—Lubricating compositions characterised by the base-material being a macromolecular compound
- C10M107/20—Lubricating compositions characterised by the base-material being a macromolecular compound containing oxygen
- C10M107/30—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- C10M107/32—Condensation polymers of aldehydes or ketones; Polyesters; Polyethers
- C10M107/34—Polyoxyalkylenes
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- 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
- C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
- C10M2209/10—Macromolecular compoundss obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- C10M2209/103—Polyethers, i.e. containing di- or higher polyoxyalkylene groups
- C10M2209/106—Polyethers, i.e. containing di- or higher polyoxyalkylene groups of alkylene oxides containing four carbon atoms only
- C10M2209/1065—Polyethers, i.e. containing di- or higher polyoxyalkylene groups of alkylene oxides containing four carbon atoms only used as base material
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/584—Recycling of catalysts
Abstract
The invention provides oil-soluble polyether and a preparation method and application thereof, wherein the preparation method comprises the following steps: (1) mixing an epoxy monomer and a catalyst in a non-oxidizing atmosphere to carry out polymerization reaction; (2) adding a terminator to terminate the polymerization reaction, and sequentially carrying out water washing, extraction and reduced pressure distillation to obtain the oil-soluble polyether. The oil-soluble polyether can be used as base oil. The polymerization condition for preparing the oil-soluble polyether is simple, mild and efficient, and the post-treatment method is simple, so that the method has great potential to replace the traditional industrial preparation process of the oil-soluble polyether base catalytic system.
Description
Technical Field
The invention belongs to the technical field of synthesis, relates to polyether base oil, and particularly relates to oil-soluble polyether and a preparation method and application thereof.
Background
The polyether is a high molecular polymer with ether bonds in a main chain generated by homopolymerization of epoxy monomers or copolymerization of different epoxy monomers. The traditional polyether is prepared by copolymerizing ethylene oxide and propylene oxide, and a polyoxyethylene chain segment of the traditional polyether has hydrophilicity, so that the defects of hygroscopicity, poor compatibility with an elastomer, immiscibility of a mineral oil product and the like are caused, and the defects limit the application of the traditional polyether in a specific occasion.
In order to improve the disadvantage of poor hydrophobicity of conventional polyethers, researchers have found that polyethers obtained by homo-or co-polymerization using alkylene oxide monomers having a high carbon number have excellent hydrophobic properties, for example, 1, 2-butylene oxide as a molecular main chain to form novel polyethers.
CN 106661479A discloses a series of oil-soluble polyether products based on copolymerization of 1, 2-butylene oxide, the kinematic viscosity at 40 ℃ of which covers from 18mm2S to 680mm2And s. The preparation method disclosed by the invention is characterized in that potassium hydroxide is used as a catalyst, alcohol is used as an initiator, and a series of oil-soluble polyethers are prepared by copolymerizing propylene oxide and 1, 2-butylene oxide monomers.
In 2014, Chengliang et al used potassium hydroxide as a catalyst and n-butanol as an initiator to copolymerize propylene oxide and butylene oxide to prepare oil-soluble polyether meeting the requirements of viscosity grades OSP-18, OSP-46 and OSP-150. (see "preparation of oil-soluble polyether and examination of antioxidant Property", Chengliang et al, oil refining and chemical engineering, vol 45, No. 6, pp 86-89)
2013 cheng liang et al propose a method for preparing oil-soluble polyether by base catalysis, which comprises the following steps: drying a three-mouth round-bottom flask provided with a stirrer and a reflux condenser in an anhydrous manner, adding an initiator and alkali under the protection of nitrogen, and stirring at room temperature until the alkali is completely dissolved; under nitrogen, adding butylene oxide into a reaction bottle, heating the device to 70 ℃, refluxing the solution, after reacting for a period of time, stopping heating and stirring, naturally cooling to room temperature, slowly adding a small amount of methanol into the reaction bottle, removing the solvent under reduced pressure, adding concentrated hydrochloric acid, adjusting the pH value to 7, adding distilled water into the reaction liquid, washing, separating, collecting the liquid phase, and drying to obtain the oil-soluble polyether product. (see "preparation of oil-soluble polyether by base catalysis", Chengliang et al, science and technology Notification, vol.29, No. 4, pp.58-60)
The preparation processes described in the three documents mentioned above, although simple, require relatively high reaction temperatures and, subsequently, complicated work-up processes to remove residual alkali from the polyether.
In summary, the main method for preparing polyether in the prior art is anionic polymerization, the residue of the alkali catalyst used in the method must be removed from the polyether product, and the purification process of polyether is complicated, and generally comprises the steps of neutralization, adsorption, decolorization, dehydration, pressure filtration and the like, and the polymerization temperature is 70-130 ℃, and the pressure is 0.2-0.5 MPa. Therefore, it is necessary to develop a method for preparing oil-soluble polyether, which has mild polymerization conditions and simple post-treatment.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide an oil-soluble polyether, and a preparation method and application thereof. Compared with the prior art, the preparation method realizes the preparation of the oil-soluble polyether by mild polymerization conditions and simple post-treatment.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the present invention provides a method for preparing an oil-soluble polyether, comprising the steps of:
(1) mixing an epoxy monomer and a catalyst in a non-oxidizing atmosphere to carry out polymerization reaction;
(2) adding a terminator to terminate the polymerization reaction, and sequentially carrying out water washing, extraction and reduced pressure distillation to obtain the oil-soluble polyether.
The polymerization reaction is carried out in a container, and specifically, the preparation method provided by the invention comprises the following steps:
(a) adding a catalyst into the reaction container, vacuumizing and decompressing the reaction container, and replacing non-oxidizing gas;
(b) injecting epoxy monomer into the reaction container under the protection of non-oxidizing gas, stirring for reaction, adjusting the polymerization temperature, and starting the polymerization reaction;
(c) adding a terminator to terminate the polymerization reaction, and sequentially carrying out water washing, extraction and reduced pressure distillation to obtain the oil-soluble polyether.
The polymerization condition for preparing the oil-soluble polyether is simple, mild and efficient, and the post-treatment method is simple, so that the method has great potential to replace the traditional industrial preparation process of the oil-soluble polyether base catalytic system.
Preferably, the catalyst of step (1) comprises a metal triflate.
Preferably, the catalyst of step (1) comprises a trifluoromethanesulfonic acid rare earth metal salt.
Preferably, the rare earth metal triflate comprises any one of scandium triflate, yttrium triflate, lanthanum triflate, cerium triflate, praseodymium triflate, neodymium triflate, promethium triflate, samarium triflate, europium triflate, gadolinium triflate, terbium triflate, dysprosium triflate, holmium triflate, erbium triflate, thulium triflate, ytterbium triflate, or lutetium triflate, or a combination of at least two; typical but non-limiting combinations include a combination of lanthanum triflate with scandium triflate, yttrium triflate with lanthanum triflate, cerium triflate with praseodymium triflate, neodymium triflate with promethium triflate, samarium triflate, europium triflate with gadolinium triflate, terbium triflate with dysprosium triflate, or thulium triflate, ytterbium triflate with lutetium triflate; further preferred is lanthanum trifluoromethanesulfonate.
Preferably, the gas used in the non-oxidizing atmosphere in step (1) includes any one or a combination of at least two of nitrogen, helium, neon, argon, krypton or xenon, and typical but non-limiting combinations include a combination of nitrogen and helium, a combination of nitrogen and neon, a combination of nitrogen and argon, a combination of nitrogen and krypton, a combination of nitrogen and xenon, or a combination of nitrogen, helium and neon.
Preferably, the epoxy monomers of step (1) comprise any one or a combination of at least two of ethylene oxide, propylene oxide or 1, 2-butylene oxide, typical but non-limiting combinations include combinations of ethylene oxide and propylene oxide, ethylene oxide and 1, 2-butylene oxide, propylene oxide and 1, 2-butylene oxide, or ethylene oxide, propylene oxide and 1, 2-butylene oxide.
Preferably, the polymerization temperature in step (1) is 0-130 ℃, for example, 0 ℃, 10 ℃, 20 ℃, 30 ℃, 40 ℃, 50 ℃, 60 ℃, 70 ℃, 80 ℃, 90 ℃, 100 ℃, 110 ℃, 120 ℃ or 130 ℃, but not limited to the recited values, and other values not recited in the range of values are also applicable; preferably 25-50 deg.c.
Preferably, the polymerization reaction time in step (1) is 2 to 72h, for example, 2h, 4h, 8h, 12h, 16h, 20h, 24h, 28h, 32h, 36h, 40h, 44h, 48h, 52h, 56h, 60h, 64h, 68h or 72h, but not limited to the recited values, and other values not recited in the numerical range are also applicable; preferably 24-48 h.
Preferably, the stirring rate of the polymerization reaction in step (1) is 1500r/min, such as 100r/min, 200r/min, 300r/min, 400r/min, 500r/min, 600r/min, 700r/min, 800r/min, 900r/min, 1000r/min, 1100r/min, 1200r/min, 1300r/min, 1400r/min or 1500r/min, but not limited to the values listed, and other values not listed in the range of values are equally applicable; preferably 450-550 r/min.
Preferably, the molar ratio of catalyst to epoxy monomer in step (1) is (1-10):500, and may be, for example, 1:500, 2:500, 3:500, 4:500, 5:500, 6:500, 7:500, 8:500, 9:500 or 10:500, but is not limited to the recited values, and other values not recited in the numerical ranges are equally applicable; preferably (1-5): 500.
Preferably, the terminating agent in the step (2) comprises any one of water, alcohol compounds, phenolic compounds or amine compounds or a combination of at least two of the water, the alcohol compounds, the phenolic compounds or the amine compounds.
Preferably, the alcohol compound comprises any one or a combination of at least two of ethanol, benzyl alcohol, ethylene glycol or polyhydric alcohol; typical, but non-limiting combinations include a combination of ethanol and benzyl alcohol, a combination of benzyl alcohol and ethylene glycol, a combination of ethylene glycol and a polyol, a combination of benzyl alcohol and ethanol, or a combination of ethanol, benzyl alcohol and ethylene glycol.
Preferably, the phenolic compound comprises any one or a combination of at least two of phenol, p-cresol, hydroquinone or p-tert-butylcatechol, typical but non-limiting combinations include combinations of phenol and p-cresol, p-cresol and hydroquinone, hydroquinone and p-tert-butylcatechol, or combinations of p-cresol, hydroquinone and p-tert-butylcatechol.
Preferably, the amine compound comprises sodium dimethyldithiocarbamate.
As a preferable technical solution of the preparation method of the first aspect of the present invention, the preparation method comprises the steps of:
(1) mixing an epoxy monomer and a catalyst in a non-oxidizing atmosphere, and carrying out a polymerization reaction for 2-72h under the conditions that the temperature is 0-130 ℃ and the stirring speed is 300-700 r/min;
(2) adding a terminator to terminate the polymerization reaction, and sequentially carrying out water washing, extraction and reduced pressure distillation to obtain the oil-soluble polyether.
Further preferably, the preparation method comprises the following steps:
(a) adding a catalyst into the reaction container, vacuumizing and decompressing the reaction container, and replacing non-oxidizing gas;
(b) injecting epoxy monomer into the reaction container under the protection of non-oxidizing gas, and carrying out polymerization reaction for 2-72h under the conditions that the temperature is 0-130 ℃ and the stirring speed is 300-700 r/min;
(c) adding a terminator to terminate the polymerization reaction, and sequentially carrying out water washing, extraction and reduced pressure distillation to obtain the oil-soluble polyether.
In a second aspect, the invention provides an oil-soluble polyether prepared by the preparation method of the first aspect.
In a third aspect, the present invention provides a use of the oil-soluble polyether of the second aspect as a base oil.
The recitation of numerical ranges herein includes not only the above-recited numerical values, but also any numerical values between non-recited numerical ranges, and is not intended to be exhaustive or to limit the invention to the precise numerical values encompassed within the range for brevity and clarity.
Compared with the prior art, the invention has the beneficial effects that:
(1) the preparation method of the oil-soluble polyether provided by the invention realizes the preparation of the oil-soluble polyether under mild polymerization conditions and simple post-treatment;
(2) the invention realizes the controllable polymerization of the molecular weight of the oil-soluble polyether by regulating and controlling the amount of the added catalyst, and the prepared polyether has the molecular weight of 500-2500, and has very wide application field as the polyether base oil.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments.
Sources of raw materials used in embodiments of the present invention include:
lanthanum trifluoromethanesulfonate: CAS number: 52093-26-2, available from Shanghai Aladdin Biotechnology, Inc.
Cerium trifluoromethanesulfonate: CAS number: 76089-77-5, available from Shanghai Allantin Biotechnology GmbH.
Neodymium trifluoromethanesulfonate: CAS number: 34622-08-7, available from Shanghai Aladdin Biotechnology Ltd.
Gadolinium trifluoromethanesulfonate: CAS number: 52093-29-5, available from Shanghai Aladdin Biotechnology, Inc.
1, 2-butylene oxide: CAS number: 106-88-7, propylene oxide; CAS number 75-56-9, ethylene oxide: CAS No. 75-21-8, all purchased from Shanghai Aladdin Biotechnology, Inc., and re-steamed with calcium hydride by reflux.
Example 1
The embodiment provides a preparation method of oil-soluble polyether, which comprises the following steps:
(a) adding catalyst lanthanum trifluoromethanesulfonate (0.24mmol, 140mg) into a dry three-neck round-bottom flask provided with a stirrer and a reflux condenser, vacuumizing and decompressing the reaction vessel, and replacing nitrogen for 3 times;
(b) injecting 1, 2-epoxybutane (60mmol, 4320mg) into a three-neck round-bottom flask by using a syringe under the protection of nitrogen, and carrying out polymerization reaction for 35h under the conditions that the temperature is 25 ℃ and the stirring speed is 500 r/min;
(c) adding 1mL of ethanol as a terminator to terminate the polymerization reaction, adding 5mL of deionized water into the polymerization solution to wash, separating and extracting to collect an oil phase, and distilling under reduced pressure to obtain the oil-soluble polyether.
Example 2
The embodiment provides a preparation method of oil-soluble polyether, which comprises the following steps:
(a) adding catalyst lanthanum trifluoromethanesulfonate (0.24mmol, 140mg) into a dry three-neck round-bottom flask provided with a stirrer and a reflux condenser, vacuumizing and decompressing the reaction vessel, and replacing nitrogen for 3 times;
(b) injecting 1, 2-epoxybutane (60mmol, 4320mg) into a three-neck round-bottom flask by using a syringe under the protection of nitrogen, and carrying out polymerization reaction for 35h under the conditions that the temperature is 50 ℃ and the stirring speed is 500 r/min;
(c) adding 1mL of ethanol as a terminator to terminate the polymerization reaction, adding 5mL of deionized water into the polymerization solution to wash, performing liquid-separation extraction to collect an oil phase, and performing reduced pressure distillation to obtain the oil-soluble polyether.
Example 3
The embodiment provides a preparation method of oil-soluble polyether, which comprises the following steps:
(a) adding catalyst lanthanum trifluoromethanesulfonate (0.6mmol, 352mg) into a dry three-neck round-bottom flask provided with a stirrer and a reflux condenser, vacuumizing and decompressing the reaction vessel, and replacing nitrogen for 3 times;
(b) injecting 1, 2-epoxybutane (60mmol, 4320mg) into a three-neck round-bottom flask by using a syringe under the protection of nitrogen, and carrying out polymerization reaction for 35h under the conditions that the temperature is 25 ℃ and the stirring speed is 500 r/min;
(c) adding 1mL of ethanol as a terminator to terminate the polymerization reaction, adding 5mL of deionized water into the polymerization solution to wash, separating and extracting to collect an oil phase, and distilling under reduced pressure to obtain the oil-soluble polyether.
Example 4
The embodiment provides a preparation method of oil-soluble polyether, which comprises the following steps:
(a) adding catalyst lanthanum trifluoromethanesulfonate (0.6mmol, 352mg) into a dry three-neck round-bottom flask provided with a stirrer and a reflux condenser, vacuumizing and decompressing the reaction vessel, and replacing nitrogen for 3 times;
(b) injecting 1, 2-butylene oxide (60mmol, 4320mg) into a three-neck round-bottom flask by using a syringe under the protection of nitrogen, and carrying out polymerization reaction for 28h under the conditions that the temperature is 50 ℃ and the stirring speed is 500 r/min;
(c) adding 1mL of ethanol as a terminator to terminate the polymerization reaction, adding 5mL of deionized water into the polymerization solution to wash, separating and extracting to collect an oil phase, and distilling under reduced pressure to obtain the oil-soluble polyether.
Example 5
The embodiment provides a preparation method of oil-soluble polyether, which comprises the following steps:
(a) adding catalyst cerium trifluoromethanesulfonate (0.6mmol, 352mg) into a dry three-neck round-bottom flask provided with a stirrer and a reflux condenser, vacuumizing and decompressing the reaction vessel, and replacing nitrogen for 3 times;
(b) injecting 1, 2-epoxybutane (60mmol, 4320mg) into a three-neck round-bottom flask by using a syringe under the protection of nitrogen, and carrying out polymerization reaction for 28h under the conditions that the temperature is 25 ℃ and the stirring speed is 500 r/min;
(c) adding 1mL of ethanol as a terminator to terminate the polymerization reaction, adding 5mL of deionized water into the polymerization solution to wash, separating and extracting to collect an oil phase, and distilling under reduced pressure to obtain the oil-soluble polyether.
Example 6
The embodiment provides a preparation method of oil-soluble polyether, which comprises the following steps:
(a) adding neodymium trifluoromethanesulfonate (0.6mmol, 353mg) serving as a catalyst into a dry three-neck round-bottom flask provided with a stirrer and a reflux condenser, vacuumizing and reducing pressure in a reaction container, and replacing nitrogen for 3 times;
(b) injecting 1, 2-epoxybutane (60mmol, 4320mg) into a three-neck round-bottom flask by using a syringe under the protection of nitrogen, and carrying out polymerization reaction for 52h under the conditions that the temperature is 25 ℃ and the stirring speed is 500 r/min;
(c) adding 1mL of ethanol as a terminator to terminate the polymerization reaction, adding 5mL of deionized water into the polymerization solution to wash, performing liquid-separation extraction to collect an oil phase, and performing reduced pressure distillation to obtain the oil-soluble polyether.
Example 7
The embodiment provides a preparation method of oil-soluble polyether, which comprises the following steps:
(a) adding catalyst gadolinium trifluoromethanesulfonate (0.6mmol, 362mg) into a dry three-neck round-bottom flask provided with a stirrer and a reflux condenser, vacuumizing and decompressing the reaction vessel, and replacing nitrogen for 3 times;
(b) injecting 1, 2-epoxybutane (60mmol, 4320mg) into a three-neck round-bottom flask by using a syringe under the protection of nitrogen, and carrying out polymerization reaction for 52h under the conditions that the temperature is 25 ℃ and the stirring speed is 500 r/min;
(c) adding 1mL of ethanol as a terminator to terminate the polymerization reaction, adding 5mL of deionized water into the polymerization solution to wash, separating and extracting to collect an oil phase, and distilling under reduced pressure to obtain the oil-soluble polyether.
Example 8
The embodiment provides a preparation method of oil-soluble polyether, which comprises the following steps:
(a) adding catalyst lanthanum trifluoromethanesulfonate (0.12mmol, 70mg) into a dry three-neck round-bottom flask provided with a stirrer and a reflux condenser, vacuumizing and decompressing the reaction vessel, and replacing nitrogen for 3 times;
(b) injecting 1, 2-epoxybutane (60mmol, 4320mg) into a three-neck round-bottom flask by using a syringe under the protection of nitrogen, and carrying out polymerization reaction for 52h under the conditions that the temperature is 25 ℃ and the stirring speed is 500 r/min;
(c) adding 1mL of ethanol as a terminator to terminate the polymerization reaction, adding 5mL of deionized water into the polymerization solution to wash, separating and extracting to collect an oil phase, and distilling under reduced pressure to obtain the oil-soluble polyether.
Example 9
The embodiment provides a preparation method of oil-soluble polyether, which comprises the following steps:
(a) adding catalyst lanthanum trifluoromethanesulfonate (0.60mmol, 352mg) into a dry three-neck round-bottom flask provided with a stirrer and a reflux condenser, vacuumizing and decompressing the reaction vessel, and replacing nitrogen for 3 times;
(b) under the protection of nitrogen, injecting 1, 2-butylene oxide (30mmol, 2160mg) and propylene oxide (30mmol, 1740mg) into a three-neck round-bottom flask by a syringe, and carrying out polymerization reaction for 52h under the conditions that the temperature is 25 ℃ and the stirring speed is 500 r/min;
(c) adding 1mL of ethanol as a terminator to terminate the polymerization reaction, adding 5mL of deionized water into the polymerization solution to wash, separating and extracting to collect an oil phase, and distilling under reduced pressure to obtain the oil-soluble polyether.
Example 10
The embodiment provides a preparation method of oil-soluble polyether, which comprises the following steps:
(a) adding catalyst lanthanum trifluoromethanesulfonate (0.60mmol, 352mg) into a dry three-neck round-bottom flask provided with a stirrer and a reflux condenser, vacuumizing and decompressing the reaction vessel, and replacing nitrogen for 3 times;
(b) under the protection of nitrogen, injecting 1, 2-epoxybutane (30mmol, 2160mg) and ethylene oxide (30mmol, 1320mg) into a three-neck round-bottom flask by a syringe to carry out polymerization reaction for 52h under the conditions that the temperature is 25 ℃ and the stirring speed is 500 r/min;
(c) adding 1mL of ethanol as a terminator to terminate the polymerization reaction, adding 5mL of deionized water into the polymerization solution to wash, separating and extracting to collect an oil phase, and distilling under reduced pressure to obtain the oil-soluble polyether.
The oil-soluble polyethers prepared in examples 1 to 10 were tested for their performance parameters and the results are shown in Table 1.
TABLE 1
As can be seen from the analysis of table 1, comparative example 1, example 3 and example 8, the smaller the amount of catalyst used, the lower the kinematic viscosity under the same conditions; it can be seen from the comparison of examples 3, 5, 6 and 7 that the oil-soluble polyether obtained by using lanthanum trifluoromethanesulfonate as a catalyst has lower kinematic viscosity, viscosity index and average molecular weight under the same reaction conditions. As can be seen from Table 1, the present invention realizes the preparation of oil-soluble polyethers under polymerization conditions of not more than 50 ℃ and simple treatments of water washing, extraction and distillation under reduced pressure.
In conclusion, the preparation method realizes the preparation of the oil-soluble polyether under mild polymerization conditions and simple post-treatment; the invention realizes the controllable polymerization of the molecular weight of the oil-soluble polyether by regulating and controlling the amount of the added catalyst, the molecular weight of the prepared polyether is between 500 and 2500, and the prepared polyether has wide application field as polyether base oil.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are only exemplary embodiments of the present invention, and are not intended to limit the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The preparation method of the oil-soluble polyether is characterized by comprising the following steps:
(1) mixing an epoxy monomer and a catalyst in a non-oxidizing atmosphere to carry out polymerization reaction;
(2) adding a terminator to terminate the polymerization reaction, and sequentially performing water washing, extraction and reduced pressure distillation to obtain the oil-soluble polyether;
the temperature of the polymerization reaction in the step (1) is 25-50 ℃;
the time of the polymerization reaction in the step (1) is 2-72 h;
the catalyst in the step (1) comprises metal triflate;
the metal triflate is a rare earth metal triflate;
the trifluoromethanesulfonic acid rare earth metal salt comprises any one of lanthanum trifluoromethanesulfonate, cerium trifluoromethanesulfonate, neodymium trifluoromethanesulfonate and gadolinium trifluoromethanesulfonate.
2. The method according to claim 1, wherein the non-oxidizing atmosphere in step (1) is a gas comprising any one of nitrogen, helium, neon, argon, krypton, or xenon, or a combination of at least two thereof.
3. The method according to claim 1, wherein the epoxy monomer of step (1) comprises propylene oxide and/or 1, 2-butylene oxide.
4. The method as claimed in claim 1, wherein the stirring rate of the polymerization reaction in step (1) is 1500 r/min.
5. The method according to claim 1, wherein the molar ratio of the catalyst to the epoxy monomer in the step (1) is (1-10): 500.
6. The preparation method according to claim 1, wherein the terminating agent in the step (2) comprises any one of water, alcohol compounds, phenolic compounds or amine compounds or a combination of at least two of the above compounds.
7. The method according to claim 6, wherein the alcohol compound comprises any one of ethanol, benzyl alcohol, ethylene glycol, or polyhydric alcohol, or a combination of at least two thereof.
8. The method of claim 6, wherein the phenolic compound comprises any one or a combination of at least two of phenol, p-cresol, hydroquinone, or p-tert-butylcatechol.
9. The method according to claim 6, wherein the amine compound comprises sodium dimethyldithiocarbamate.
10. The production method according to any one of claims 1 to 9, characterized by comprising the steps of:
(1) mixing an epoxy monomer and a catalyst in a non-oxidizing atmosphere, and carrying out a polymerization reaction for 2-72h at a temperature of 0-130 ℃ and a stirring speed of 300-700 r/min;
(2) adding a terminator to terminate the polymerization reaction, and sequentially carrying out water washing, extraction and reduced pressure distillation to obtain the oil-soluble polyether.
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| CN113831526B (en) * | 2021-10-27 | 2022-12-09 | 中国科学院过程工程研究所 | Polyether base oil and application thereof |
| CN113773485B (en) * | 2021-10-27 | 2022-10-28 | 中国科学院过程工程研究所 | Preparation method of polyether |
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