CN105622918B - A kind of polymer, preparation method and the usage - Google Patents
A kind of polymer, preparation method and the usage Download PDFInfo
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Abstract
The invention provides a kind of polymer, preparation method and the usage.The structure of Inventive polymers is：Wherein X group is
Description
Technical field
The present invention relates to a kind of polymer, more particularly to a kind of polymer as lubricant demulsifier.
Background technology
Lubricating oil frequently encounters the situation of water, such as bunker oil, industrial gear oil, Oil Film of Bearing Oil etc. when working, this
A little lubricating oil easily form the emulsification system of Water-In-Oil with water, are especially containing more metal detergent, ashless dispersant
Or during extreme pressure anti-wear additives, the surface-active of lubricating oil improves, and oil water interfacial tension reduces, and emulsification of lubricating oils situation can be tighter
Weight.If water-oil separating can not be realized in time, it will deteriorate the lubrication state of lubricating oil, the lighter can influence the formation of oil film, drop
Low lubricating ability, severe one can cause the corrosion and abrasion of machinery, or even infringement equipment, influence production and safety.Therefore, lubricating oil
Demulsification resistance be an important physical and chemical index.
In lubricating oil breaking method, addition demulsifying agent makes the chemical demulsification method of the profit quick separating of lubricating oil, is not required to
Additionally to increase equipment, not only simply, it is convenient but also economical, while the physicochemical property of oil product is typically had no adverse effects, is a kind of head
The method of choosing.Therefore the development for demulsifier, there are many research reports, wherein main demulsifier is with oxirane, ring
Ethylene Oxide and initiator react obtained polyether compound.
Such as：US 2979528 describes nitrogenous Pluronic F-127, propylene oxide composition detersive, wherein not surpass
The nitrogen-containing compound for crossing 6 carbon atoms is initial action raw material, and these nitrogen-containing compounds can be ammonia, secondary amine, alkenyl polyamine, alcohol
Amine, piperazine, alkyl-substituted piperazine, ammoniacal liquor, phenol amine, wherein oxygen propyl group chain are connected with being connected the atom of reactive hydrogen, oxyethylene chain
It is connected with oxypropylene group chain end.The mean molecule quantity of oxygen propyl group chain is 900~25000, and oxyethylene chain accounts for the 20% of compound
~90%, the compound has preferable detergency.
US 4596653 describes a kind of preparation method of profit demulsifier, wherein using polysiloxanes and polyoxygenated alkene
Copolymer, wherein polyoxygenated alkene is formed by the random copolymerization of oxireme and propylene oxide monomer, prepared demulsification
Agent is applied to crude oil demulsification.
CN 100516116C describe a kind of synthetic method of multi block copolyether emulsion resistant agent, wherein using mesoporous silicon
Oxide carried potassium or silicon-Zirconium oxide load potassium catalyst, use monohydric alcohol, dihydric alcohol, polyalcohol as initiator, with epoxy
Oxide-propylene oxide carries out block copolymerization reaction, is then post-processed to obtain object.The more blocks of product that this method obtains
Copolyether emulsion resistant agent is copolymerized, molecular weight is 4800~5500, overall excellent demulsification performance, and production application cost is relatively low, is applicable profit
Lubricating oil oil product is in extensive range, structure-controllable, it is low foaming, it is less toxic, efficient, environmentally friendly.
US 3957854A, US 3957854A describe a kind of ester type demulsifier, are the carboxylic acyl radicals by HMW
More alcoxyl alkenyl alcohols of agent and aqueous phase react to obtain esterification products, and this esterification products can be used for lubricating oil and liquid fuel
Demulsification.
US 5407585A, US 5505878A describe a kind of synthetic method of oil-in-water type demulsifier, wherein using broken
Emulsion is the polyene ethyl glycol and oxirane either polypropylene oxide and 2-glycidyl that molecular weight is 8000~18000
Ether addition reaction obtains, and this demulsifier has good demulsification, can be used alone, can also be with other demulsifiers together
Use.
Also have and the patent that various demulsifiers reach demulsification is applied in combination, such as：CN1013502B describes a kind of profit
Lubricating oil anti-emulsifying compound additive, be by mean molecule quantity 2000~10000 the poly- trimethylene derivative of alkylene diamine four and be selected from
C10~C20 alkenyl succinic acids, C10~C36 carboxylic acid dimerizations, the saturated or unsaturated aliphatic acid of C10~C22 it is a kind of organic
Carboxylic acid composition forms.The anti-emulsifying compound agent is used as the lubricating oil component including steam turbine oil, gear oil, hydraulic oil, can
Effectively improve its demulsification performance and rustless property.
Although the demulsifier of document above introduction can be used for lubricating oil demulsification, there are still demulsification is effective
Fruit is bad, it is necessary to the problem of adding more demulsifier.In addition, some demulsifiers, particularly polyethers demulsifier is due to containing parent
Water base group and easily separated with oil phase, not only cause the production cost of lubricating oil to rise, while be also not easy to ensure lubricating oil
Quality.Therefore, existing lubricating oil still has limitation, it is necessary to further improve with demulsifier.
The content of the invention
The invention provides a kind of polymer, preparation method and the usage.
The structure of Inventive polymers is：
Wherein X group isA be 10~100 between integer, preferably 15~80, most
It is preferred that 20~60, b are the integer between 5~100, preferably 5~60, most preferably 10~40；M is the integer between 1~10, preferably
1~6, most preferably 1~2；N is the integer between 1~10, and the n on each sulphur bridge can be the same or different, preferably 1~6,
Most preferably 1~4；R is C1~C18 alkyl or its mixed alkyl, preferably C3~C15 alkyl or its mixed alkyl, most preferably C3~
C12 alkyl or its mixed alkyl.
The preparation method of the polymer of the present invention includes：By sulfenyl phenolate first with Polymerization of Propylene Oxide, again with epoxy second
Alkane polymerize, and collects product.
The sulfenyl phenolate is vulcanization C1~C18 alkyl phenols, preferably vulcanizes C3~C15 alkyl phenols, most preferably vulcanizes C3
~C12 aligns alkyl phenol；The sulfenyl phenolate is reacted to obtain by alkyl phenol with vulcanizing agent, and the vulcanizing agent can select sulphur
One or more in sulphur, sulfur chloride and sulfur dichloride, the mol ratio of the alkyl phenol and the vulcanizing agent is 1~3：3~1,
The temperature of vulcanization be normal temperature to 200 DEG C, the sulfur content of obtained sulfenyl phenolate is 5%~30%.
The mol ratio of phenolic hydroxyl group and expoxy propane in the sulfenyl phenolate is 1：10~100, preferably 1：15~80, most
It is preferred that 1：20~60；The mol ratio of phenolic hydroxyl group and oxirane in the sulfenyl phenolate is 1：5~100, preferably 1：5~
60, most preferably 1：10~40.
When preparing the polymer of the present invention, solvent, most preferably the solvent preferred aromatic hydrocarbons solvent, dimethylbenzene are preferably added to
And/or toluene, the mass ratio preferably 1 of the sulfenyl phenolate and the solvent：0.1~50, more preferably 1：0.2~20, it is optimal
Select 1：0.5~10.
When preparing the polymer of the present invention, catalyst is preferably added to, the catalyst preferred alkali metal hydroxide, most
It is preferred that potassium hydroxide and/or sodium hydroxide, the mol ratio preferably 1 of the sulfenyl phenolate and the catalyst：1~20, it is more excellent
Select 1：1~10, most preferably 1：3~8.
The sulfenyl phenolate and expoxy propane, the reaction pressure of ethylene oxide polymerization are 0.1~1MPa, preferably 0.1~
0.8MPa, most preferably 0.2~0.6MPa；Reaction temperature be 80 DEG C~200 DEG C, preferably 100 DEG C~160 DEG C, most preferably 120 DEG C~
140℃；Reaction time is 1~10 hour, preferably 2~8 hours, most preferably 2~4 hours.
After polymerisation terminates, 60~90 DEG C of petroleum ethers, 10% sulfuric acid solution, neutralization reaction are added into reaction product
Product after dividing water, drying, adds neutral oil, steams solvent, obtain sulfenyl phenolate expoxy propane ethylene oxide polymerization to neutrality
Thing.
The molecular weight of Inventive polymers is 1000~30000, preferably 5000~20000, most preferably 10000~20000.
The polymer of the present invention may be used as lubricant demulsifier, and stability is good in lubricating oil, and has excellent oil
Water separating effect, demulsification, the separation of minor amount of water suitable for lubricating oil, can be used for industrial gear oil, steam turbine oil, ship
Use crankcase oils.
Embodiment
The present invention is further illustrated below by example, but the present invention is not limited thereto.
Unless stated otherwise, percentage as described below is mass percent.
Test method and experiment raw material
The oil of 1.GB/T 7305 and Synthesis liquid resistance to emulsion pipette method：
In graduated cylinder, under measurement temperature, it will be stirred as defined in sample and each 40mL loadings of distilled water with 1500r/min rotating speed
Mix and keep standing after 5min, and start timing, record Synthesis liquid, water and remaining emulsification volume integral do not reach 40mL, 37mL,
3mL either 40mL, 40mL, 0mL when time, the time used is shorter, illustrates that the resistance to emulsion of oil product is better.If left standing for
(when test temperature is 82 ± 1 DEG C, oil and water still can not separate, then report oil by 30min (test temperature is 54 ± 1 DEG C) or 1h
The either milliliter number of Synthesis liquid, water and remaining emulsion volume.It is qualified to be basically separated to reach 40-37-3, reaches 40-40-0
To be kept completely separate.
2. test raw materials
The physical and chemical index of the lube base oil of table 1
The lube oil additive species of table 2 and producer
| Additive | Title | Source |
| T102 | Middle base number calcium mahogany sulfonate | Sinopec Shanghai additive factory |
| T307 | D2EHDTPA amine salt | Liaoning Tianhe Fine Chemical Co., Ltd. |
| T321 | Sulfide isobutene | Liaoning Tianhe Fine Chemical Co., Ltd. |
| T405 | Sulfurized olefin cotton oil | Liaoning Tianhe Fine Chemical Co., Ltd. |
| T451 | Phosphate | Jiangsu Hai'an petrochemical plant |
| T502A | Liquid mixed type shields phenol | Liaoning Tianhe Fine Chemical Co., Ltd. |
| T551 | Benzotriazole derivative | Liaoning Tianhe Fine Chemical Co., Ltd. |
| T746 | Alkenyl succinic acid | Liaoning Tianhe Fine Chemical Co., Ltd. |
| T1001 | Ethylenediamine propylene oxide polyether compound | Jinzhou Kangtai Lube Additive Co., Ltd. |
| DL32 | SYNPERONIC PE/F68 | Wuxi south additive Co., Ltd |
Sulfenyl phenolate A synthesis
With temperature control and water cooling, stirring 500ml three-necked flasks in add nonyl phenol 100 grams (0.455mol), 100mL
N-decane, sulphur 35 grams (1.09mol) is added, is then gradually heating to 160 DEG C, reaction mass is protected with nitrogen, while will be anti-
Tail gas is answered to be passed through 10% sodium hydroxide solution, the hydrogen sulfide gas generated with absorbing reaction, now nonyl phenol is by colourless gradually change
For dark brown, black liquor is eventually become, after reacting 4 hours, is evaporated under reduced pressure, it is 165 DEG C to control temperature, is obtained after steaming desolventizing
Sulfenyl phenolate A, sulfur content is measured as 23.9%.Determined with VPO methods, vulcanization nonyl phenol A mean molecule quantity is (equivalent for 881
Contain 3 alkyl phenols in each molecule, 3.5) m 1, number of sulfur atoms n average value is.
Sulfenyl phenolate B synthesis
With temperature control and water cooling, stirring 500ml three-necked flasks in add dodecylphenol 100 grams (0.382mol),
60~90 DEG C of petroleum ethers of 100ml, control temperature be 25~35 DEG C, then be added dropwise sulfur monochloride 36 grams (0.267mol), then by
160 DEG C are gradually warming up to, reaction mass is protected with nitrogen, while reaction end gas is passed through 10% sodium hydroxide solution, it is anti-to absorb
The hydrogen chloride gas that should be generated, now dodecylphenol gradually become dark brown by colourless, black liquor is eventually become, by 5
Dripped off after hour, then heat to 100 DEG C, desolvation, obtain sulfenyl phenolate B, measure sulfur content as 14.7%.Use VPO
Method determines, and vulcanization dodecylphenol B mean molecule quantity (contains 3 alkyl phenols, m 1, sulphur original for 912 in equivalent each molecule
2) subnumber n is.
Sulfenyl phenolate C synthesis
With temperature control and water cooling, stirring 500ml three-necked flasks in add nonyl phenol 100 grams (0.455mol), 100mL
N-decane, sulfur dichloride 35.1 grams (0.34mol) is added, is then gradually heating to 160 DEG C, protect reaction mass with nitrogen, together
When reaction end gas is passed through 10% sodium hydroxide solution, the hydrogen chloride gas generated with absorbing reaction, now nonyl phenol is by colourless
Dark brown is gradually become, eventually becomes black liquor, after reacting 4 hours, is evaporated under reduced pressure, it is 165 DEG C to control temperature, steams desolventizing
After obtain sulfenyl phenolate C, measure sulfur content as 10.2%, determined with VPO methods, vulcanization nonyl phenol A mean molecule quantity is 970
(convert into and contain 4 alkyl phenols in each molecule, 1) m 2, number of sulfur atoms n is.
The sulfenyl phenolate expoxy propane ethylene oxide polymer M1 of embodiment 1 preparation
With motor agitators and condensation, heating mantle 250 milliliters of autoclaves in, add sulfenyl phenolate A 3.4
Gram (0.0039mol, containing 0.012mol phenolic hydroxyl groups), 5 grams of dimethylbenzene, 1 gram of solid potassium hydroxide (0.0179mol), Ran Houyong
Nitrogen displacement is warming up to 90 DEG C afterwards three times；30 grams of expoxy propane (0.517mol) are added dropwise into autoclave, control reaction pressure
0.6MPa, reaction temperature are 122 DEG C, are reacted 2.5 hours；Oxirane 12 grams (0.272mol), control are added dropwise into autoclave
Reaction pressure 0.5MPa, reaction temperature are 125 DEG C, are reacted 2 hours；Reaction is transferred the material into 200ml beakers after terminating, and is added
Enter 60~90 DEG C of 30 grams of petroleum ethers, 50 milliliters of 10% sulfuric acid solution, the potassium hydroxide remained in neutralization reaction product, and spend
Ion water washing, until reaction product is in neutrality；12 grams of HVI150 neutral oils are added, the oil reservoir in material is put into vacuum distillation
Device, 53.3 grams of product is obtained after steaming solvent, as vulcanize nonyl phenol expoxy propane ethylene oxide polymer M1, infrared analysis
As a result show, 723cm in product-1Neighbouring peak corresponds to the stretching vibration peak of S -- S, 1500cm-1、1249cm-1Neighbouring peak is corresponding
In aromatic ring and the stretching vibration peak of hydroxyl oxygen, in 1060~1150cm-1Nearby there is the stretching vibration peak of alkyl ehter bond,
2900cm-1Neighbouring peak corresponds to methyl and methylene stretching vibration peak, and the compound for showing generation is sulfenyl phenolate epoxy third
Alkane ethylene oxide polymer, determination of elemental analysis sulfur content are 1.56%, and it is 11094 that by gpc analysis, it, which counts equal molecular mass,.
The sulfenyl phenolate expoxy propane ethylene oxide polymer M2 of embodiment 2 preparation
With motor agitators and condensation, heating mantle 250 milliliters of autoclaves in, add sulfenyl phenolate B 4.25
Gram (0.00467mol, containing 0.014mol phenolic hydroxyl groups), 6 grams of dimethylbenzene, 1.2 grams of solid potassium hydroxides (0.0214mol), then
90 DEG C are warming up to afterwards three times with nitrogen displacement；28 grams of expoxy propane (0.483mol) are added dropwise into autoclave, control reaction pressure
0.6MPa, reaction temperature are 122 DEG C, are reacted 2.5 hours；Oxirane 17 grams (0.386mol), control are added dropwise into autoclave
Reaction pressure 0.5MPa, reaction temperature are 125 DEG C, are reacted 3 hours；Reaction is transferred the material into 200ml beakers after terminating, and is added
Enter 60~90 DEG C of 40 grams of petroleum ethers, add in 10% 50 milliliters of neutralization reaction products of sulfuric acid solution the potassium hydroxide remained, and
It is washed with deionized, until reaction product is in neutrality；10 grams of 6# hydrogenated oils are added, the oil reservoir in material is put into vacuum distillation
Device, 58.8 grams of thick liquid is obtained after steaming solvent, as vulcanizes dodecylphenol expoxy propane ethylene oxide polymer M2,
Infrared analysis result shows, 723cm in product-1Neighbouring peak corresponds to the stretching vibration peak of S -- S, 1500cm-1、1249cm-1It is attached
Nearly peak corresponds to the stretching vibration peak of aromatic ring and hydroxyl oxygen, in 1060~1150cm-1Nearby there is the stretching vibration of alkyl ehter bond
Peak, in 2900cm-1Neighbouring peak corresponds to methyl and methylene stretching vibration peak, and the compound for showing generation is sulfenyl phenolate ring
Ethylene Oxide ethylene oxide polymer, determination of elemental analysis sulfur content are 1.06%, and by gpc analysis, its equal molecular mass of number is
10366。
The sulfenyl phenolate expoxy propane ethylene oxide polymer M3 of embodiment 3 preparation
With motor agitators and condensation, heating mantle 250 milliliters of autoclaves in, add sulfenyl phenolate C 3.0
Gram 5 grams of (0.0031mol, containing 0.0124mol phenolic hydroxyl groups) dimethylbenzene, 1.3 grams of solid potassium hydroxides (0.0232mol), then
90 DEG C are warming up to afterwards three times with nitrogen displacement；22 grams of expoxy propane (0.38mol) are added dropwise into autoclave, control reaction pressure
0.6MPa, reaction temperature are 122 DEG C, are reacted 2.5 hours；Oxirane 20 grams (0.455mol), control are added dropwise into autoclave
Reaction pressure 0.5MPa, reaction temperature are 125 DEG C, are reacted 3 hours；Reaction is transferred the material into 200ml beakers after terminating, and is added
Enter 60~90 DEG C of 35 grams of petroleum ethers, add in 10% 50 milliliters of neutralization reaction products of sulfuric acid solution the potassium hydroxide remained, and
It is washed with deionized, until reaction product is in neutrality；9 grams of HVI150 oil is added, the oil reservoir in material is put into vacuum distillation
Device, 54.6 grams of thick liquid is obtained after steaming solvent, as vulcanization nonyl phenol expoxy propane ethylene oxide polymer M3, it is infrared
Analysis result shows, 723cm-1Neighbouring peak corresponds to the stretching vibration peak of S -- S, 1500cm-1、1249cm-1Neighbouring peak corresponds to
The stretching vibration peak of aromatic ring and hydroxyl oxygen, in 1060~1150cm-1Between peak correspond to alkyl ehter bond stretching vibration peak,
2900cm-1Neighbouring peak corresponds to methyl and methylene stretching vibration peak, and the compound for showing generation is sulfenyl phenolate epoxy third
Alkane ethylene oxide polymer, determination of elemental analysis sulfur content are 0.57%, and it is 14353 that by gpc analysis, it, which counts equal molecular mass,.
The alkyl phenol expoxy propane ethylene oxide polymer N1 of comparative example 1 synthesis
With motor agitators and condensation, heating mantle 250 milliliters of autoclaves in, add 2.8 grams of nonyl phenol
(0.0127mol, containing 0.0127mol phenolic hydroxyl groups), 1 gram of solid potassium hydroxide (0.0179mol), then with being risen after nitrogen displacement
Temperature is to 92 DEG C；30 grams of expoxy propane (0.517mol) are added dropwise into autoclave, control reaction pressure 0.6MPa, reaction temperature is
125 DEG C, react 2.5 hours；Oxirane 12 grams (0.272mol) is added dropwise into autoclave, controls reaction pressure 0.5MPa, instead
It is 125 DEG C to answer temperature, is reacted 2 hours；Reaction is transferred the material into 200ml beakers after terminating, and adds 60~90 DEG C of petroleum ethers
50 grams, the potassium hydroxide remained in 10% 50 milliliters of neutralization reaction products of sulfuric acid solution, and be washed with deionized, until anti-
Product is answered in neutrality；12 grams of HVI150 neutral oils are added, the oil reservoir in material is put into vacuum distillation apparatus, are obtained after steaming solvent
To 55.6 grams of thick liquid, infrared analysis result shows, 1500cm-1、1249cm-1Neighbouring peak corresponds to aromatic ring and hydroxyl oxygen
Stretching vibration peak, 1060~1150cm-1Between peak correspond to the stretching vibration peak of alkyl ehter bond, in 2900cm-1Neighbouring peak corresponds to
Methyl and methylene stretching vibration peak, the compound for showing generation is nonyl phenol expoxy propane ethylene oxide polymer N1, is passed through
Its equal molecular mass of number of gpc analysis is 3561.
The alkyl phenolic resin expoxy propane ethylene oxide polymer N2 of comparative example 2 synthesis
Nonyl phenol phenolic resin is synthesized first, and its method is：In three mouthfuls equipped with 0.6mol nonyl phenols and 0.2mol KOH
In flask, 90 DEG C are warming up to, 37% formaldehyde (formaldehyde amount 0.4mol) is then added dropwise, time for adding was at 0.5~1 hour, then
115 DEG C of reaction 1.5h are warming up to, finally obtain phenolic resin in 160 DEG C of vacuum dehydrations, nonyl phenol and methylene in phenolic resin
Mol ratio be 3:2, molecular weight 685.
Followed by polymer N2 synthesis：
With motor agitators and condensation, heating mantle 250 milliliters of autoclaves in, add above-mentioned nonyl phenolic aldehyde tree
Fat 2.74 grams (0.004mol, containing phenolic hydroxyl group 0.012mol), 1 gram of solid potassium hydroxide (0.0179mol), is then put with nitrogen
92 DEG C are warming up to after changing；30 grams of expoxy propane (0.517mol) are added dropwise into autoclave, control reaction pressure 0.6MPa, reaction temperature
Spend for 125 DEG C, react 2.5 hours；Oxirane 12 grams (0.272mol) is added dropwise into autoclave, controls reaction pressure
0.5MPa, reaction temperature are 125 DEG C, are reacted 2 hours；Reaction is transferred the material into 200ml beakers after terminating, and adds 60~90
DEG C 55 grams of petroleum ether, 50 milliliters of 10% sulfuric acid solution, the potassium hydroxide remained in neutralization reaction product, and be washed with deionized water
Wash, until reaction product is in neutrality；12 grams of HVI150 neutral oils are added, the oil reservoir in material is put into vacuum distillation apparatus, are steamed
54.9 grams of thick liquid, as nonyl phenol expoxy propane ethylene oxide polymer N2 are obtained after going out solvent, passes through its number of gpc analysis
Equal molecular mass is 10557.
The embodiment 4~9 and comparative example 3~10 of Industrial gear oil composition
Be separately added into 1.2% T321,1.5% T307,0.1% T405,0.1% T451,0.06% T102,
The Inventive polymers or contrast demulsifier, the base oil for then adding surplus of 0.05% T502A, 0.02% or 0.03% are matched somebody with somebody
The embodiment 4~9 and comparative example 3~10 of L-CKD N220 industrial gear oils is made, the base oil is to be by mass ratio
7：3 HVI750 and 150BS is modulated and obtained；Be added without demulsifier for blank sample.
The embodiment 10~15 and comparative example 11~18 of turbine oil composition
Be separately added into 0.5% T502A antioxidant, 0.1% T551 metal deactivators, 0.1% T746 antirust agent,
0.01% or 0.02% Inventive polymers or contrast demulsifier, the base oil for then adding surplus are prepared to obtain L-TSA32
The embodiment 10~15 and comparative example 11~18 of steam turbine oil, the base oil be by mass ratio be 1：4 HVI 200N and HVI
150 modulate and obtain；Be added without demulsifier for blank sample.
Above-mentioned industrial gear oil, turbine oil composition and respective blank sample are resisted according to the methods of GB/T 7305
Emulsification test.
Polymer or contrast demulsifier in industrial gear oil, the embodiment of turbine oil composition, comparative example and blank sample
Type and addition be shown in Table 3, table 4 respectively, its demulsibility test result is also the same as being shown in Table 3,4.
The embodiment 4~9 and comparative example 3~10 of the Industrial gear oil composition of table 3
The embodiment 10~15 and comparative example 11~18 of the turbine oil composition of table 4
As can be seen from the above results, the industrial gear oil modulated using Inventive polymers as demulsifier, steam turbine oil group
Compound has preferable demulsification performance, better than traditional polyether demulsification agent T1001, DL32, and also superior to alkylphenol formaldehyde tree
Fat polyether demulsification agent.
Claims (11)
1. a kind of polymer, its structure are：
Wherein X group isA be 10~100 between integer, b be 5~100 between it is whole
Number；M is the integer between 1~10；N is the integer between 1~10, and the n on each sulphur bridge can be the same or different；R is each
From independently selected from C1~C18 alkyl.
2. according to the polymer described in claim 1, it is characterised in that a is the integer between 15~80, between b is 5~60
Integer；M is the integer between 1~6；N is the integer between 1~6；R is each independently selected from C3~C15 alkyl.
3. the preparation method of the polymer of claim 1 or 2, including：By sulfenyl phenolate first with Polymerization of Propylene Oxide, again with
Ethylene oxide polymerization, collect product.
4. in accordance with the method for claim 3, it is characterised in that the sulfenyl phenolate is vulcanization C1~C18 alkyl phenols.
5. in accordance with the method for claim 3, it is characterised in that phenolic hydroxyl group and expoxy propane in the sulfenyl phenolate
Mol ratio is 1：10~100；The mol ratio of phenolic hydroxyl group and oxirane in the sulfenyl phenolate is 1：5~100.
6. in accordance with the method for claim 3, it is characterised in that add solvent, the sulfenyl phenolate in the polymerization
Mass ratio with the solvent is 1：0.1~50.
7. in accordance with the method for claim 3, it is characterised in that add catalyst, the alkyl monosulfide in the polymerization
The mol ratio of phenol and the catalyst is 1：1~20.
8. in accordance with the method for claim 7, it is characterised in that the catalyst is alkali metal hydroxide.
9. in accordance with the method for claim 3, it is characterised in that the sulfenyl phenolate gathers with expoxy propane, oxirane
The reaction pressure of conjunction is 0.1~1MPa, and reaction temperature is 80 DEG C~200 DEG C, and the reaction time is 1~10 hour.
10. in accordance with the method for claim 3, it is characterised in that the molecular weight of the polymer is 1000~30000.
11. the polymer described in one of claim 1-10 is used as lubricant demulsifier.
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| CN103725358A (en) * | 2012-10-15 | 2014-04-16 | 中国石油化工股份有限公司 | Preparation method for vulcanized alkylphenol |
| CN103965459A (en) * | 2014-05-13 | 2014-08-06 | 新疆福利精细化工厂 | Preparation method of demulsifying agent |
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|---|---|---|---|---|
| US4973764A (en) * | 1986-10-24 | 1990-11-27 | Exxon Research And Engineering Company | Alkylphenols and derivatives thereof via phenol alkylation by cracked petroleum distillates |
| CN103725358A (en) * | 2012-10-15 | 2014-04-16 | 中国石油化工股份有限公司 | Preparation method for vulcanized alkylphenol |
| CN103183821A (en) * | 2013-04-16 | 2013-07-03 | 西南石油大学 | Block polymer demulsifier employing isostearyl alcohol as initiator and preparation method of block polymer demulsifier |
| CN103965459A (en) * | 2014-05-13 | 2014-08-06 | 新疆福利精细化工厂 | Preparation method of demulsifying agent |
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