CN101851525B - Preparation of organic silicon petroleum de-emulsifier - Google Patents

Preparation of organic silicon petroleum de-emulsifier Download PDF

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Publication number
CN101851525B
CN101851525B CN 200910113488 CN200910113488A CN101851525B CN 101851525 B CN101851525 B CN 101851525B CN 200910113488 CN200910113488 CN 200910113488 CN 200910113488 A CN200910113488 A CN 200910113488A CN 101851525 B CN101851525 B CN 101851525B
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organic silicon
dimethylbenzene
reactor
pressure
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CN101851525A (en
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曾凡付
王刚
李攀峰
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DELAND WATER TECHNOLOGY Co.,Ltd.
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XINJIANG DELAN CO Ltd
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Abstract

The invention discloses the preparation of an organic silicon petroleum de-emulsifier, which comprises the following components in part by weight: 80 to 120 parts of organic silicon polyester, 80 to 120 parts of dimethylbenzene and 2.5 to 3.5 parts of toluene diisocynate. The de-emulsifier is prepared by the following steps of: adding the organic silicon polyester and the dimethylbenzene into a reactor; adding the toluene diisocynate into the reactor dropwise with stirring for 28 to 32 minutes when the mixed solution of the organic silicon polyester and the dimethylbenzene are heated to be between 70 and 80 DEG C; and continuously stirring the mixture for 90 to 100 minutes to obtain the de-emulsifier. In the invention, the organic silicon polyester is synthesized by using the following components in part by weight: 40 to 60 parts of dimethylbenzene, 0.8 to 1.3 parts of tetraethylene pentamine, 80 to 130 parts of epoxypropane, 160 to 270 parts of ethylene oxide and 250 to 400 parts of methyl silicone oil, wherein the synthesis is implemented by the following steps of: adding the solvent dimethylbenzene and the initiator tetraethylene pentamine into the reactor in sequence; uniformly mixing the materials in the reactor; adding the epoxypropane into the mixed solution when the mixed solution is heated to be between 120 and 130 DEG C and keeping the temperature between 120 and 130 DEG C to perform a reaction for 3 to 4 hours under the pressure of between 0.2 and 0.3 MPa; keeping the temperature and the pressure and adding the ethylene oxide into the reactor to perform a reaction for 2 to 3 hours; and lowering the temperature to 80 to 90 DEG C, adding the methyl silicone oil into the reactor under the pressure of between 0.4 and 0.5 MPa and keeping the temperature and pressure to perform a reaction for 4 to 5 hours to obtain the polyester product.

Description

A kind of preparation of organic silicon petroleum de-emulsifier
Technical field
The present invention relates to the demulsifier of oil extraction, is organosilicon type series, and the product of the crude oil demulsifier that obtains and application thereof are safe reliably.
Background technology
Crude oil demulsifier is oil extraction, implements the chemical agents of a large amount of uses of processed institute.At present main use alcohols polyether demulsification agent, polyethylene polyamine block polyether demulsifier, novolac systems demulsifier and composite product thereof etc. are arranged.Retrieving information discloses: the patent No. is the patent of 02138900.4 " a kind of broad spectrum type crude oil demulsifier ", with polynary polyethers, polyamine polyethers and the composite enhancing demulsifier of pour-point depressant adaptability.The patent No. is the patent of 98113742.3 " a kind of crude oil demulsifiers and preparation method thereof ", gets oxirane, propylene oxide block polyethers take ethylene glycol or propane diols as initiator and must adapt to the demulsifier of viscous crude with multi isocyanate crosslinking.Yet along with the exploitation in each oil field has entered the oil recovery stage in later stage in succession, some chemical agents that the later stage oil recovery adds and the quality retrogradation of oil have brought challenge to the breakdown of emulsion that recovers the oil, the breakdown of emulsion ability of existing demulsifier more and more can not satisfy the requirement of production well breakdown of emulsion, is badly in need of the strong novel demulsifier of exploitation breakdown of emulsion ability.Find that by research the key of crude oil demulsification is to reduce tension force and the interface film strength of oil-water interfaces, high molecular weight demulsifier is siliceous, has preferably hydrophilic ability, the wettability that has in addition and osmotic effect, the demulsifier molecule occupies larger sectional area at oil-water interfaces, thereby consumption is few, and demulsification is good.The Production requirement in oil field had both been satisfied in the present invention's design, can make again achievement in research can effectively be converted into productivity, constantly expanded the technology path of the novel demulsifier of improvement and increased the market share, walked Innovation.
Summary of the invention
The object of the invention is to: a kind of high-polymer strong demulsifier is provided, and its consumption is few, and energy consumption is low, can satisfy the development and use in the oil field that has entered tertiary oil recovery, has also opened up new approach for solving thickened oil recovery and volume increase.
The present invention seeks to realize like this: a kind of preparation of organic silicon petroleum de-emulsifier, with the parts by weight preparation, get organic silicon polyether 80-120 part, dimethylbenzene 80-120 part, toluene di-isocyanate(TDI) 2.5-3.5 part; Its best is formulated as 100 parts of machine silicon polyethers, 100 parts of dimethylbenzene, 3 parts of toluene di-isocyanate(TDI)s; When organic silicon polyether, dimethylbenzene are inserted in the reactor 70-80 ℃ of heating, need to stir, drip toluene di-isocyanate(TDI), the time is controlled at 28-32 minute, continues to stir namely to get demulsifier in 90-100 minute again.
The preparation of described demulsifier, synthesizing of organic silicon polyether got dimethylbenzene 40-60 part, TEPA 0.8-1.3 part, expoxy propane 80-130 part, oxirane 160-270 part, methyl-silicone oil 250-400 part with parts by weight; In reactor, add solvent xylene, initiator TEPA successively when synthetic, mix, when being heated to 120-130 ℃, add expoxy propane, the control temperature, react 3-4 hour at 0.2-0.3MPa at 120-130 ℃, pressure, and the maintenance temperature and pressure adds oxirane again, react and reduce the temperature to 80-90 ℃ after 2-3 hour, pressure is controlled at 0.4-0.5MPa and adds methyl-silicone oil, keeps temperature and pressure 4-5 hour, namely gets polyether product.
The preparation of described demulsifier, the dimethylbenzene of selecting, toluene di-isocyanate(TDI), TEPA, expoxy propane, oxirane, methyl-silicone oil are commercially available technical grade product.
Design of the present invention and know-why:
This demulsifier, take TEPA as initiator, connect oxygen ethene, oxypropylene block copolymerization, draw the long-chain organosilicon and get polyethers, use again toluene diisopropyl cyanate crosslinked, obtain high molecular weight demulsifier, the water that consumption is few, breakdown of emulsion power strong, deviate from is clear, and high asphalitine and the crude oil that contains other emulsifying agents are had good demulsification.
Technique effect of the present invention:
This demulsifier, to 50 ℃, viscosity of crude is 950mPa.S, oil density is 0.9822g/cm 3, the viscous crude oil exploitation that colloid, wax and asphalt content are higher; Higher to a large amount of use polymer oil recoveries or chemical agent content, crude oil emulsion is stable, the oil exploitation that the breakdown of emulsion difficulty is large, the same demulsification well that produces.
The present invention adopts oil and gas industry standard SY/T5281-2000, verifies that the dehydration experiment of its product the results are shown in Table.
Table
Figure G2009101134888D00021
Upper table result shows, crude oil demulsifier breakdown of emulsion ability of the present invention is strong, and viscous crude is had good demulsification performance, and breaking emulsion and dewatering efficient is higher than on-the-spot used demulsifier, and oil-water interfaces are clear, deviate from water colour limpid.
The present invention adopts the high-polymer strong demulsifier, makes the exploitation that enters three phase oil fields or the oil well of chronic administration chemical agent breakdown of emulsion, radiates vigour, and can make oil-water interfaces clear, deviates from the limpid technique effect of water colour, shows technological progress.
The specific embodiment
Be described further below in conjunction with embodiment.
Embodiment 1
Demulsifier is comprised of 3.5 parts of 80 parts of organic silicon polyethers, 120 parts of dimethylbenzene, toluene di-isocyanate(TDI);
Embodiment 2
Demulsifier is comprised of 2.5 parts of 90 parts of organic silicon polyethers, 80 parts of dimethylbenzene, toluene di-isocyanate(TDI);
Embodiment 3
Demulsifier is comprised of 3 parts of 100 parts of organic silicon polyethers, 100 parts of dimethylbenzene, toluene di-isocyanate(TDI);
Above-mentioned different preparation operates with same steps as: with parts by weight successively to reactor feed, add organic silicon polyether, dimethylbenzene, in the time of agitating heating 70-80 ℃, drip toluene di-isocyanate(TDI), time is controlled at 28-32 minute, continues stirring again and namely gets demulsifier in 90-100 minute.
Embodiment 4
Polyethers is comprised of 299 parts of 50 parts of dimethylbenzene, 1 part of TEPA, 99 parts of expoxy propane, 199 parts of methyl-silicone oils of oxirane;
Embodiment 5
Polyethers is comprised of 250 parts of 40 parts of dimethylbenzene, 0.8 part of TEPA, 80 parts of expoxy propane, 160 parts in oxirane, methyl-silicone oil;
Embodiment 6
Polyethers is comprised of 400 parts of 60 parts of dimethylbenzene, 1.3 parts of TEPAs, 130 parts of expoxy propane, 270 parts in oxirane, methyl-silicone oil;
Above-mentioned different preparation operates with same steps as: successively to reactor feed, add solvent xylene, initiator TEPA with parts by weight, mix, be heated to 130 ℃; Then add expoxy propane, the control temperature is 120 ℃, pressure 0.2MPa, reacts 4 hours; Under the condition of constant temperature and constant voltage, add oxirane, reacted 3 hours, reduce the temperature to 80 ℃, when pressure is controlled at 0.4Mpa, add methyl-silicone oil, kept temperature and pressure 5 hours, namely get organic silicon polyether.
Oil well experiment place:
The Tahe multi-purpose station: well water 28%, viscosity of crude are 950mPa.S, and oil density is 0.9822g/cm 3, belong to heavy oil wells.
Adopt demulsifier-TH-01,50mg/L, poor effect, but adopt demulsification performance, and breaking emulsion and dewatering efficient is higher than on-the-spot used demulsifier, and oil-water interfaces are clear, deviate from water colour limpid.

Claims (2)

1. the preparation of an organic silicon petroleum de-emulsifier is characterized in that: with the parts by weight preparation, get organic silicon polyether 80-120 part, dimethylbenzene 80-120 part, toluene di-isocyanate(TDI) 2.5-3.5 part; Organic silicon polyether, dimethylbenzene are inserted in the reactor, in the time of agitating heating 70-80 ℃, drip toluene di-isocyanate(TDI), the time is controlled at 28-32 minute, continues stirring again and namely gets demulsifier in 90-100 minute;
Wherein organic silicon polyether is synthetic, gets dimethylbenzene 40-60 part, TEPA 0.8-1.3 part, expoxy propane 80-130 part, oxirane 160-270 part, methyl-silicone oil 250-400 part with parts by weight; In reactor, add solvent xylene, initiator TEPA successively when synthetic, mix, when being heated to 120-130 ℃, add expoxy propane, the control temperature, react 3-4 hour at 0.2-0.3MPa at 120-130 ℃, pressure, and the maintenance temperature and pressure adds oxirane again, react and reduce the temperature to 80-90 ℃ after 2-3 hour, pressure is controlled at 0.4-0.5MPa and adds methyl-silicone oil, keeps temperature and pressure 4-5 hour, namely gets polyether product.
2. the preparation of demulsifier according to claim 1 is characterized in that: the dimethylbenzene of selecting, toluene di-isocyanate(TDI), TEPA, expoxy propane, oxirane, methyl-silicone oil are commercially available technical grade product.
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CN104448118B (en) * 2014-11-27 2016-05-25 新疆德蓝股份有限公司 A kind of low temperature crude oil demulsifier and preparation method thereof
CN106398748B (en) * 2015-07-27 2018-09-28 中国石油化工股份有限公司 A kind of method of hydrocarbon ils deferrization agent and hydrocarbon ils deferrization
CN106701151B (en) * 2015-07-27 2018-08-28 中国石油化工股份有限公司 A kind of method of hydrocarbon ils deferrization agent and hydrocarbon ils deferrization
CN114292664A (en) * 2021-12-28 2022-04-08 江苏汉光实业股份有限公司 Oil-soluble demulsifying desalting agent and preparation method thereof

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1223896A (en) * 1998-01-21 1999-07-28 辽河石油勘探局勘察设计研究院 Crude de-emulsifier and its preparing process
CN1396238A (en) * 2002-08-06 2003-02-12 中国石油化工集团公司 Broad-spectrum demulsifier for crude oil
CN1810933A (en) * 2006-03-13 2006-08-02 辽宁奥克化学集团有限公司 Thick oil demulsifier and its prepn
CN101407730A (en) * 2008-11-28 2009-04-15 句容市宁武化工有限公司 Preparation of high performance demulsifying agent
CN101497814A (en) * 2008-12-30 2009-08-05 江苏三星化工有限公司 Organosilicon reinforced composite type oil phase dispersed demulsifying agent

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1223896A (en) * 1998-01-21 1999-07-28 辽河石油勘探局勘察设计研究院 Crude de-emulsifier and its preparing process
CN1396238A (en) * 2002-08-06 2003-02-12 中国石油化工集团公司 Broad-spectrum demulsifier for crude oil
CN1810933A (en) * 2006-03-13 2006-08-02 辽宁奥克化学集团有限公司 Thick oil demulsifier and its prepn
CN101407730A (en) * 2008-11-28 2009-04-15 句容市宁武化工有限公司 Preparation of high performance demulsifying agent
CN101497814A (en) * 2008-12-30 2009-08-05 江苏三星化工有限公司 Organosilicon reinforced composite type oil phase dispersed demulsifying agent

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Address after: 830013 Urumqi high tech Zone (new city) North Industrial Park, blue sky road, No. 216, No.

Patentee after: DELAND WATER TECHNOLOGY Co.,Ltd.

Address before: 830011 No. 682 South Tianjin Road, the Xinjiang Uygur Autonomous Region, Urumqi

Patentee before: XINJIANG DELAND Co.,Ltd.

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