CN104004181B - A kind of poly-flooding produced liquid process emulsion splitter and preparation method thereof - Google Patents
A kind of poly-flooding produced liquid process emulsion splitter and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of poly-flooding produced liquid process emulsion splitter and preparation method thereof.Gather the structure of flooding produced liquid process emulsion splitter such as formula shown in II, wherein, initiator shown in F-xy expression I.The preparation method of initiator shown in formula I comprises the steps: that (1) is under anaerobic and catalyzer existent condition, and polytetrahydrofuran and butylene oxide ring carry out polyreaction; (2) in step (1) reaction system after completion of the reaction, add propylene oxide, again carry out polyreaction, obtain described initiator.The preparation method of emulsion splitter shown in formula II comprises the steps: that (1) is under anaerobic and catalyzer existent condition, and initiator shown in formula I and oxyethane carry out polyreaction; (2) in step (1) reaction system after completion of the reaction, add propylene oxide, again carry out polyreaction, obtain described poly-flooding produced liquid process emulsion splitter.The emulsion splitter that the present invention obtains, gathers to oil field the crude oil emulsion driving rear generation and has good demulsification.
Description
Technical field
The present invention relates to a kind of emulsion splitter and preparation method thereof, be specifically related to a kind of poly-flooding produced liquid process emulsion splitter and preparation method thereof, belong to technical field of petrochemical industry.
Background technology
At present, numerous domestic oil field has entered the poly-stage of note comprehensively, and polymer flooding exists larger nature difference relative to water drive Produced Liquid.For poly-flooding produced liquid, residual polymer is distributed in aqueous phase and water-oil interface result in the enhancing of water-oil emulsion stability, and during breakdown of emulsion, dehydration rate reduces.So far, the emulsion splitter that each oil field uses mainly proposes for crude oil emulsion after water drive, and to drive the work that rear crude oil emulsion breakdown of emulsion emulsion splitter carries out also little for poly-.Therefore, synthesize a class can realize improving the poly-emulsion splitter driving rear crude oil emulsion breaking emulsion and dewatering rate, for field produces, there is certain directive significance.
Summary of the invention
The object of this invention is to provide a kind of poly-flooding produced liquid process emulsion splitter and preparation method thereof, emulsion splitter provided by the invention take polytetrahydrofuran as raw material, and the block polyether being comonomer with butylene oxide ring, propylene oxide and oxyethane gathers the emulsion splitter of flooding produced liquid process.
The invention provides initiator shown in a kind of formula I,
In formula I, the value of x/y is 19 ~ 39:20 ~ 40.
Shown in above-mentioned formula I, the preparation method of initiator, comprises the steps:
(1) under anaerobic and catalyzer existent condition, polytetrahydrofuran and butylene oxide ring carry out polyreaction;
Described catalyzer is any one in potassium hydroxide, sodium hydroxide, hydrated barta and lime acetate;
(2) in step (1) reaction system after completion of the reaction, add propylene oxide, again carry out polyreaction, obtain described initiator.
Above-mentioned preparation method, in step (1) and step (2), the temperature of described polyreaction is not all higher than 140 DEG C, and pressure is not all higher than 0.4MPa.
The temperature of above-mentioned polyreaction specifically can be 120 DEG C ~ 140 DEG C; Pressure specifically can be 0 ~ 0.4MPa, the pressure of this reaction system is that reaction raw materials butylene oxide ring or propylene oxide self produce, and along with the minimizing of reaction raw materials, the pressure of reaction system reduces gradually, when reaction raw materials reacts completely, the pressure in reaction system is just reduced to zero; So the pressure in this reaction process is change, only need be controlled it not higher than 0.4MPa.
Above-mentioned preparation method, the amount of the described catalyzer added in step (1) can be 0.2% ~ 0.6% of the total mass of the described propylene oxide added in the described polytetrahydrofuran and described butylene oxide ring and step (2) added in step (1), specifically can be 0.26%, 0.35% or 0.52%.
In above-mentioned preparation method, the mass ratio added of described polytetrahydrofuran, described butylene oxide ring and described propylene oxide can be 1:19 ~ 39:20 ~ 40, specifically can be 1:19:20,1:39:40,1:39:20 or 1:39:40.
Present invention also offers poly-flooding produced liquid process emulsion splitter shown in a kind of formula II,
In formula II, initiator shown in F-xy expression I, a:b:c is 1 ~ 8:1 ~ 7:2 ~ 8;
In formula I, the value of x/y is 19 ~ 39:20 ~ 40.
Shown in above-mentioned formula III, the preparation method of poly-flooding produced liquid process emulsion splitter, comprises the steps:
(1) under anaerobic and catalyzer existent condition, initiator shown in formula I and oxyethane carry out polyreaction;
Described catalyzer is any one in potassium hydroxide, sodium hydroxide, hydrated barta and lime acetate;
(2) in step (1) reaction system after completion of the reaction, add propylene oxide, again carry out polyreaction, obtain described poly-flooding produced liquid process emulsion splitter;
Above-mentioned preparation method, in step (1), the temperature of described polyreaction is not higher than 130 DEG C, and pressure is not higher than 0.4MPa; In step (2), the temperature of described polyreaction is not higher than 140 DEG C, and pressure is not higher than 0.4MPa.
In above-mentioned steps (1), the temperature of described polyreaction specifically can be 120 DEG C ~ 130 DEG C, pressure specifically can be 0 ~ 0.4MPa, the pressure of this reaction system is that reaction raw materials butylene oxide ring or propylene oxide self produce, along with the minimizing of reaction raw materials, the pressure of reaction system reduces gradually, and when reaction raw materials reacts completely, the pressure in reaction system is just reduced to zero; So the pressure in this reaction process is change, only need be controlled it not higher than 0.4MPa.
In above-mentioned steps (2), the temperature of described polyreaction specifically can be 120 DEG C ~ 140 DEG C, and pressure specifically can be 0 ~ 0.4MPa.The pressure of this reaction system is that reaction raw materials butylene oxide ring or propylene oxide self produce, and along with the minimizing of reaction raw materials, the pressure of reaction system reduces gradually, and when reaction raw materials reacts completely, the pressure in reaction system is just reduced to zero; So the pressure in this reaction process is change, only need be controlled it not higher than 0.4MPa.
The add-on of described catalyzer can be 0.2% ~ 1.2% of initiator shown in formula I, described oxyethane and described propylene oxide total mass, specifically can be 0.3%, 1.04% or 1.2%;
The mass ratio added of initiator shown in formula I, described oxyethane and described propylene oxide can be 1 ~ 8:1 ~ 7:2 ~ 8, specifically can be 1:2:7,2:1:2,1:3:6 or 8:7:8.
The molecular weight of the emulsion splitter prepared by above-mentioned preparation method is utilized to can be: 1793 ~ 4287g/mol, specifically can be 3647g/mol, 1793g/mol, 4117g/mol or 1958g/mol.
Present invention also offers the application of initiator shown in a kind of formula I in the poly-flooding produced liquid process emulsion splitter of preparation.
Invention further provides poly-flooding produced liquid process emulsion splitter shown in a kind of formula III and gather the application in flooding produced liquid separating oil Tanaka.
Tool of the present invention has the following advantages:
The present invention take polytetrahydrofuran as raw material, under high-temperature and high-pressure conditions, obtains a kind of emulsion splitter being applicable to poly-flooding produced liquid process by butylene oxide ring, propylene oxide and epoxyethane ring-expansion polymerization.The emulsion splitter that the present invention obtains, gathers to oil field the crude oil emulsion driving rear generation and has good demulsification.
Accompanying drawing explanation
Fig. 1 is the schematic diagram of poly-flooding produced liquid after different concns emulsion splitter process prepared by the present invention.
Embodiment
The experimental technique used in following embodiment if no special instructions, is ordinary method.
Material used in following embodiment, reagent etc., if no special instructions, all can obtain from commercial channels.
The preparation of embodiment 1, initiator F-39/40
By the 10g polymerization degree be 12 polytetrahydrofuran and 2.10g potassium hydroxide join high-temperature high-pressure reaction kettle, airtight good reactor.First replace with nitrogen purging before intensification, vacuumize again, twice repeatedly, then start and stir and heat up, heating is stopped when temperature rises to 120 DEG C, open feed valve, drip butylene oxide ring 390g, control temperature of reaction is 120 ~ 140 DEG C (in reaction process, temperature is fluctuation) and initial pressure is 0.4MPa; ; Fall after rise until the complete pressure of material reaction and drip propylene oxide 400g again to 0MPa, control temperature of reaction is 120 ~ 140 DEG C (in reaction process, temperature is fluctuation) and initial pressure is 0.4MPa, treat that material reaction is complete, pressure falls after rise and react 30min again to 0MPa, finally cooling is opened still discharging and is obtained initiator shown in formula I, is labeled as F-39/40.
In the present embodiment, the add-on of potassium hydroxide is 0.26% of polytetrahydrofuran, butylene oxide ring and propylene oxide total mass, and the mass ratio of polytetrahydrofuran, butylene oxide ring and propylene oxide is 1:39:40,
In the initiator F-39/40 of this enforcement preparation, the value of x/y is 39/40.
The preparation of embodiment 2, initiator F-19/20
By the 10g polymerization degree be 12 polytetrahydrofuran and 2.10g potassium hydroxide join high-temperature high-pressure reaction kettle, airtight good reactor.First replace with nitrogen purging before intensification, vacuumize again, twice repeatedly, then start and stir and heat up, heating is stopped when temperature rises to 120 DEG C, open feed valve, drip butylene oxide ring 190g, control temperature of reaction is 120 ~ 140 DEG C (in reaction process, temperature is fluctuation) and initial pressure is 0.4MPa; ; Fall after rise until the complete pressure of material reaction and drip propylene oxide 200g again to 0MPa, control temperature of reaction is 120 ~ 140 DEG C (in reaction process, temperature is fluctuation) and initial pressure is 0.4MPa, treat that material reaction is complete, pressure falls after rise and react 30min again to 0MPa, finally cooling is opened still discharging and is obtained initiator shown in formula I, is labeled as F-19/20.
In the present embodiment, the add-on of potassium hydroxide is 0.52% of polytetrahydrofuran, butylene oxide ring and propylene oxide total mass, and the mass ratio of polytetrahydrofuran, butylene oxide ring and propylene oxide is 1:19:20.
In the initiator F-19/20 of this enforcement preparation, the value of x/y is 19/20.
The preparation of embodiment 3, initiator F-19/40 and F-39/20
Adopt the method for embodiment 1, but the amount of butylene oxide ring changes to 190g respectively obtains initiator shown in formula I, be labeled as F-19/40; Adopt the method for embodiment 2, but the amount of butylene oxide ring changes to 390g respectively obtains initiator shown in formula I, be labeled as F-39/20.
In the present embodiment, the add-on of potassium hydroxide is 0.35% of polytetrahydrofuran, butylene oxide ring and propylene oxide total mass, and the mass ratio of polytetrahydrofuran, butylene oxide ring and propylene oxide is respectively 1:19:40 and 1:39:20.
In the initiator F-19/40 of this enforcement preparation, the value of x/y is 19/40.In the initiator F-39/20 of this enforcement preparation, x/y is 39/20.
Embodiment 4, be applicable to the preparation of poly-flooding produced liquid process emulsion splitter F-19/20-1/2/7
40gF-19/20 initiator and 1.20g potassium hydroxide are joined high-temperature high-pressure reaction kettle, airtight good reactor.First replace with nitrogen purging before intensification, use vacuum pump evacuation again, twice repeatedly, then start and stir and heat up, heating is stopped when temperature rises to 120 DEG C, open feed valve, drip oxyethane 80g, control temperature of reaction is 120 ~ 130 DEG C (in reaction process, temperature is fluctuation) and initial pressure is 0.4MPa; Treat that material reaction is complete, pressure falls after rise and add 280g propylene oxide again to 0MPa, control temperature of reaction is 120 ~ 140 DEG C (in reaction process, temperature is fluctuation) and initial pressure is 0.4MPa, treat that material reaction is complete, pressure falls after rise and react 30min again to 0MPa, and finally cooling is opened still discharging and obtained a kind of poly-flooding produced liquid process emulsion splitter, is labeled as F-19/20-1/2/7.
In the present embodiment, the add-on of potassium hydroxide is 0.3% of initiator, oxyethane and propylene oxide total mass.
In emulsion splitter F-19/20-1/2/7 prepared by the present embodiment, a:b:c is 1:2:7.
Embodiment 5, be applicable to the preparation of poly-flooding produced liquid process emulsion splitter F-19/40-1/2/7, F-39/20-1/2/7 and F-39/40-1/2/7
Adopt the method for embodiment 4, but F-19/20 initiator is changed to F-19/40, F-39/20 and F-39/40 respectively, obtain poly-flooding produced liquid process rapid demulsifier, be labeled as F-19/40-1/2/7, F-39/20-1/2/7 and F-39/40-1/2/7 respectively.
In the present embodiment, the add-on of potassium hydroxide is 0.3% of initiator, oxyethane and propylene oxide total mass.
In emulsion splitter F-19/40-1/2/7, F-39/20-1/2/7 and F-39/40-1/2/7 prepared by the present embodiment, a:b:c is 1:2:7.
Embodiment 6, be applicable to poly-flooding produced liquid process emulsion splitter F-19/20-2/1/2, the preparation of F-19/20-1/3/6 and F-19/20-8/7/8
Adopt the method for embodiment 4, but the quality of oxyethane and propylene oxide is become 20g and 40g, 120g and 240g and 35g and 40g respectively, obtain being that the block polyether of initiator gathers flooding produced liquid process emulsion splitter with polytetrahydrofuran, be labeled as F-19/20-2/1/2, F-19/20-1/3/6 and F-19/20-8/7/8.
In the embodiment of above-mentioned preparation F-19/20-2/1/2, the add-on of potassium hydroxide is respectively 1.2% of initiator, oxyethane and propylene oxide total mass;
In the embodiment of above-mentioned preparation F-19/20-1/3/6, the add-on of potassium hydroxide is respectively 0.3% of initiator, oxyethane and propylene oxide total mass;
In the embodiment of above-mentioned preparation F-19/20-8/7/8, the add-on of potassium hydroxide is respectively 1.04% of initiator, oxyethane and propylene oxide total mass;
Emulsion splitter F-19/20-2/1/2 prepared by the present embodiment, in F-19/20-1/3/6 and F-19/20-8/7/8, a:b:c is respectively 2:1:2,1:3:6 and 8:7:8.
The molecular weight of F-19/20-abc series emulsion splitter is in table 1.
The molecular weight of table 1F-19/20-abc series emulsion splitter
| Sample | F-19/20-1/2/7 | F-19/20-2/1/2 | F-19/20-1/3/6 | F-19/20-8/7/8 |
| Molecular weight (g/mol) | 3647 | 1793 | 4117 | 1958 |
The performance study of embodiment 7, poly-flooding produced liquid process emulsion splitter
Rear Produced Liquid (water content is for 65%) is driven for handling object so that certain oil field is poly-, emulsion splitter consumption is 100mg/L, get 80mL and load dehydration bottle, when temperature is 65 DEG C, evaluation time is 60min, record is the dehydration rate in the same time cumulative volume of the front emulsified water of lower layer of water volume/experiment and free-water (at the end of the dehydration rate=experiment in bottle) not, and the effect of breakdown of emulsion prepared by the present invention as shown in Table 2 and Figure 1.
From table 2 and Fig. 1, part F-xy-a/b/c emulsion splitter (No. 2, No. 5, No. 6 and No. 7 emulsion splitters) dehydration when 60min is all greater than 85%, has good demulsification.
The performance evaluation (in Produced Liquid moisture 65%, 1h time dehydration rate) of table 2F-xy-a/b/c series emulsion splitter
| Sample | Blank | F-19/20-1/2/7 | F-19/20-2/1/2 | F-19/20-1/3/6 | F-19/20-8/7/8 | F-39/40-1/2/7 |
| Numbering | 1 | 2 | 3 | 4 | 5 | 6 |
| Dehydration rate (%) | 3.0 | 86.6 | 68.3 | 81.6 | 86.6 | 85.0 |
| Sample | F-39/40-2/1/2 | F-39/40-1/3/6 | F-39/40-8/7/8 | |||
| Numbering | 7 | 8 | 9 |
| Dehydration rate (%) | 86.9 | 84.6 | 83.5 |
Should be understood that, for those of ordinary skills, can be improved according to the above description or convert, and all these improve and convert the protection domain that all should belong to claims of the present invention.
Claims (10)
1. initiator shown in formula I,
In formula I, the value of x/y is 19 ~ 39:20 ~ 40.
2. a preparation method for initiator shown in formula I described in claim 1, comprises the steps:
(1) under anaerobic and catalyzer existent condition, polytetrahydrofuran and butylene oxide ring carry out polyreaction;
Described catalyzer is any one in potassium hydroxide, sodium hydroxide, hydrated barta and lime acetate;
The polymerization degree of described polytetrahydrofuran is 12;
(2) in step (1) reaction system after completion of the reaction, add propylene oxide, again carry out polyreaction, obtain described initiator.
3. preparation method according to claim 2, is characterized in that: step (1) and step (2), and the temperature of described polyreaction is not all higher than 140 DEG C, and pressure is not all higher than 0.4MPa.
4. the preparation method according to Claims 2 or 3, is characterized in that: the amount of the described catalyzer added in step (1) is 0.2% ~ 0.6% of the total mass of the described propylene oxide added in the described polytetrahydrofuran and described butylene oxide ring and step (2) added in step (1);
Described in polytetrahydrofuran described in step (1), described butylene oxide ring and step (2), the mass ratio of propylene oxide is 1:19 ~ 39:20 ~ 40.
5. poly-flooding produced liquid process emulsion splitter shown in formula II,
In formula II, initiator shown in F-xy expression I, a:b:c is 1 ~ 8:1 ~ 7:2 ~ 8;
In formula I, the value of x/y is 19 ~ 39:20 ~ 40.
6. the preparation method of poly-flooding produced liquid process emulsion splitter shown in formula II described in claim 5, comprises the steps:
(1) under anaerobic and catalyzer existent condition, initiator shown in formula I and oxyethane carry out polyreaction;
Described catalyzer is any one in potassium hydroxide, sodium hydroxide, hydrated barta and lime acetate;
In formula I, the value of x/y is 19 ~ 39:20 ~ 40;
(2) in step (1) reaction system after completion of the reaction, add propylene oxide, again carry out polyreaction, obtain described poly-flooding produced liquid process emulsion splitter.
7. preparation method according to claim 6, is characterized in that: in step (1), and the temperature of described polyreaction is not higher than 130 DEG C, and pressure is not higher than 0.4MPa;
In step (2), the temperature of described polyreaction is not higher than 140 DEG C, and pressure is not higher than 0.4MPa.
8. the preparation method according to claim 6 or 7, is characterized in that: the amount of the described catalyzer added in step (1) for add in initiator shown in the formula I that adds in step (1) and described oxyethane and step (2) 0.2% ~ 1.2% of the total mass of described propylene oxide;
The mass ratio added of initiator shown in formula I, described oxyethane and described propylene oxide is 1 ~ 8:1 ~ 7:2 ~ 8.
9. the application of initiator shown in formula I described in claim 1 in the poly-flooding produced liquid process emulsion splitter of preparation.
10. described in claim 5, shown in formula II, poly-flooding produced liquid process emulsion splitter gathers the application in flooding produced liquid separating oil Tanaka.
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| CN104828903A (en) * | 2015-04-20 | 2015-08-12 | 南京工业大学 | Preparation method for novel composite demulsifying degresaer |
| CN104945612A (en) * | 2015-07-21 | 2015-09-30 | 克拉玛依市天明化工有限责任公司 | Efficient emulsion breaker containing polymer for processing crude oil and preparation method thereof |
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| US4537701A (en) * | 1977-05-04 | 1985-08-27 | Basf Aktiengesellschaft | Demulsifiers for breaking crude-oil emulsions and their use |
| US6423107B1 (en) * | 1999-08-12 | 2002-07-23 | Institut Francais Du Petrole | Detergent compositions for gasoline-type fuels that contain polytetrahydrofuran derivatives |
| CN103193971A (en) * | 2013-04-16 | 2013-07-10 | 西南石油大学 | Polypropylene oxide oil head and block polyether demulsifier using dihydro tallow secondary amine as initiator, and preparation method of same |
| CN103620005A (en) * | 2011-06-21 | 2014-03-05 | 陶氏环球技术有限责任公司 | Energy efficient polyalkylene glycols and lubricant composition containing same |
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Patent Citations (5)
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| GB941496A (en) * | 1960-07-07 | 1963-11-13 | Bayer Ag | Hydraulic fluids |
| US4537701A (en) * | 1977-05-04 | 1985-08-27 | Basf Aktiengesellschaft | Demulsifiers for breaking crude-oil emulsions and their use |
| US6423107B1 (en) * | 1999-08-12 | 2002-07-23 | Institut Francais Du Petrole | Detergent compositions for gasoline-type fuels that contain polytetrahydrofuran derivatives |
| CN103620005A (en) * | 2011-06-21 | 2014-03-05 | 陶氏环球技术有限责任公司 | Energy efficient polyalkylene glycols and lubricant composition containing same |
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Address after: 100010 Beijing, Chaoyangmen, North Street, No. 25, No. Co-patentee after: CNOOC research institute limited liability company Patentee after: China Offshore Oil Group Co., Ltd. Co-patentee after: Southwest Petroleum University Address before: 100010 Beijing, Chaoyangmen, North Street, No. 25, No. Co-patentee before: CNOOC Research Institute Patentee before: China National Offshore Oil Corporation Co-patentee before: Southwest Petroleum University |
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Effective date of registration: 20191211 Address after: 100010 Beijing, Chaoyangmen, North Street, No. 25, No. Co-patentee after: CNOOC research institute limited liability company Patentee after: China Offshore Oil Group Co., Ltd. Address before: 100010 Beijing, Chaoyangmen, North Street, No. 25, No. Co-patentee before: CNOOC research institute limited liability company Patentee before: China Offshore Oil Group Co., Ltd. Co-patentee before: Southwest Petroleum University |