CN103193971A - Polypropylene oxide oil head and block polyether demulsifier using dihydro tallow secondary amine as initiator, and preparation method of same - Google Patents
Polypropylene oxide oil head and block polyether demulsifier using dihydro tallow secondary amine as initiator, and preparation method of same Download PDFInfo
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- CN103193971A CN103193971A CN2013101318411A CN201310131841A CN103193971A CN 103193971 A CN103193971 A CN 103193971A CN 2013101318411 A CN2013101318411 A CN 2013101318411A CN 201310131841 A CN201310131841 A CN 201310131841A CN 103193971 A CN103193971 A CN 103193971A
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- propylene oxide
- secondary amine
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- dihydro tallow
- tallow secondary
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- 125000000467 secondary amino group Chemical class [H]N([*:1])[*:2] 0.000 title claims abstract description 64
- 239000003760 tallow Substances 0.000 title claims abstract description 64
- 239000003999 initiator Substances 0.000 title claims abstract description 52
- 239000004721 Polyphenylene oxide Substances 0.000 title claims abstract description 36
- 229920000570 polyether Polymers 0.000 title claims abstract description 36
- 239000003921 oil Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 229920001451 polypropylene glycol Polymers 0.000 title claims abstract description 25
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 claims abstract description 51
- -1 poly(propylene oxide) Polymers 0.000 claims abstract description 49
- 239000000839 emulsion Substances 0.000 claims abstract description 34
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims description 40
- 239000003795 chemical substances by application Substances 0.000 claims description 26
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 24
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical group [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 24
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims description 12
- 238000010926 purge Methods 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 8
- 238000007599 discharging Methods 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 6
- VSGNNIFQASZAOI-UHFFFAOYSA-L calcium acetate Chemical compound [Ca+2].CC([O-])=O.CC([O-])=O VSGNNIFQASZAOI-UHFFFAOYSA-L 0.000 claims description 5
- 239000003054 catalyst Substances 0.000 claims description 4
- 238000006073 displacement reaction Methods 0.000 claims description 4
- 238000010792 warming Methods 0.000 claims description 4
- 229920000642 polymer Polymers 0.000 abstract description 2
- 238000007151 ring opening polymerisation reaction Methods 0.000 abstract 1
- 238000000605 extraction Methods 0.000 description 9
- 239000007788 liquid Substances 0.000 description 9
- 239000000463 material Substances 0.000 description 7
- 230000018044 dehydration Effects 0.000 description 6
- 238000006297 dehydration reaction Methods 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 4
- 230000000630 rising effect Effects 0.000 description 4
- 239000010779 crude oil Substances 0.000 description 3
- 238000011156 evaluation Methods 0.000 description 3
- 238000012545 processing Methods 0.000 description 2
- 239000002569 water oil cream Substances 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000006049 ring expansion reaction Methods 0.000 description 1
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- Polyethers (AREA)
Abstract
本发明公开了一种嵌段聚醚破乳剂的制备技术领域的以二氢化牛油基仲胺为起始剂的聚环氧丙烷油头及嵌段聚醚破乳剂及其制备方法，本发明以二氢化牛油基仲胺为起始剂，在高温高压条件下，通过环氧丙烷和环氧乙烷开环聚合得到一种以二氢化牛油基仲胺为起始剂的环氧乙烷和环氧丙烷嵌段聚醚破乳剂。该发明的破乳剂，针对油田聚驱后产生的O/W型乳液具有良好的破乳效果。The invention discloses a poly(propylene oxide) oil head and block polyether demulsifier in the technical field of preparation of a block polyether demulsifier using dihydrogenated tallow-based secondary amine as an initiator and a preparation method thereof. With dihydrogenated tallow-based secondary amine as the initiator, under high temperature and high pressure conditions, a kind of ethylene oxide with dihydrogenated tallow-based secondary amine as the initiator is obtained by ring-opening polymerization of propylene oxide and ethylene oxide Alkane and propylene oxide block polyether demulsifier. The demulsifier of the invention has a good demulsification effect on the O/W emulsion produced after polymer flooding in oilfields.
Description
Technical field
The present invention relates to a kind of preparation of block polyether emulsion splitter, particularly a kind of is poly(propylene oxide) oil head and oxyethane and propylene oxide block polyether demulsification agent and preparation method thereof of initiator with dihydro tallow secondary amine.
Background technology
At present, the numerous domestic oil field has entered the poly-stage of comprehensive notes, and there is big nature difference in polymer flooding extraction liquid phase to water drive extraction liquid: (1) oil-water emulsion degree height, and water-oil emulsion stability is strong; (2) along with the growth of extraction liquid water ratio, significant variation has also taken place in the emulsion type of extraction liquid, and emulsion type changes oil-in-water-type (O/W) and water-in-oil-in-water type (W/O/W) multiple emulsion into by the water-in-oil-type (W/O) of early field life.These characteristics have brought many difficulties for the processing of extraction liquid, as: the processing of the poly-output liquid of the inapplicable notes of original emulsion splitter, cause its consumption to enlarge markedly; Dehydration back crude oil water content exceed standard with separate recovered water in oleaginousness increase substantially.So far, the emulsion splitter that use in each oil field mainly proposes at w/o type crude oil emulsion after the water drive, drives work that O/W type crude oil emulsion breakdown of emulsion that the back produces carries out with emulsion splitter also seldom at poly-.Therefore, drive O/W type extraction liquid that the back produces and have very important significance with the research of emulsion splitter about poly-.
Summary of the invention
The purpose of this invention is to provide with dihydro tallow secondary amine is poly(propylene oxide) oil head and oxyethane and propylene oxide block polyether demulsification agent and preparation method thereof of initiator.
Provided by the invention a kind of be the poly(propylene oxide) oil head (DHCA-x) of initiator with dihydro tallow secondary amine, its structural formula is shown in formula I:
R=C wherein
16-C
18, the mass ratio of x representative ring Ethylene Oxide and dihydro tallow secondary amine, x=34,40,45,51 or 57.
The invention provides shown in the above-mentioned formula I with dihydro tallow secondary amine is the preparation method of the poly(propylene oxide) oil head of initiator, it may further comprise the steps: dihydro tallow secondary amine and catalyzer are joined high-temperature high-pressure reaction kettle, airtight good reactor, before intensification, replace with nitrogen purging earlier, vacuumize then, the operation that elder generation's nitrogen purging displacement vacuumizes again repeatedly at least twice, start then and stir and be warming up to temperature of reaction, add propylene oxide again, react under the High Temperature High Pressure to the still internal pressure be 0 MPa, it is the poly(propylene oxide) oil head of initiator that cooling at last opens that the still discharging obtains with dihydro tallow secondary amine;
Among the above-mentioned preparation method, described reaction pressure should be controlled at 0-0.4MPa; Described temperature of reaction is 120-150 ℃, preferred 130 ℃.
Among the above-mentioned preparation method, the mass ratio of propylene oxide and dihydro tallow secondary amine specifically can be 34,40,45,51 or 57.
Among the above-mentioned preparation method, described catalyzer is potassium hydroxide, sodium hydroxide, hydrated barta or lime acetate.
Among the above-mentioned preparation method, catalyst levels is the 0.2%-0.6% of reaction raw materials (dihydro tallow secondary amine and propylene oxide) quality sum, preferred 0.3%.
The invention provides a kind of is oxyethane and the propylene oxide block polyether demulsification agent (DHCA-x-mnp) of initiator with dihydro tallow secondary amine, and its structural formula is shown in formula II:
Wherein, m, it is the quality of poly(propylene oxide) oil head, ethylene oxide block and the propylene oxide block of initiator that n and p represent respectively in the emulsion splitter with dihydro tallow secondary amine, it is the mass ratio of poly(propylene oxide) oil head, ethylene oxide block and the propylene oxide block of initiator that m:n:p represents in the emulsion splitter with dihydro tallow secondary amine, R=C
16-C
18, the mass ratio of x representative ring Ethylene Oxide and dihydro tallow secondary amine, x=34,40,45,51 or 57.
Of the present invention is in the oxyethane and propylene oxide block polyether demulsification agent of initiator with dihydro tallow secondary amine, is that the mass ratio of poly(propylene oxide) oil head, ethylene oxide block and the propylene oxide block of initiator specifically can be 1:6:3,1:6:6,1:6:9 or 1:6:12 with dihydro tallow secondary amine.
Above-mentioned is oxyethane and the propylene oxide block polyether demulsification agent of initiator with dihydro tallow secondary amine, and its molecular weight is 1107-3155g/mol.
Above-mentioned is oxyethane and the propylene oxide block polyether demulsification agent of initiator with dihydro tallow secondary amine, and its cloud point is 24.2-32.3 ℃.
The invention provides shown in the above-mentioned formula II with dihydro tallow secondary amine is the preparation method of oxyethane and the propylene oxide block polyether demulsification agent of initiator, it may further comprise the steps: adding with dihydro tallow secondary amine in the high-temperature high-pressure reaction kettle is poly(propylene oxide) oil head and the catalyzer of initiator, airtight good reactor, before intensification, replace with nitrogen purging earlier, vacuumize then, the operation that elder generation's nitrogen purging displacement vacuumizes again repeatedly at least twice, start then and stir and be warming up to temperature of reaction, add oxyethane again, react under the High Temperature High Pressure to the still internal pressure be 0MPa; Add propylene oxide afterwards again, react under the High Temperature High Pressure to the still internal pressure be 0MPa, i.e. reaction finishes, the still discharging is opened in cooling at last, obtaining with dihydro tallow secondary amine is oxyethane and the propylene oxide block polyether demulsification agent of initiator;
Among the above-mentioned block polyether emulsion splitter preparation method, pressure should be controlled at 0-0.4MPa in the reaction process, and temperature should be controlled at 120-150 ℃ in the reaction process, preferred 130 ℃.
Among the above-mentioned block polyether emulsion splitter preparation method, adding be that the mass ratio of poly(propylene oxide) oil head, oxyethane and the propylene oxide of initiator specifically can be 1:6:3,1:6:6,1:6:9 or 1:6:12 with dihydro tallow secondary amine.
Among the above-mentioned block polyether emulsion splitter preparation method, described catalyzer is selected from potassium hydroxide, sodium hydroxide, hydrated barta or lime acetate.
Among the above-mentioned block polyether emulsion splitter preparation method, catalyst levels is the 0.2%-0.6% of reaction raw materials (be poly(propylene oxide) oil head, oxyethane and the propylene oxide of initiator with dihydro tallow secondary amine) quality sum, preferred 0.3%.
The present invention is initiator with dihydro tallow secondary amine, and under high-temperature and high-pressure conditions, obtaining a kind of by propylene oxide and epoxyethane ring-expansion polymerization is oxyethane and the propylene oxide block polyether demulsification agent of initiator with dihydro tallow secondary amine.The emulsion splitter of this invention has good demulsification at the poly-O/W type emulsion of driving the back generation in oil field.
Embodiment
The following examples can make those skilled in the art more fully understand the present invention, but do not limit the present invention in any way.
Employed experimental technique is ordinary method if no special instructions among the following embodiment.
Used material, reagent etc. if no special instructions, all can obtain from commercial channels among the following embodiment.
Embodiment 1, dihydro tallow secondary amine are the preparation of the poly(propylene oxide) oil head of initiator
10g dihydro tallow secondary amine and 1.38g potassium hydroxide are joined high-temperature high-pressure reaction kettle, airtight good reactor.Before intensification, replace with nitrogen purging earlier, vacuumize with vacuum pump then, twice repeatedly, start then and stir and intensification, when rising to 120 ℃, temperature stops heating, open feed valve, drip propylene oxide 450g, the control temperature of reaction is no more than 140 ℃ and pressure-controlling below 0.4MPa, treat that material reaction finishes, pressure reacts 30min after falling after rise again, makes pressure be down to 0MPa, cooling is at last opened the still discharging and is obtained the poly(propylene oxide) oil head that dihydro tallow secondary amine is initiator, is labeled as DHCA-45.
Embodiment 2, dihydro tallow secondary amine are the preparation of the poly(propylene oxide) oil head of initiator
10g dihydro tallow secondary amine and 1.16g potassium hydroxide are joined high-temperature high-pressure reaction kettle, airtight good reactor.Before intensification, replace with nitrogen purging earlier, vacuumize with vacuum pump then, twice repeatedly, start then and stir and intensification, when rising to 120 ℃, temperature stops heating, open feed valve, drip propylene oxide 570g, the control temperature of reaction is no more than 140 ℃ and pressure-controlling below 0.4MPa, treat that material reaction finishes, pressure reacts 30min after falling after rise again, makes pressure be down to 0MPa, cooling is at last opened the still discharging and is obtained the poly(propylene oxide) oil head that dihydro tallow secondary amine is initiator, is labeled as DHCA-57.
Embodiment 3
Adopt the method for embodiment 1, but the amount of propylene oxide changes to 340g, 400g, 510g respectively, what obtain is that the poly(propylene oxide) oil head of initiator is labeled as DHCA-34, DHCA-40, DHCA-51 respectively with dihydro tallow secondary amine.
Embodiment 4, be the preparation of oxyethane and the propylene oxide block polyether demulsification agent of initiator with dihydro tallow secondary amine
40gDHCA-45 oil head and 2.08g potassium hydroxide are joined high-temperature high-pressure reaction kettle, airtight good reactor.Before intensification, replace with nitrogen purging earlier, vacuumize with vacuum pump then, repeatedly twice, start then and stir and heat up, when rising to 120 ℃, temperature stops heating, open feed valve, drip oxyethane 240g, the control temperature of reaction is no more than 140 ℃ and pressure-controlling below 0.4MPa, treats that material reaction finishes, pressure reacts 30min after falling after rise again, makes pressure be down to 0MPa; Then, be heated to 130 ℃ and add the 240g propylene oxide again, the control temperature of reaction is no more than 150 ℃ and pressure-controlling below 0.4MPa, treat that material reaction finishes, pressure reacts 30min after falling after rise again, make pressure be down to 0MPa, it is oxyethane and the propylene oxide block polyether demulsification agent of initiator that cooling at last opens that the still discharging obtains with dihydro tallow secondary amine, is labeled as DHCA-45-166.
Embodiment 5,
Adopt the method for embodiment 4, but the DHCA-45 oil head is changed to DHCA-34, DHCA-40, DHCA-51 and DHCA-57 respectively, what obtain is oxyethane and the propylene oxide block polyether demulsification agent of initiator with dihydro tallow secondary amine, is labeled as DHCA-34-166, DHCA-40-166, DHCA-51-166 and DHCA-57-166 respectively.
The molecular weight of DHCA-x-166 series emulsion splitter and cloud point see Table 1 and table 2 respectively.
The molecular weight of table 1DHCA-x-166 series emulsion splitter
| Sample | DHCA-34-166 | DHCA-40-166 | DHCA-45-166 | DHCA-51-166 | DHCA-57-166 |
| Molecular weight (g/mol) | 2091 | 3084 | 2784 | 3134 | 3073 |
The cloud point of table 2DHCA-x-166 series emulsion splitter
| Sample | DHCA-34-166 | DHCA-40-166 | DHCA-45-166 | DHCA-51-166 | DHCA-57-166 |
| Cloud point (℃) | 28.9 | 32.3 | 29.0 | 29.0 | 32.0 |
Embodiment 6, be the preparation of oxyethane and the propylene oxide block polyether demulsification agent of initiator with dihydro tallow secondary amine
40gDHCA-45 oil head and 2.40g potassium hydroxide are joined high-temperature high-pressure reaction kettle, airtight good reactor.Before intensification, replace with nitrogen purging earlier, vacuumize with vacuum pump then, repeatedly twice, start then and stir and heat up, when rising to 120 ℃, temperature stops heating, open feed valve, drip oxyethane 240g, the control temperature of reaction is no more than 140 ℃ and pressure-controlling below 0.4MPa, and material reaction to be treated finishes, pressure reacts 30min after falling after rise again, makes pressure be down to 0MPa; Then, be heated to 130 ℃ and add the 360g propylene oxide again, the control temperature of reaction is no more than 150 ℃ and pressure-controlling below 0.4MPa, treat that material reaction finishes, pressure reacts 30min after falling after rise again, make pressure be down to 0MPa, it is oxyethane and the propylene oxide block polyether demulsification agent of initiator that cooling at last opens that the still discharging obtains with dihydro tallow secondary amine, is labeled as DHCA-45-169.
Embodiment 7,
Adopt the method for embodiment 6, but the DHCA-45 oil head is changed to DHCA-34, DHCA-40, DHCA-51 and DHCA-57 respectively, catalyzer changes to lime acetate, consumption changes to 3.84g, what obtain is oxyethane and the propylene oxide block polyether demulsification agent of initiator with dihydro tallow secondary amine, is labeled as DHCA-34-169, DHCA-40-169, DHCA-51-169 and DHCA-57-169 respectively.
The molecular weight of DHCA-x-169 series emulsion splitter and cloud point see Table 3 and table 4 respectively.
The molecular weight of table 3DHCA-x-169 series emulsion splitter
| Sample | DHCA-34-169 | DHCA-40-169 | DHCA-45-169 | DHCA-51-169 | DHCA-57-169 |
| Molecular weight (g/mol) | 1624 | 1691 | 2817 | 2137 | 3155 |
The cloud point of table 4DHCA-x-169 series emulsion splitter
| Sample | DHCA-34-169 | DHCA-40-169 | DHCA-45-169 | DHCA-51-169 | DHCA-57-169 |
| Cloud point (℃) | 27.5 | 28.0 | 23.8 | 24.4 | 26.3 |
Embodiment 8, be the oxyethane of initiator and the performance study of propylene oxide block polyether demulsification agent with dihydro tallow secondary amine
Serve as to handle object with the poly-back extraction liquid that drives in certain oil field, the emulsion splitter consumption is 200mg/L, and when temperature was 65 ℃, the dehydration rate when dihydro tallow secondary amine is the oxyethane of initiator and propylene oxide block polyether demulsification agent 1h saw Table 5 and table 6.
In the performance evaluation 1(extraction liquid of table 5DHCA series emulsion splitter moisture 65%)
| Sample | DHCA-34-166 | DHCA-40-166 | DHCA-45-166 | DHCA-51-166 | DHCA-57-166 |
| Numbering | 1 | 2 | 3 | 4 | 5 |
| Dehydration rate (%) | 85.0 | 86.6 | 78.3 | 81.6 | 81.6 |
| Sample | DHCA-34-169 | DHCA-40-169 | DHCA-45-169 | DHCA-51-169 | DHCA-59-169 |
| Numbering | 6 | 7 | 8 | 9 | 10 |
| Dehydration rate (%) | 86.6 | 85.0 | 96.6 | 86.6 | 86.6 |
In the performance evaluation 2(extraction liquid of table 6DHCA series emulsion splitter moisture 75%)
| Sample | DHCA-34-166 | DHCA-40-166 | DHCA-45-166 | DHCA-51-166 | DHCA-57-166 |
| Numbering | 1 | 2 | 3 | 4 | 5 |
| Dehydration rate (%) | 85.2 | 81.7 | 95.5 | 73.1 | 95.5 |
| Sample | DHCA-34-169 | DHCA-40-169 | DHCA-45-169 | DHCA-51-169 | DHCA-57-169 |
| Numbering | 6 | 7 | 8 | 9 | 10 |
| Dehydration rate (%) | 98.9 | 98.9 | 92.6 | 98.9 | 95.5 |
Be the performance evaluation result of oxyethane and the propylene oxide block polyether demulsification agent of initiator with dihydro tallow secondary amine to sum up, can find that it has good demulsification for poly-O/W type emulsion of driving the back generation, can satisfy the basic demand of field produces.
The above; only for the preferable embodiment of the present invention, but protection scope of the present invention is not limited thereto, and anyly is familiar with those skilled in the art in the technical scope that the present invention discloses; the variation that can expect easily or replacement all should be encompassed within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain of claim.
Claims (10)
1. one kind is the poly(propylene oxide) oil head of initiator with dihydro tallow secondary amine, and it is characterized in that: its structural formula is shown in formula I:
R=C wherein
16-C
18, the mass ratio of x representative ring Ethylene Oxide and dihydro tallow secondary amine, x=34,40,45,51 or 57.
2. claim 1 is described is the preparation method of the poly(propylene oxide) oil head of initiator with dihydro tallow secondary amine, it is characterized in that may further comprise the steps: dihydro tallow secondary amine and catalyzer are joined high-temperature high-pressure reaction kettle, airtight good reactor, before intensification, replace with nitrogen purging earlier, vacuumize then, the operation that elder generation's nitrogen purging displacement vacuumizes again repeatedly at least twice, start then and stir and be warming up to temperature of reaction, add propylene oxide again, react under the High Temperature High Pressure to the still internal pressure be 0MPa, it is the poly(propylene oxide) oil head of initiator that cooling at last opens that the still discharging obtains with dihydro tallow secondary amine;
Wherein, described reaction pressure should be controlled at 0-0.4MPa; Described temperature of reaction is 120-150 ℃.
3. method according to claim 2, it is characterized in that: the mass ratio of propylene oxide and dihydro tallow secondary amine is specially 34,40,45,51 or 57.
4. method according to claim 2, it is characterized in that: described catalyzer is potassium hydroxide, sodium hydroxide, hydrated barta or lime acetate, described catalyst levels is the 0.2%-0.6% of reaction raw materials quality sum, preferred 0.3%, described reaction raw materials refers to dihydro tallow secondary amine and propylene oxide.
5. one kind is oxyethane and the propylene oxide block polyether demulsification agent of initiator with dihydro tallow secondary amine, and its structural formula is shown in formula II:
Wherein, m, n and p represent the quality of oil head in the emulsion splitter, ethylene oxide block and propylene oxide block, R=C respectively
16-C
18, the mass ratio of x representative ring Ethylene Oxide and dihydro tallow secondary amine, x=34,40,45,51 or 57.
6. according to claim 5 is oxyethane and the propylene oxide block polyether demulsification agent of initiator with dihydro tallow secondary amine, and it is characterized in that: the mass ratio of oil head, ethylene oxide block and propylene oxide block is specially 1:6:3,1:6:6,1:6:9 or 1:6:12.
7. according to claim 5 is oxyethane and the propylene oxide block polyether demulsification agent of initiator with dihydro tallow secondary amine, it is characterized in that: be oxyethane and the propylene oxide block polyether demulsification agent of initiator with dihydro tallow secondary amine, its molecular weight is 1107-3155g/mol, and cloud point is 24.2-32.3 ℃.
8. any one claim of claim 5 to 7 is described is the preparation method of oxyethane and the propylene oxide block polyether demulsification agent of initiator with dihydro tallow secondary amine, it is characterized in that may further comprise the steps: adding with dihydro tallow secondary amine in the high-temperature high-pressure reaction kettle is poly(propylene oxide) oil head and the catalyzer of initiator, airtight good reactor, before intensification, replace with nitrogen purging earlier, vacuumize then, the operation that elder generation's nitrogen purging displacement vacuumizes again repeatedly at least twice, start then and stir and be warming up to temperature of reaction, add oxyethane again, react under the High Temperature High Pressure to the still internal pressure be 0MPa; Add propylene oxide afterwards again, react under the High Temperature High Pressure to the still internal pressure be 0MPa, i.e. reaction finishes, the still discharging is opened in cooling at last, obtaining with dihydro tallow secondary amine is oxyethane and the propylene oxide block polyether demulsification agent of initiator;
Wherein, pressure should be controlled at 0-0.4MPa in the reaction process, and temperature should be controlled at 120-150 ℃ in the reaction process, preferred 130 ℃.
9. according to claim 8 is the preparation method of oxyethane and the propylene oxide block polyether demulsification agent of initiator with dihydro tallow secondary amine, it is characterized in that: in the emulsion splitter preparation process, adding be that the mass ratio of poly(propylene oxide) oil head, oxyethane and the propylene oxide of initiator is specially 1:6:3,1:6:6,1:6:9 or 1:6:12 with dihydro tallow secondary amine.
10. according to claim 8 is the preparation method of oxyethane and the propylene oxide block polyether demulsification agent of initiator with dihydro tallow secondary amine, it is characterized in that: described catalyzer is selected from potassium hydroxide, sodium hydroxide, hydrated barta or lime acetate, catalyst levels is the 0.2%-0.6% of reaction raw materials quality sum, preferred 0.3%, described reaction raw materials refers in the emulsion splitter preparation process, adding be poly(propylene oxide) oil head, oxyethane and the propylene oxide of initiator with dihydro tallow secondary amine.
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| CN103709390A (en) * | 2013-12-20 | 2014-04-09 | 西南石油大学 | Block polyether demulsifier using polymine as initiator and preparation method thereof |
| CN103755884A (en) * | 2013-12-20 | 2014-04-30 | 西南石油大学 | Reverse-phase demulsifying agent for treating polymer flooding produced liquid of oil fields and preparation method thereof |
| CN104004181A (en) * | 2014-05-23 | 2014-08-27 | 中国海洋石油总公司 | Demulsifying agent for treating polymer flooding produced liquid and preparation method of demulsifying agent |
| CN105368428A (en) * | 2014-08-27 | 2016-03-02 | 中国石油化工股份有限公司 | Cathode non-mixed type oil displacement surfactants and preparation method and application thereof |
| CN106317401A (en) * | 2016-08-19 | 2017-01-11 | 浙江皇马科技股份有限公司 | Synthetic method of low color value polyether |
| CN106590595A (en) * | 2015-10-20 | 2017-04-26 | 中国石油化工股份有限公司 | Oil displacement composition applicable to low calcium-magnesium oil reservoir and preparation method of oil displacement composition |
| CN107641523A (en) * | 2017-10-11 | 2018-01-30 | 中国海洋石油总公司 | A kind of fluorine-containing crosslinked polyethers demulsifier and preparation method |
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| CN103709390A (en) * | 2013-12-20 | 2014-04-09 | 西南石油大学 | Block polyether demulsifier using polymine as initiator and preparation method thereof |
| CN103755884A (en) * | 2013-12-20 | 2014-04-30 | 西南石油大学 | Reverse-phase demulsifying agent for treating polymer flooding produced liquid of oil fields and preparation method thereof |
| CN103755884B (en) * | 2013-12-20 | 2016-03-30 | 西南石油大学 | Flooding produced liquid reverse-phase emulsifier and preparation method thereof is gathered in a kind of process oil field |
| CN103709390B (en) * | 2013-12-20 | 2016-05-18 | 西南石油大学 | A kind of block polyether demulsifier taking polymine as initiator and preparation method thereof |
| CN104004181A (en) * | 2014-05-23 | 2014-08-27 | 中国海洋石油总公司 | Demulsifying agent for treating polymer flooding produced liquid and preparation method of demulsifying agent |
| CN104004181B (en) * | 2014-05-23 | 2016-02-17 | 中国海洋石油总公司 | A kind of poly-flooding produced liquid process emulsion splitter and preparation method thereof |
| CN105368428A (en) * | 2014-08-27 | 2016-03-02 | 中国石油化工股份有限公司 | Cathode non-mixed type oil displacement surfactants and preparation method and application thereof |
| CN105368428B (en) * | 2014-08-27 | 2019-12-10 | 中国石油化工股份有限公司 | Anionic-nonionic mixed oil-displacing surfactant and preparation method and application thereof |
| CN106590595A (en) * | 2015-10-20 | 2017-04-26 | 中国石油化工股份有限公司 | Oil displacement composition applicable to low calcium-magnesium oil reservoir and preparation method of oil displacement composition |
| CN106590595B (en) * | 2015-10-20 | 2020-02-07 | 中国石油化工股份有限公司 | Oil displacement composition suitable for low-calcium magnesium oil reservoir and preparation method thereof |
| CN106317401A (en) * | 2016-08-19 | 2017-01-11 | 浙江皇马科技股份有限公司 | Synthetic method of low color value polyether |
| CN107641523A (en) * | 2017-10-11 | 2018-01-30 | 中国海洋石油总公司 | A kind of fluorine-containing crosslinked polyethers demulsifier and preparation method |
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