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CN114768309A - Reverse demulsifier and preparation method thereof - Google Patents

Reverse demulsifier and preparation method thereof Download PDF

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Publication number
CN114768309A
CN114768309A CN202210512660.2A CN202210512660A CN114768309A CN 114768309 A CN114768309 A CN 114768309A CN 202210512660 A CN202210512660 A CN 202210512660A CN 114768309 A CN114768309 A CN 114768309A
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Prior art keywords
reverse demulsifier
reverse
preparation
demulsifier
catalyst
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付海明
傅小川
李兆军
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Guangdong Yueshou New Technology Co ltd
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Guangdong Yueshou New Technology Co ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D17/00Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
    • B01D17/02Separation of non-miscible liquids
    • B01D17/04Breaking emulsions
    • B01D17/047Breaking emulsions with separation aids

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  • Thermal Sciences (AREA)
  • Chemical & Material Sciences (AREA)
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Abstract

The invention relates to the technical field of reverse demulsifiers, in particular to a reverse demulsifier, which comprises the following raw materials: polyvinyl alcohol, 2, 3-epoxypropyltrimethylammonium chloride, methyl acrylate, a polyamine compound, epichlorohydrin, an initiator and a catalyst; a reverse demulsifier and a preparation method thereof comprise the following steps: s1: adding polyvinyl alcohol and 2, 3-epoxypropyl trimethyl ammonium chloride into a reaction tank, and reacting under the conditions of a catalyst and an initiator to obtain cation modified polyvinyl alcohol; s2: and (3) putting the methyl acrylate and the polyamine compound into a reaction tank to react to obtain the linear polyamide. The invention has the beneficial effects that: the reverse demulsifier has the characteristics of both a polyacrylate reverse demulsifier and a cationic reverse demulsifier, avoids the use limitation of the two demulsifiers, and avoids the problems of generation of viscous oil sludge, serious wall-sticking eye and incapability of wide application, so that the reverse demulsifier has good demulsification effect and wider application range.

Description

Reverse demulsifier and preparation method thereof
Technical Field
The invention relates to the technical field of reverse demulsifiers, in particular to a reverse demulsifier and a preparation method thereof.
Background
With the oil field entering the middle and later oil extraction stages, the water content of the produced liquid is higher and higher, and the comprehensive water content of the oil field developed at present exceeds 85 percent in a certain oil field in Bohai sea area. A large amount of production fluid exists as an oil-in-water (O/W) emulsion. Therefore, the reverse demulsifier is particularly important for treating oil field produced liquid. In the process of treating produced liquid, the reverse demulsifier is a kind of medicament which is added in a three-phase separator to promote separation of O/W emulsion.
Chinese patent No. CN108579132A provides a high-efficiency reverse demulsifier and a preparation method thereof, which comprises the following raw materials: aldehyde compounds, amine compounds, urea compounds, polymerization inhibitors and aldehyde removers; it is also proposed to comprise the following steps: s1, adding an aldehyde compound into the reaction kettle, and adding an amine compound and a urea compound under the stirring condition; s2, adding a pH regulator into the reaction kettle, heating to 40-100 ℃, and reacting for 1-12 h to obtain hydroxymethyl amine salt and hydroxyurea; s3, adding a catalyst into the reaction kettle, and continuously stirring and mixing; and S4, after the reaction is finished, adding a polymerization inhibitor and an aldehyde remover into the reaction kettle, and continuously stirring and mixing to form orange yellow transparent liquid, thus obtaining the high-efficiency reverse demulsifier.
The prior reverse demulsifier and the preparation method and the application thereof are mainly divided into a cationic reverse demulsifier and a polyacrylate demulsifier, wherein the cationic reverse demulsifier is mainly a high molecular weight high cationic polymer containing quaternary ammonium salt or primary amine group, the performance of the reverse demulsifier is less influenced by temperature, the demulsification time is short, a double electric layer can be effectively destroyed, oil drops are aggregated, but viscous oil sludge is generated in the using process, the wall sticking is serious, and the polyacrylate demulsifier mainly has a good effect on a sodium bicarbonate water-type produced liquid, so that the wider application of the polyacrylate demulsifier is limited, and the wide popularization is not facilitated.
Disclosure of Invention
The invention aims to provide a reverse demulsifier and a preparation method thereof, and aims to solve the problems that viscous oil sludge is generated, wall-sticking holes are serious, and a polyacrylate demulsifier cannot be widely applied in the cationic reverse demulsifier provided by the background art.
The technical scheme of the invention is as follows: the reverse demulsifier comprises the following raw materials: polyvinyl alcohol, 2, 3-epoxypropyltrimethylammonium chloride, methyl acrylate, polyamine compound, epichlorohydrin, initiator and catalyst.
A reverse demulsifier and a preparation method thereof comprise the following steps:
s1: adding polyvinyl alcohol and 2, 3-epoxypropyltrimethylammonium chloride into a reaction tank, and reacting under the conditions of a catalyst and an initiator to obtain cation modified polyvinyl alcohol;
s2: placing acrylic acid A and polyamine compound into a reaction tank to react to obtain linear polyamide;
s3: adding epoxy chloropropane into the linear polyamide in S2 under the condition of stirring to react to obtain linear polyamide-amine quaternary ammonium salt, and continuously stirring and uniformly mixing;
s4: adding the linear polyamide-amine quaternary ammonium salt, the cation modified polyethylene propanol, the cation surfactant and the distilled water into a stirring tank, and stirring and mixing;
s5: and adding the mixed liquid obtained in the step S4 into a filter tank for filtering to obtain the finished product reverse demulsifier.
Further, the catalyst in S1 is: a basic catalyst; is one of potassium hydroxide, sodium hydroxide and sodium ethoxide.
Further, the temperature of the reaction in the step S1 is 60-75 ℃; the reaction time is 2-4 h.
Further, the molar ratio of the polyvinyl alcohol, the 2, 3-epoxypropyltrimethylammonium chloride, the initiator and the catalyst in the S1 is 1: 1: 0.3:0.5.
Further, the polyamine compound in S1 is ethylenediamine.
Further, the reaction temperature in the S3 is 60-100 ℃, the reaction time is 1-3.5h, and the stirring time is 20-30 min.
Further, the mixing and stirring time in the S4 is 2-3h, and the temperature is 50-80 ℃.
Further, the mass part ratio of the linear polyamide-amine quaternary ammonium salt, the cation modified polyethylene propanol, the cation surfactant and the distilled water in the S4 is 1: 1: 1: 15.
the invention provides a reverse demulsifier and a preparation method thereof through improvement, and compared with the prior art, the reverse demulsifier has the following improvements and advantages:
(1) the reverse demulsifier has the characteristics of both a polyacrylate reverse demulsifier and a cationic reverse demulsifier, avoids the use limitation of the two demulsifiers, and avoids the problems of generation of viscous oil sludge, serious wall-sticking eye and incapability of wide application, so that the reverse demulsifier has good demulsification effect and wider application range.
(2) The preparation method of the invention has low requirements on equipment, no high-temperature high-pressure reaction exists, the prepared reverse demulsifier is relatively stable, and the prepared reverse demulsifier has better effect at proper temperature and reaction time.
Drawings
The invention is further explained below with reference to the figures and examples:
FIG. 1 is a schematic diagram of the present invention.
Detailed Description
The present invention will be described in detail with reference to the accompanying fig. 1, and the technical solutions in the embodiments of the present invention will be clearly and completely described, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It will be understood that when an element is referred to as being "secured to" another element, it can be directly on the other element or intervening elements may also be present. When a component is referred to as being "connected" to another component, it can be directly connected to the other component or intervening components may also be present. When a component is referred to as being "disposed on" another component, it can be directly on the other component or intervening components may also be present. The terms "vertical," "horizontal," "left," "right," and the like are used herein for purposes of illustration only.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
The invention provides a reverse demulsifier through improvement, which is shown in figure 1 and comprises the following raw materials: polyvinyl alcohol, 2, 3-epoxypropyltrimethylammonium chloride, methyl acrylate, polyamine compound, epichlorohydrin, initiator and catalyst.
A reverse demulsifier and a preparation method thereof comprise the following steps:
s1: adding polyvinyl alcohol and 2, 3-epoxypropyl trimethyl ammonium chloride into a reaction tank, and reacting under the conditions of a catalyst and an initiator to obtain cation modified polyvinyl alcohol;
s2: placing acrylic acid A and polyamine compound into a reaction tank to react to obtain linear polyamide;
s3: adding epoxy chloropropane into the linear polyamide in S2 under the condition of stirring to react to obtain linear polyamide-amine quaternary ammonium salt, and continuously stirring and uniformly mixing;
s4: adding linear polyamide-amine quaternary ammonium salt, cation modified polyethylene propanol, a cation surfactant and distilled water into a stirring tank, and stirring and mixing;
s5: and (4) adding the mixed liquid obtained in the step (S4) into a filter tank for filtering to obtain the finished product reverse demulsifier.
Further, the catalyst in S1 is: a basic catalyst; is one of potassium hydroxide, sodium hydroxide and sodium ethoxide.
Further, the temperature of the reaction in the step S1 is 60-75 ℃; the reaction time is 2-4 h.
Further, the molar ratio of polyvinyl alcohol, 2, 3-epoxypropyltrimethylammonium chloride, initiator and catalyst in S1 is 1: 1: 0.3:0.5.
Further, the polyamine compound in S1 is ethylenediamine.
Further, the reaction temperature in S3 is 60-100 ℃, the reaction time is 1-3.5h, and the stirring time is 20-30 min.
Further, the mixing and stirring time in the S4 is 2-3h, and the temperature is 50-80 ℃.
Further, the mass part ratio of the linear polyamide-amine quaternary ammonium salt, the cation modified polyethylene propanol, the cation surfactant and the distilled water in S4 is 1: 1: 1: 15.
example one
A reverse demulsifier comprises the following raw materials: polyvinyl alcohol, 2, 3-epoxypropyltrimethylammonium chloride, methyl acrylate, polyamine compound, epichlorohydrin, initiator and catalyst.
A reverse demulsifier and a preparation method thereof comprise the following steps:
s1: adding polyvinyl alcohol and 2, 3-epoxypropyltrimethylammonium chloride into a reaction tank, and reacting under the conditions of a catalyst and an initiator to obtain cation modified polyvinyl alcohol;
s2: placing the methyl acrylate and the polyamine compound into a reaction tank to react to obtain linear polyamide;
s3: adding epoxy chloropropane into the linear polyamide in S2 under stirring to react to obtain linear polyamide-amine quaternary ammonium salt, and continuously stirring and uniformly mixing;
s4: adding linear polyamide-amine quaternary ammonium salt, cation modified polyethylene propanol, a cation surfactant and distilled water into a stirring tank, and stirring and mixing;
s5: and (4) adding the mixed liquid obtained in the step (S4) into a filter tank for filtering to obtain the finished product reverse demulsifier.
Further, the catalyst in S1 is: a basic catalyst; is one of potassium hydroxide, sodium hydroxide and sodium ethoxide.
Further, the temperature of the reaction in step S1 is 60 ℃; the reaction time was 2 h.
Further, the molar ratio of the polyvinyl alcohol, the 2, 3-epoxypropyltrimethylammonium chloride, the initiator and the catalyst in S1 is 1: 1: 0.3:0.5.
Further, the polyamine compound in S1 is ethylenediamine.
Further, the reaction temperature in S3 was 60 ℃, the time was 1h, and the stirring time was 20 min.
Further, in S4, the mixing and stirring time was 2 hours and the temperature was 50 ℃.
Further, the mass part ratio of the linear polyamide-amine quaternary ammonium salt, the cation modified polyethylene propanol, the cation surfactant and the distilled water in S4 is 1: 1: 1: 15.
example two
A reverse demulsifier comprises the following raw materials: polyvinyl alcohol, 2, 3-epoxypropyltrimethylammonium chloride, methyl acrylate, polyamine compound, epichlorohydrin, initiator and catalyst.
A reverse demulsifier and a preparation method thereof comprise the following steps:
s1: adding polyvinyl alcohol and 2, 3-epoxypropyl trimethyl ammonium chloride into a reaction tank, and reacting under the conditions of a catalyst and an initiator to obtain cation modified polyvinyl alcohol;
s2: placing acrylic acid A and polyamine compound into a reaction tank to react to obtain linear polyamide;
s3: adding epoxy chloropropane into the linear polyamide in S2 under the condition of stirring to react to obtain linear polyamide-amine quaternary ammonium salt, and continuously stirring and uniformly mixing;
s4: adding the linear polyamide-amine quaternary ammonium salt, the cation modified polyethylene propanol, the cation surfactant and the distilled water into a stirring tank, and stirring and mixing;
s5: and adding the mixed liquid obtained in the step S4 into a filter tank for filtering to obtain the finished product reverse demulsifier.
Further, the catalyst in S1 is: a basic catalyst; is one of potassium hydroxide, sodium hydroxide and sodium ethoxide.
Further, the temperature of the reaction in step S1 is 70 ℃; the reaction time was 3 h.
Further, the molar ratio of polyvinyl alcohol, 2, 3-epoxypropyltrimethylammonium chloride, initiator and catalyst in S1 is 1: 1: 0.3:0.5.
Further, the polyamine compound in S1 is ethylenediamine.
Further, the reaction temperature in S3 was 80 ℃ for 2 hours and the stirring time was 25 min.
Further, the mixing and stirring time in S4 was 2.5 hours, and the temperature was 65 ℃.
Further, in S4, the mass part ratio of the linear polyamide-amine quaternary ammonium salt, the cation modified polyethylene propanol, the cation surfactant and the distilled water is 1: 1: 1: 15.
EXAMPLE III
The reverse demulsifier comprises the following raw materials: polyvinyl alcohol, 2, 3-epoxypropyltrimethylammonium chloride, methyl acrylate, polyamine compound, epichlorohydrin, initiator and catalyst.
A reverse demulsifier and a preparation method thereof comprise the following steps:
s1: adding polyvinyl alcohol and 2, 3-epoxypropyl trimethyl ammonium chloride into a reaction tank, and reacting under the conditions of a catalyst and an initiator to obtain cation modified polyvinyl alcohol;
s2: placing acrylic acid A and polyamine compound into a reaction tank to react to obtain linear polyamide;
s3: adding epoxy chloropropane into the linear polyamide in S2 under the condition of stirring to react to obtain linear polyamide-amine quaternary ammonium salt, and continuously stirring and uniformly mixing;
s4: adding linear polyamide-amine quaternary ammonium salt, cation modified polyethylene propanol, a cation surfactant and distilled water into a stirring tank, and stirring and mixing;
s5: and (4) adding the mixed liquid obtained in the step (S4) into a filter tank for filtering to obtain the finished product reverse demulsifier.
Further, the catalyst in S1 is: a basic catalyst; is one of potassium hydroxide, sodium hydroxide and sodium ethoxide.
Further, the temperature of the reaction in step S1 is 75 ℃; the reaction time was 4 h.
Further, the molar ratio of the polyvinyl alcohol, the 2, 3-epoxypropyltrimethylammonium chloride, the initiator and the catalyst in S1 is 1: 1: 0.3:0.5.
Further, the polyamine compound in S1 is ethylenediamine.
Further, the reaction temperature in S3 is 100 ℃, the reaction time is 3.5h, and the stirring time is 20-30 min.
Further, in S4, the mixing and stirring time was 3 hours and the temperature was 80 ℃.
Further, the mass part ratio of the linear polyamide-amine quaternary ammonium salt, the cation modified polyethylene propanol, the cation surfactant and the distilled water in S4 is 1: 1: 1: 15.
the working principle of the invention is as follows: adding polyvinyl alcohol and 2, 3-epoxypropyltrimethylammonium chloride into a reaction tank, wherein under the conditions of a catalyst (one of potassium hydroxide, sodium hydroxide and sodium ethoxide) and an initiator, the molar ratio of the polyvinyl alcohol to the 2, 3-epoxypropyltrimethylammonium chloride to the initiator to the catalyst is 1: 1: 0.3:0.5, reacting at the temperature of 60-75 ℃ for 2-4h to obtain cation modified polypropylene glycol; placing acrylic acid A and polyamine compound (ethylenediamine) into a reaction tank to react to obtain linear polyamide; adding epoxy chloropropane into linear polyamide under stirring to react to obtain linear polyamide-amine quaternary ammonium salt, wherein the reaction temperature is 60-100 ℃, the reaction time is 1-3.5h, and continuously stirring and uniformly mixing for 20-30 min; linear polyamide-amine quaternary ammonium salt, cation modified polyethylene propanol, a cation surfactant and distilled water are mixed according to a mass ratio of 1: 1: 1: 15 adding the mixture into a stirring tank, stirring and mixing for 2-3h at the temperature of 50-80 ℃; and adding the obtained mixed solution into a filter tank for filtering to obtain the finished product reverse demulsifier.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.

Claims (9)

1. A reverse demulsifier, characterized by: the method comprises the following raw materials: polyvinyl alcohol, 2, 3-epoxypropyltrimethylammonium chloride, methyl acrylate, polyamine compound, epichlorohydrin, initiator and catalyst.
2. The reverse demulsifier and the preparation method thereof are characterized in that: the method comprises the following steps:
s1: adding polyvinyl alcohol and 2, 3-epoxypropyltrimethylammonium chloride into a reaction tank, and reacting under the conditions of a catalyst and an initiator to obtain cation modified polyvinyl alcohol;
s2: placing acrylic acid A and polyamine compound into a reaction tank to react to obtain linear polyamide;
s3: adding epoxy chloropropane into the linear polyamide in S2 under the condition of stirring to react to obtain linear polyamide-amine quaternary ammonium salt, and continuously stirring and uniformly mixing;
s4: adding the linear polyamide-amine quaternary ammonium salt, the cation modified polyethylene propanol, the cation surfactant and the distilled water into a stirring tank, and stirring and mixing;
s5: and adding the mixed liquid obtained in the step S4 into a filter tank for filtering to obtain the finished product reverse demulsifier.
3. The reverse demulsifier and the preparation method thereof according to claim 2, wherein the reverse demulsifier comprises: the catalyst in the S1 is: a basic catalyst; is one of potassium hydroxide, sodium hydroxide and sodium ethoxide.
4. The reverse demulsifier and the preparation method thereof according to claim 2, wherein the reverse demulsifier comprises: the reaction temperature in the step S1 is 60-75 ℃; the reaction time is 2-4 h.
5. The reverse demulsifier and the preparation method thereof according to claim 2, wherein the reverse demulsifier comprises: the molar ratio of polyvinyl alcohol, 2, 3-epoxypropyltrimethylammonium chloride, initiator and catalyst in S1 is 1: 1: 0.3:0.5.
6. The reverse demulsifier and the preparation method thereof according to claim 2, wherein the reverse demulsifier comprises: the polyamine compound in the S1 is ethylenediamine.
7. The reverse demulsifier and the preparation method thereof according to claim 2, wherein the reverse demulsifier comprises: the reaction temperature in the S3 is 60-100 ℃, the reaction time is 1-3.5h, and the stirring time is 20-30 min.
8. The reverse demulsifier and the preparation method thereof according to claim 2, wherein the reverse demulsifier comprises: the S4 is mixed and stirred for 2-3h at the temperature of 50-80 ℃.
9. The reverse demulsifier and the preparation method thereof according to claim 2, wherein the reverse demulsifier comprises: the mass part ratio of the linear polyamide-amine quaternary ammonium salt, the cation modified polyethylene propanol, the cation surfactant and the distilled water in the S4 is 1: 1: 1: 15.
CN202210512660.2A 2022-05-12 2022-05-12 Reverse demulsifier and preparation method thereof Pending CN114768309A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115672064A (en) * 2022-11-28 2023-02-03 浙江工业大学 Epoxy group grafted modified polyvinyl alcohol nanofiltration membrane and preparation method thereof
CN117417469A (en) * 2023-11-21 2024-01-19 江西省宏丰塑胶有限公司 A kind of high-efficiency polyvinyl butyral resin and preparation method thereof

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CN105295988A (en) * 2014-12-16 2016-02-03 新疆科力新技术发展有限公司 Aqueous-phase demulsifier and preparation method thereof
CN108179023A (en) * 2017-12-07 2018-06-19 中海油天津化工研究设计院有限公司 A kind of viscous crude Produced Liquid reverse-phase emulsifier and preparation method thereof
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US4457860A (en) * 1982-04-26 1984-07-03 The Dow Chemical Company Use of heterocyclic ammonium polyamidoamines as demulsifiers
CN102234526A (en) * 2010-04-30 2011-11-09 中国石油天然气集团公司 Dendritic reverse demulsifier
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115672064A (en) * 2022-11-28 2023-02-03 浙江工业大学 Epoxy group grafted modified polyvinyl alcohol nanofiltration membrane and preparation method thereof
CN115672064B (en) * 2022-11-28 2025-04-25 浙江工业大学 A grafted epoxy group modified polyvinyl alcohol nanofiltration membrane and preparation method thereof
CN117417469A (en) * 2023-11-21 2024-01-19 江西省宏丰塑胶有限公司 A kind of high-efficiency polyvinyl butyral resin and preparation method thereof

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Application publication date: 20220722