CN106565426A - High-efficiency and environment-friendly type oxa-perfluoropolyether oil field demulsifier and preparation method - Google Patents
High-efficiency and environment-friendly type oxa-perfluoropolyether oil field demulsifier and preparation method Download PDFInfo
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- CN106565426A CN106565426A CN201610999081.XA CN201610999081A CN106565426A CN 106565426 A CN106565426 A CN 106565426A CN 201610999081 A CN201610999081 A CN 201610999081A CN 106565426 A CN106565426 A CN 106565426A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/01—Preparation of ethers
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/08—Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/28—Preparation of carboxylic acid esters by modifying the hydroxylic moiety of the ester, such modification not being an introduction of an ester group
- C07C67/287—Preparation of carboxylic acid esters by modifying the hydroxylic moiety of the ester, such modification not being an introduction of an ester group by introduction of halogen; by substitution of halogen atoms by other halogen atoms
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G33/00—Dewatering or demulsification of hydrocarbon oils
- C10G33/04—Dewatering or demulsification of hydrocarbon oils with chemical means
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/10—Feedstock materials
- C10G2300/1033—Oil well production fluids
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Abstract
The invention provides a high-efficiency and environment-friendly type oxa-perfluoropolyether oil field demulsifier and a preparation method. The demulsifier is prepared from multi-hydroxyl-containing dendritic polyglycerol (A) and a carboxyl modified product (B) of (A) through polymerization with biodegradable hydrophobic and oilphobic oxa-perfluoropolyether (C), wherein (A) is prepared from 1,1,1-trimethylolpropane (TMP) and epoxy isopropyl alcohol through ring opening polymerization; (B) is prepared from (A) through anhydride carboxyl modification; (A) or (B) is subjected to a substitution reaction with (C) at the normal temperature, and the dendritic oxa-perfluoropolyether-containing demulsifier with different hydrophilic and oilphobic properties can be prepared. Compared with an existing oil field demulsifier, the series of the demulsifier has the advantages of low consumption, high dehydration rate, high dehydration speed, clean dehydrated water and the like, overcomes common defects of the existing oil field demulsifier and reduces environmental pollution.
Description
Technical field
The invention belongs to petrochemical industry, is a kind of height suitable for processes such as oil field mining liquid, reinjected water and transfers
Effect environment-friendly type oxa- PFPE oil field demulsifier and preparation method.
Background technology
At this stage, domestic most of oil field has been enter into tertiary phase, and the water content of Produced Liquid typically 70 ~
90 %, and the moisture content index of tank oil is：The water content of lightweight and middle matter crude oil will be less than 0.5 %, and heavy crude contains
The water yield will then be less than 1.0 %.
The discharge standard of national oilfield sewage is：Two grades of water oil content are less than 20 mg/L, and one-level water oil content is then less than 10
Mg/L, is generally processed to reinjected water using technologies such as sedimentation-coagulation air-float-filtrations, and process is loaded down with trivial details and inefficient.And it is right
The physics of externally discharged waste water is mainly using technologies such as biodegradation, chemical degradation, membrane filtration and electrochemistry depth sewage disposals.From adopting
Go out liquid to the processing procedure of commercial crude, the extraction efficiency of crude oil is low, cumbersome, energy consumption is big, and pollute environment.
At present, domestic widely used oil field demulsifier mainly with oleic alcohol, phenolic resin, phenol-amine resin etc. for
Beginning agent epoxy butane, expoxy propane, oxirane carry out the polyether type demulsifying agent that block polymerization is obtained, this kind of product usage amount
Under 100-200 ppm hot conditionss, dehydration rate is up to 90 %, but deviates from the oil content of water much larger than national secondary discharge standard,
Abjection water is not directly discharged, and also needs just to reach discharge standard through further processed.
Research and develop the thick oil demulsifier that a kind of consumption is few, dehydration rate is high, abjection water oil content is low extremely urgent.With reference to market
The biodegradable fluoride of " hydrophobic and oil repellent " is grafted to polyether type demulsifying agent, can make polyether type demulsifying agent more by demand
The surface tension of good reduction oil-water interfaces, so as to accelerate rate of water loss, lifts dehydration rate, so as to reach more preferable breakdown of emulsion effect
Really.
Pertinent literature points out breakdown of emulsion effect is obtained after the hydrophilicity fabulous perfluorinated agent modifier of polyglycidyl ether
Fruit preferably anti emulsifier, such as：yue zhang (Colloids and Surfaces A: Physicochemical and
Engineering Aspects, are 436,2013) raw material and the bromo- 2- methyl propionyl bromides of 2- in water-bath bar with polyglycidyl ether
After atomic radicals transfer is carried out under part, synthesis fluorine-containing section and modified macromole are acted on perfluoroethyl butyl ester then at 90 DEG C
Polymer, the product can be used for medicine and oilfield, but there is synthetic method complexity, and the requirement to raw material is higher, product
Stability it is inadequate the problems such as；Beautiful (the University Of Shanxi's journal, 34,2011) with bis- fluoro- 1,3- methylimidazoles of 2,2- of a word used in person's names stamen
Ketone (DFI) replaces the terminal hydroxy group of polyglycidyl ether to synthesize anti emulsifier, but the method complex operation for fluorination reagent, reacts
Temperature is high, product structure is difficult to control to, the problems such as application range of products is narrow；Chinese patent CN102210995A describes one kind and contains
Fluorine surfactant preparation method, but the product that obtains of the method is multiple perfluor Long carbon chains, and fluorochemical monomer prepares difficult, product
Production cost is quite high, and perfluor Long carbon chain is not allowed degradable, does not reach environmental requirement, so as to promote.Therefore it is of the invention
With the polyglycidyl ether and hydrophobic performance of good hydrophilic property, preferable two ~ trimerization of the hydrophobic type oxa- perfluoroacyl fluoride of polarity as raw material,
Hydrophilic or hydrophobic type anhydride is modifying agent, more preferable by two-step method and three-step approach synthesis ratio tradition 169 demulsification performance of de-emulsifier SP
The biodegradable efficient polyether type demulsifying agent of (consumption is few, dewatering speed is fast), the series product can act on difference simultaneously
The crude oil emulsion of oil content, deviates from water clean and transparent after breakdown of emulsion.
The content of the invention：
The purpose of the present invention is to provide a kind of efficient and environment-friendly type oxa- to solve the problems, such as above-mentioned existing crude oil demulsifier
PFPE oil field demulsifier and preparation method.
The purpose of the present invention is mainly achieved through the following technical solutions：
A kind of efficient and environment-friendly type oxa- PFPE oil field demulsifier, it is characterised in that the raw material composition of demulsifier D and quality hundred
Divide content as follows：A10 ~ 15 %, C85 ~ 90 %；Above-mentioned A is a kind of polyglycidyl ether of dendroid containing multiple hydroxyls, and it is
Prepared by TMP and epoxy isopropanol Jing ring-opening polymerisations, above-mentioned C is a kind of extremely strong low polymerization degree oxa- perfluor acyl of activity
Fluorine, is the two ~ tetramer obtained by the ring-opening polymerisation of hexafluoropropylene oxide Jing.
The structural formula of described A and C and demulsifier D includes:
In formula：A only represents the structure of polyglycidyl ether；In C, n can be 0,1,2；Rf in D represents C.
A kind of efficient and environment-friendly type oxa- PFPE oil field demulsifier, it is characterised in that the composition and quality hundred of demulsifier E
Divide content as follows：A30 ~ 35 %, anhydrides (using different anhydride, obtain the different product of hydrophilic and oleophilic performance) 20 ~ 25 %,
C40 %~50 %.Above-mentioned A is a kind of polyglycidyl ether of dendroid containing multiple hydroxyls, and it is by TPM and epoxy isopropanol Jing
Ring-opening polymerisation is prepared, and above-mentioned C is a kind of extremely strong low polymerization degree oxa- perfluoroacyl fluoride of activity, is by hexafluoropropylene oxide Jing
Ring-opening polymerisation is obtained.The end group of A obtains B Jing after anhydride moiety is carboxy-modified, then is polymerized with C and can be prepared by demulsifier E.
The structural formula of B and demulsifier E includes：
Wherein：Rf in formula represents C, and R is represented respectively：(CH2)n, n=2,3,4；C6H6, (C6H6)CHCH2。
The preparation method of a kind of efficient and environment-friendly type oxa- PFPE oil field demulsifier, preferably, comprising the following steps：The preparation of C：Referring especially to utility model patent：A kind of production equipment of hexafluoropropylene oxide oligomer correspondence carboxylate.
The synthesizing formula of C is：
350 ~ 400 mg of hexafluoropropylene oxide
250 mL of tetraethyl dimethyl ether
0.8 ~ 1.0 g of catalyst
The preparation of A：10 mL Feldalat KM methanol solutions are added in the four-hole bottle equipped with electric mixing device and nitrogen inlet,
The 2.86 g TMP for accurately weighing, heating (carry out 10% deprotonation to TMP) after making which be completely dissolved 2 h, Jing vacuum distillations
Remove solvent methanol.Maintain reaction temperature at 95 DEG C, 25 mL epoxy isopropanols are slowly dropped to reactor in 12 h by control
It is interior, drip off 2 h of sustained response, lower the temperature A product.
Above-mentioned products therefrom is dissolved in methyl alcohol, A is placed in methanol solution with the permeable membrane of 1000 molecular weight and is removed
Small molecule, permeates 24 h in neutrality under the conditions of 4 DEG C.In vacuum drying oven, 60 DEG C of 15 h of drying, obtain raw material A.
The synthesizing formula of A：
Feldalat KM 0.42g
TMP 2.68g
Methanol 5mL
Epoxy isopropanol 25mL
Reaction equation：
A Jing succinic anhydrides are carboxy-modified into B：1.1 g succinic anhydrides are weighed accurately in equipped with agitator, the four of letting nitrogen in and deoxidizing
In mouth bottle, 0.15 g DMAP of Deca after adding 20 mL DMF to be heated to 70 DEG C.Accurately weigh 2.0 g A and be dissolved in 20 mL DMF
In solution, it is transferred in constant pressure funnel after dissolving completely, is slowly dropped in four-hole bottle, as the addition of A occurs instead
Answer device temperature to reduce, it is necessary to which controlling reaction temperature is higher than 70 DEG C, 2 h of sustained response is still needed to after dripping off to reacting complete, methanol is used
After lysate, it is settled out after product with ethyl acetate, 60 DEG C of 15 h of vacuum drying obtain raw material B.
The carboxy-modified formula into B of A Jing succinic anhydrides：
Succinic anhydride 1.1g
A 2.0g
DMAP 0.15g
DMF 40mL
Ethyl acetate 30mL
Reaction equation：
Demulsification performance is analyzed：The requirement that method is tried according to SY/T5281-2000 bottles determines the demulsification of each product.
Preferably, stepMiddle Feldalat KM methanol solution must be suitably excessive, and adds fraction of potassium hydroxide.
Preferably, stepMiddle solvent methanol could dropwise reaction monomer after thoroughly must being evaporated.
Preferably, stepMiddle methanol solution needs to carry out Ghana's silk distillation except water process.
Preferably, stepThe rate of addition of middle epoxy isopropanol must be slow as far as possible, is divided into 12h and is added drop-wise to reaction
In device.
Preferably, stepMiddle DMF makees solvent, and DMAP makees catalyst.
Preferably, stepThe sedimentation agent ethyl acetate of middle product B, replaces acetone.
Preferably, stepMiddle A will be controlled in more than 1h as far as possible slowly to the speed of the Deca of reactor containing anhydrides, and is protected
Temperature of reactor is held more than 70 DEG C.
The beneficial effects of the present invention is：There is provided demulsifier by the dendritic polyglycidyl ether containing multiple hydroxyls
A and its carboxy-modified product B is polymerized with biodegradable hydrophobic and oil repellent oxa- perfluoroacyl fluoride C.A or B and C is at normal temperatures
Carry out substitution reaction and can be prepared by different dendroid PFPE containing the oxa- demulsifier of hydrophilic and oleophobic.Compare existing oil field
Demulsifier, the serial demulsifier have the advantages that consumption is few, dehydration rate is high, dewatering speed is fast, abjection water is clean, and preparation side
Method is simple, solves the defect of conventional oil field demulsifier generally existing, reduces environmental pollution.
Specific embodiment：
Contrast case
The widely used oil field demulsifier SP169 in oil field is a kind of with oleic alcohol as initiator and oxireme, epoxy at present
Propylene is polymerized under catalyst action and obtains polyether type demulsifying agent.Jing demulsifications are analyzed：When the consumption of SP169 is 70 ppm,
When 60 DEG C, 20 min dehydrations more than 60%, in 30 min the W/O crude oil emulsions of water content 50% can be dehydrated completely, and abjection water is omited
Band is muddy in faint yellow.
Embodiment 1
8mL (C) is taken with the constant pressure funnel equipped with tetraethyl dimethyl ether interleaving agent, and is slowly added dropwise under stirring at normal temperature state
To in the there-necked flask equipped with 2.0 g (A) of anhydrous and oxygen-free, tail gas is collected with unsaturated carbonate potassium solution.Sustained response 2 under room temperature
H, products therefrom 24 h of natural air drying in air are dried 24 h after 60 DEG C of vacuum drying ovens, obtain demulsifier (D).
Reaction equation is：
Embodiment 2
Appropriate 4mL (C) is taken with the constant pressure funnel equipped with tetraethyl dimethyl ether interleaving agent, and it is slow under stirring at normal temperature state
It is added drop-wise in the four-hole bottle equipped with 6.0 g (B), tail gas is collected with unsaturated carbonate potassium solution.Continue in 40 DEG C of waters bath with thermostatic control anti-
2 h, products therefrom 24 h of natural air drying in air are answered to be dried 24 h after 60 DEG C of vacuum drying ovens, obtain demulsifier (E).
Reaction equation：
Embodiment 3
4.4g phthalic anhydrides are accurately weighed in equipped with agitator, in the four-hole bottle of letting nitrogen in and deoxidizing, adds 20mLDMF to be heated to
0.15 g DMAP of Deca after 70 DEG C.Accurately weigh 2.0 g (A) to be dissolved in 20 mLDMF solution, after dissolving completely, be transferred to perseverance
In pressure Dropping funnel, it is slowly dropped in four-hole bottle, as the addition of (A) occurs that temperature of reactor is reduced, it is necessary to which control is anti-
Temperature is answered higher than 70 DEG C, 2 h of sustained response is still needed to after dripping off to reacting complete, with methanol lysate after, it is heavy with ethyl acetate
Form sediment after product, 60 DEG C of 15 h of vacuum drying obtain raw material (F).
The reaction equation and (B) for preparing (F) is essentially identical, simply using phthalic anhydride as the carboxy-modified of (A)
Agent.
Appropriate 2 mL (C) is taken with the constant pressure funnel equipped with tetraethyl dimethyl ether interleaving agent, and in stirring at normal temperature state
Under be slowly dropped in the four-hole bottle equipped with 6.0 g (F), tail gas with unsaturated carbonate potassium solution collect.In 40 DEG C of waters bath with thermostatic control
2 h of sustained response, products therefrom 24 h of natural air drying in air are dried 24 h after 60 DEG C of vacuum drying ovens, obtain demulsifier
(G), reaction equation is essentially identical with example 2.
Embodiment 4
2.0g isobutyric anhydrides are accurately weighed in equipped with agitator, in the four-hole bottle of letting nitrogen in and deoxidizing, adds 20mLDMF to be heated to 70 DEG C
0.15 g DMAP of Deca afterwards.Accurately weigh 2.0 g (A) to be dissolved in 20 mLDMF solution, after dissolving completely, be transferred to constant pressure drop
In liquid funnel, it is slowly dropped in four-hole bottle, as the addition of (A) occurs that temperature of reactor is reduced, it is necessary to control reaction temperature
Degree still needs to 2 h of sustained response to reacting complete higher than 70 DEG C after dripping off, with methanol lysate after, be settled out with ethyl acetate
After product, 60 DEG C of 15 h of vacuum drying obtain raw material (H).
The reaction equation and (B) for preparing (H) is essentially identical, simply using isobutyric anhydride as carboxy-modified dose of (A).
Appropriate 4 mL (C) is taken with the constant pressure funnel equipped with tetraethyl dimethyl ether interleaving agent, and in stirring at normal temperature state
Under be slowly dropped in the four-hole bottle equipped with 6.0 g (H), tail gas with unsaturated carbonate potassium solution collect.In 40 DEG C of waters bath with thermostatic control
2 h of sustained response, products therefrom 24 h of natural air drying in air are dried 24 h after 60 DEG C of vacuum drying ovens, obtain demulsifier
(I), reaction equation is essentially identical with example 2.
Embodiment 5
7.0 g phenylsuccinic acids acid anhydrides are accurately weighed in equipped with agitator, in the four-hole bottle of letting nitrogen in and deoxidizing, adds 20 mL DMF to add
Heat is to 0.15 g DMAP of Deca after 70 DEG C.Accurately weigh 2.0 g (A) to be dissolved in 20 mLDMF solution, proceed to after dissolving completely
To in constant pressure funnel, it is slowly dropped in four-hole bottle, as the addition of (A) occurs that temperature of reactor is reduced, it is necessary to control
Reaction temperature processed is higher than 70 DEG C, still needs to 2 h of sustained response to reacting complete after dripping off, with methanol lysate after, use acetic acid second
After ester is settled out product, 60 DEG C of 15 h of vacuum drying obtain raw material (J).
The reaction equation and (B) for preparing (J) is essentially identical, simply using phenylsuccinic acid acid anhydride as the carboxy-modified of (A)
Agent.
Appropriate 2mL (C) is taken with the constant pressure funnel equipped with tetraethyl dimethyl ether interleaving agent, and under stirring at normal temperature state
It is slowly dropped in the four-hole bottle equipped with 6.0 g (J), tail gas is collected with unsaturated carbonate potassium solution.Hold in 40 DEG C of waters bath with thermostatic control
2 h of continuous reaction, products therefrom 24 h of natural air drying in air are dried 24 h after 60 DEG C of vacuum drying ovens, obtain demulsifier (K),
Reaction equation is substantially the same manner as Example 2.
Claims (11)
1. a kind of efficient and environment-friendly type oxa- PFPE oil field demulsifier, it is characterised in that：Described environment-friendly type oxa- perfluor gathers
Ether oil field demulsifier is obtained by three-step synthesis method, and the demulsifier is by the dendritic polyglycidyl ether A containing multiple hydroxyls
And its carboxy-modified product B is polymerized with biodegradable hydrophobic and oil repellent oxa- perfluoroacyl fluoride C.
2. a kind of efficient and environment-friendly type oxa- PFPE oil field demulsifier according to claim 1, it is characterised in that：It is described
Environment-friendly type oxa- PFPE oil field demulsifier include demulsifier D and anhydride modified demulsifier E, G, I, K；D and E, G, I, K
The structure of formula is:
D formulas
In formula, the structure of C is as follows, wherein for n=2-4
R in E is (CH2)2, the R in G is C6H6, the R in I is (CH2)6, in K, R is (C6H6)CHCH2K the R in) is (C6H6)2。
3. a kind of efficient and environment-friendly type oxa- PFPE oil field demulsifier according to claim 2, it is characterised in that：It is described
Demulsifier D composition and weight/mass percentage composition it is as follows：A10 ~ 15 %, C85 ~ 90 %；Above-mentioned A is that a kind of dendroid contains multiple hydroxyls
The polyglycidyl ether of base, it is prepared by TMP and epoxy isopropanol Jing ring-opening polymerisations, and above-mentioned C is extremely strong for a kind of activity
Low polymerization degree oxa- perfluoroacyl fluoride, be the two ~ tetramer obtained by the ring-opening polymerisation of hexafluoropropylene oxide Jing.
4. a kind of efficient and environment-friendly type oxa- PFPE oil field demulsifier according to claim 3, it is characterised in that：It is described
The synthesis step of demulsifier D be：4 mLC are existed by A of the synthesis containing 24 hydroxyls by terminal groups modification agent of the anhydride of hydrophilic
It is added drop-wise in the state of anhydrous and oxygen-free in the A of corresponding amount, appropriate triethylamine is Fu's acid agent, the ratio of the amount of the material of wherein A and C
For 1:After reacting 1 h under 24 normal temperature and pressure states, 60 DEG C of vacuum drying ovens dry to obtain demulsifier D after filtering.
5. a kind of efficient and environment-friendly type oxa- PFPE oil field demulsifier according to claim 2, it is characterised in that：It is described
Demulsifier E and I composition and weight/mass percentage composition it is as follows：A30 ~ 35 %, 20 ~ 25 % of hydrophilic anhydride, C40 ~ 50 %, A's
End group obtains B Jing after anhydride moiety is carboxy-modified, then is polymerized with C and can be prepared by demulsifier E.
6. a kind of efficient and environment-friendly type oxa- PFPE oil field demulsifier according to claim 5, it is characterised in that：It is described
Hydrophilic anhydride be one or two kinds of in succinic anhydride or isobutyric anhydride.
7. a kind of efficient and environment-friendly type oxa- PFPE oil field demulsifier according to claim 6, it is characterised in that：It is described
The synthesis step of demulsifier E and I be：According to A of the synthesis containing 24 hydroxyls, 1.1 g succinic anhydrides and 2.0 g are accurately weighed
Isobutyric anhydride in equipped with agitator letting nitrogen in and deoxidizing four-hole bottle in, add 20 mL DMF be heated to 70 DEG C after Deca 0.15g
DMAP；Accurately weigh 2.0 g A to be dissolved in 20 mL DMF solutions, be transferred in constant pressure funnel after dissolving completely, it is slow to drip
It is added in four-hole bottle；A adds post-reactor temperature significantly reduce, it is necessary to which controlling reaction temperature is higher than 70 DEG C, is still needed to after dripping off
2 h of sustained response to reacting complete, with methanol lysate after, be settled out after product with ethyl acetate, 60 DEG C of vacuum drying 15
H, obtains raw material B, H；C is added drop-wise in the B and H of corresponding amount in the state of anhydrous and oxygen-free, appropriate triethylamine is Fu's acid agent, its
The ratio of the amount of the material of middle B, H and C is 1:2, after reacting 1h under normal temperature and pressure stirring, after filtering, 60 DEG C of vacuum drying
Case dries to obtain target product.
8. a kind of efficient and environment-friendly type oxa- PFPE oil field demulsifier according to claim 7, it is characterised in that：It is hydrophilic
Type anhydride with hydrophilic it is carboxy-modified when, in modified B the quantity ratio of hydroxyl and carboxyl be 2:When 1 product performance most
It is good.
9. a kind of efficient and environment-friendly type oxa- PFPE oil field demulsifier according to claim 2, it is characterised in that：It is described
Demulsifier G, K by demulsifier E and I constitute and weight/mass percentage composition is as follows：A30 ~ 35 %, hydrophobic type anhydrides 30 ~ 50
%, C15 ~ 20 %；The end group of A Jing after anhydride moiety is carboxy-modified F, J, then be polymerized with C and can be prepared by demulsifier G, K.
10. a kind of efficient and environment-friendly type oxa- PFPE oil field demulsifier according to claim 9, it is characterised in that：Institute
The hydrophobic type anhydride stated is phenylsuccinic acid acid anhydride, the one or two kinds of in phthalic anhydride.
A kind of 11. efficient and environment-friendly type oxa- PFPE oil field demulsifiers according to claim 10, it is characterised in that：Institute
The synthesis step of the demulsifier G and K that state is:
A of the synthesis containing 24 hydroxyls, accurately weighs 4.4 g phenylsuccinic acids acid anhydrides and 7.0g phthalic anhydrides in equipped with stirring
In the four-hole bottle of device letting nitrogen in and deoxidizing, 0.15 g DMAP of Deca after adding 20 mL DMF to be heated to 70 DEG C；2.0 g A are weighed accurately
It is dissolved in 20 mL DMF solutions, is transferred in constant pressure funnel after dissolving completely, is slowly dropped in four-hole bottle, due to A's
Addition occurs that temperature of reactor is reduced, it is necessary to which controlling reaction temperature is higher than 70 DEG C, still needs to 2 h of sustained response to reaction after dripping off
Completely, after with methanol lysate, it is settled out after product with ethyl acetate, 60 DEG C of 15 h of vacuum drying obtain raw material F, J；C is existed
It is added drop-wise in the state of anhydrous and oxygen-free in the F and H of corresponding amount, wherein the ratio of the amount of the material of F, H and C is 2:1, normal temperature and pressure shape
After reacting 1h under state, Jing is filtered, and 60 DEG C of vacuum drying ovens dry to obtain target product.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1618835A (en) * | 2003-11-21 | 2005-05-25 | 西安石油大学 | Preparation method of high efficiency broad spectrum deemulsifier |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1618835A (en) * | 2003-11-21 | 2005-05-25 | 西安石油大学 | Preparation method of high efficiency broad spectrum deemulsifier |
Non-Patent Citations (2)
| Title |
|---|
| FLORIAN K. WOLF等: "Poly(glycolide) multi-arm star polymers: Improved solubility via limited arm length", 《J.ORG.CHEM.》 * |
| 任朝华等: "原油破乳剂的合成方法", 《精细石油化工进展》 * |
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