CN107236092A - One kind contains silicate sturcture monomer and preparation method and application - Google Patents
One kind contains silicate sturcture monomer and preparation method and application Download PDFInfo
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- CN107236092A CN107236092A CN201710595145.4A CN201710595145A CN107236092A CN 107236092 A CN107236092 A CN 107236092A CN 201710595145 A CN201710595145 A CN 201710595145A CN 107236092 A CN107236092 A CN 107236092A
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/12—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polysiloxanes
- C08F283/124—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polysiloxanes on to polysiloxanes having carbon-to-carbon double bonds
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- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
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Abstract
Contain silicate sturcture monomer and preparation method and application the invention discloses one kind.It comprises the following steps：Solution containing silicate structure monomer is added dropwise in aqueous silicate solution, hybrid reaction, obtains the aqueous solution containing silicate sturcture monomer, separation is obtained containing silicate sturcture monomer.Preparation method of the present invention is simple；What is prepared is higher containing silicate sturcture monomer reactivity, it is easy to prepare high molecular weight products, thickening property is excellent, product dosage is small when using.
Description
Technical field
The present invention relates to one kind containing silicate sturcture monomer and preparation method and application, belong to water soluble polymer conjunction
Into technical field.
Background technology
Development of the exploitation and utilization of oil to national economy has important effect.At present, China's developed field
It is most of to enter middle-late waterflooding stage, only can constant rate of production by tertiary oil recovery technology.In tertiary oil recovery technology,
Polymer displacement of reservoir oil tech is a kind of flooding method that water-soluble polymer solution is injected into oil reservoir.Due to adding injection water
Viscosity, mobility ratio is improved, the region that displacing phase involves can be effectively improved, reduced oil saturation, adopted so as to improve crude oil
Yield.Therefore, polymer displacement of reservoir oil, binary combination flooding (polymer-surfactant), ternary composite oil-displacing (alkali-polymer-table
Face activating agent) etc. tertiary oil recovery technology field test has all been carried out in the major oil area such as grand celebration, triumph, Kelamayi and has been achieved
Immense success, particularly Daqing oil field, polymer displacement of reservoir oil tech have been enter into the large-scale industrial application stage, and polymer per ton increases oil
Amount has reached 120~150 tons.
In view of the specific feature of domestic oil reservoir and crude oil, reservoir temperature is more than 75 DEG C, formation water salinity is more than
30000mg/L high temperature and high salt oil deposit, shared stock number is quite big.At present, the most frequently used flooding polymers, partial hydrolysis gathers
Acrylamide (HPAM), easily occurs hydrolysis and oxidative degradation, the viscosity of HPAM solution is with the increasing of ageing time at high temperature
Plus and drastically decline, do not possess long-time stability, which has limited application of the HPAM oil displacement systems in high temperature and high salt oil deposit.Cause
How this, provide a kind of flooding polymers with good temperature-resistant anti-salt performance, be that present polymer technology of reservoir sweep is urgently to be resolved hurrily
One of the problem of.
Currently, in order to improve stability of the acrylamide copolymer under salting liquid and high temperature, from point of polymer
Minor structure design angle sets out, and the method that people are usually taken mainly has：(1) being introduced on main polymer chain has big space
The polymer chain of steric hindrance, improves polymer chain rigidity；(2) interaction between polymer molecular chain is improved, to maintain it
Hydrodynamic volume under salting liquid and high temperature, prevents being greatly lowered for viscosity.However, the introducing of multifunctional monomer is crossed,
On the one hand the cost of product can be increased, on the other hand, often polymerization activity is poor for function monomer, thus causes the molecule of copolymer
Amount is relatively low, and its thickening property is not good, and this will improve the concentration of product.In addition, current main by between hydrophobic monomer
Association improves the interaction strength between polymer molecular chain, and the intensity of this heat resistance and salt tolerance is weaker, by temperature
The influence of degree is larger, meanwhile, the addition of excessive hydrophobic monomer will reduce the solute effect of polymer, influence the use of product.
Chinese patent document CN105085800A discloses a kind of preparation method of Heat Resistant and Salt Tolerant Polymer oil displacement agent, prepares
Method is as follows：Monomer, 3- acrylamidos -3 Methylbutanoic acid sodium by acrylamide, containing phenyl and Sulfonic acid structures are dissolved in
In ionized water, regulation pH be 6-10, by complexing agent of disodium ethylene diamine tetraacetate, urea be cosolvent, lauryl sodium sulfate
For solubilizer, from redox-azo Water Soluble Compound initiator, polymerisation is divided to two sections of progress, first paragraph reaction temperature
Spend for 5~10 DEG C, second segment reaction temperature is 40~70 DEG C, obtains temperature-resistant anti-salt oil displacement agent.
Chinese patent document CN105566565A discloses the hydrophobic association type temperature-resistant anti-salt that a kind of side chain contains double bond and gathered
The preparation method of compound, preparation method is as follows：By acrylamide, methacrylic acid, 2- acrylamide-2-methyl propane sulfonics, third
The reactant of olefin(e) acid octadecyl ester and mixed solvent first adjusts pH value with NaOH solution, then makes total monomer quality point in reaction system
Number is 10~30%；The acrylamide derivative hydrophobic monomer that the functional structure containing Capsaicin is added after lauryl sodium sulfate is added,
Logical N2Polymerisation is carried out afterwards and obtains new hydrophobic association polymer, and resulting polymers have application prospect in oil field development.
Above-mentioned patent realizes the lifting of polymer temperature-resistant anti-salt performance by introducing function monomer, in the process,
Often have the following disadvantages：Function monomer preparation process is cumbersome, there is the subsequent operations such as purification, adds product cost；With third
Acrylamide single phase ratio, function monomer polymerization activity is poor, and polymer molecular weight is not high, during use, it is necessary to polymer
Concentration is high；The introducing of hydrophobic type function monomer, interior salt form function monomer, reduces the solubility property of polymer, during use,
The dissolution time of polymer increases, the increase of insoluble matter ratio, influences using and promoting for product.
The content of the invention
It is an object of the invention to provide one kind containing silicate sturcture monomer and preparation method and application, prepared by the present invention
Method is simple；What is prepared is higher containing silicate sturcture monomer reactivity, it is easy to prepare high molecular weight products, thickening property is excellent
Good, product dosage is small when using.
A kind of preparation method containing silicate sturcture monomer that the present invention is provided, comprises the following steps：Silicic acid will be contained
The solution of ester structure monomer is added dropwise in aqueous silicate solution, hybrid reaction, obtains the aqueous solution containing silicate sturcture monomer,
Separation is obtained containing silicate sturcture monomer.
In above-mentioned preparation method, the solution of contained silicate structure monomer has to be dissolved in containing silicate structure monomer
The solution of machine solvent configuration；
The organic solvent includes at least one in n-hexane, hexamethylene, normal heptane, acetone, ether, ethyl acetate and benzene
Kind；
It is described to contain SiO in silicate structure monomer and the aqueous silicate solution3 2-Mol ratio can be 1：0.5~5,
It is preferred that 1：1~4.
In above-mentioned preparation method, the concentration of the solution containing silicate structure monomer can be 400~800g/L, excellent
Select 500~600g/L；
The concentration of the aqueous silicate solution can be 10~150g/L, preferably 20~100g L.
It is described to be selected from vinyltrimethoxy silane, vinyl containing silicate structure monomer in above-mentioned preparation method
In triethoxysilane, methacryloxypropyl trimethoxy silane and methacryloxypropyl
At least one；
The cation of silicate is selected from sodium and/or potassium in the aqueous silicate solution.
In the present invention, prepare the aqueous silicate solution and water is dissolved in using silicate, the silicate is commonly used in the art
Silicate ion salt, concretely Na2SiO3·9H2O、Na2SiO3·5H2O、Na2SiO3And K2SiO3In at least one
Kind.
In above-mentioned preparation method, the speed that the solution containing silicate structure monomer is added dropwise is 0.1~0.4mL/
Min, concretely 0.2mL/min, 0.1~0.2mL/min, 0.2~0.4mL/min or 0.15~0.35mL/min；
The temperature of the reaction is room temperature；
The time of the reaction can be 2~8h, preferably 3~5h.
In the present invention, the room temperature refers to 10~30 DEG C.
It is described to be hydrolyzed containing silicate structure monomer under the silicic acid salt action of alkalescence, it may be possible to single, two in the present invention
Individual or three silicate functional groups are hydrolyzed, therefore the obtained silicate sturcture monomer that contains is mixture.
Contain silicate sturcture monomer present invention also offers what above-mentioned preparation method was prepared.
Invention further provides the application containing silicate sturcture monomer in flooding polymers are prepared.
The aqueous solution containing silicate sturcture monomer obtained in preparation method of the present invention can be without isolating
State containing silicate sturcture monomer, directly prepare flooding polymers with the aqueous solution containing silicate sturcture monomer, can save
Go the operation of separating-purifying.
The aqueous solution containing silicate sturcture monomer is prepared and contained described in being obtained in the preparation method provided using the present invention
There are the flooding polymers of silicate sturcture, its preparation method comprises the following steps：
(1) in an inert atmosphere, the solution mixing by water-soluble monomer, water and containing silicate sturcture monomer, is mixed
Close liquid；
(2) sodium citrate, ferrous sulfate, tetramethylethylenediamine, 4,4'- azos are sequentially added in the mixed liquor double
(4- cyanopentanoic acids), ammonium persulfate and hydrogen peroxide mixing, reaction, that is, obtain the polymer containing silicate sturcture.
In above-mentioned preparation method, the water-soluble monomer includes acrylamide and remaining monomer；Remaining described monomer is
Vinyl pyrrolidone, PAA, 2- acrylamide-2-methylpro panesulfonic acids sodium, sodium vinyl sulfonate and styrene sulfonic acid
At least one of sodium.
In the present invention, the room temperature refers to 10~30 DEG C.
In above-mentioned preparation method, the inert atmosphere is blanket of nitrogen and/or argon atmospher；
The mass ratio containing silicate structure monomer and the water-soluble monomer can be 0.1~10：90~99.9；
The mass ratio of the acrylamide and remaining monomer can be 1~90：1；
It is described to be with the mass ratio of the water with the quality sum of the water-soluble monomer containing silicate structure monomer
1：0.5~15.
In above-mentioned preparation method, the temperature of mixing can be 5~10 DEG C in step (1), concretely 8 DEG C, pH value is 7~
10, concretely 8.5.
In above-mentioned preparation method, in step (2), the reaction includes following 1) -2) process：1) can be for 8 with temperature
~10 DEG C, concretely 8 DEG C or 10 DEG C, pH value is 7~10, concretely 8.5, reacts 1~10h, specifically react 4h, 6h, 4~
6h or 2~8h；2) temperature rises to 60~80 DEG C, and pH value can be 7~10, react 0.5~5h；Temperature can specifically rise to 60 DEG C, pH
Value can be 8.5, specifically react 1h, 1.5h, 1~5h or 1~4h.
In above-mentioned preparation method, the sodium citrate, the ferrous sulfate, the tetramethylethylenediamine, described 4,4'-
Azo double (4- cyanopentanoic acids), the ammonium persulfate, the hydrogen peroxide and the water-soluble monomer mass ratio can for 1~
30：0.2~5：0.5~10：30~300：1~10：0.1~5：105。
In above-mentioned preparation method, the mass ratio containing silicate structure monomer and the water-soluble monomer can be 1
~5：95~99, concretely 3:97、4.5:97th, 3~4.5:97 or 2~5:100；
The mass ratio of the acrylamide and remaining monomer can be 1~9：1, concretely 75:22、85:12 or 3~
7:1；
The mass ratio of the quality sum containing silicate structure monomer and the water-soluble monomer and the water is 1：1
~4, concretely 1:2.5、1.1:2.5th, 1~1.1：2.5 or 1：2~3.
In above-mentioned preparation method, the sodium citrate, the ferrous sulfate, the tetramethylethylenediamine, described 4,4'-
Azo double (4- cyanopentanoic acids), the ammonium persulfate, the hydrogen peroxide and the water-soluble monomer mass ratio can for 15~
30：0.5~3.5：1.5~5：40~100：3~7：.1~3.5：105, concretely 20:1.5:3:50:5:2.5:970000、
30:1.5:3:50:5:2.5:970000、20:1.5:2:70:5:2.5:970000th, 20~30:1.5:2~3:50~70:5:
2.5:970000 or 20~30：0.5~3.5：2~4：40~90：4~6：1.5~3.5：106。
In the preparation of flooding polymers of the present invention containing silicate sturcture, in addition to the flooding polymers are done
It is dry, crush the step of.
Present invention also offers above-mentioned preparation method prepare described in the flooding polymers containing silicate sturcture.
Flooding polymers of the present invention containing silicate sturcture are applied to as in oil displacement agent.
The present invention has advantages below：
(1) raw material of the present invention is easy to get, cheap, and preparation technology is simple, it is easy to operate.
(2) monomer reactivity of the present invention is higher, and good hydrophilic property, dissolution velocity is fast, it is easy to prepare high molecular weight products, tackifying
Can be excellent, product dosage is small when using.
Brief description of the drawings
Fig. 1 is that oil displacement experiment moisture content/recovery ratio of the polymer of the embodiment of the present invention 1 and the relation of solution injected slurry volume are bent
Line.
Embodiment
Experimental method used in following embodiments is conventional method unless otherwise specified.
Material, reagent used etc., unless otherwise specified, are commercially obtained in following embodiments.
Embodiment 1, temperature-resistant anti-salt flooding polymers of the preparation containing silicate sturcture
The temperature-resistant anti-salt flooding polymers containing silicate sturcture are prepared in accordance with the following steps：
(1) preparation containing silicate sturcture monomer
By 7.5g Na2SiO3·9H2O is dissolved in 50mL deionized waters, prepares sodium silicate aqueous solution.By 3g metering systems
Acryloxypropylethoxysilane trimethoxy silane is dissolved in 5mL n-hexanes, is then instilled in above-mentioned sodium silicate aqueous solution, and drop rate is
0.2mL/min.Completion of dropping.4h is stirred under solution room temperature (25 DEG C), the monomer solution containing silicate sturcture is obtained.
(2) preparation of the temperature-resistant anti-salt flooding polymers containing silicate sturcture
By 250g deionized waters, the monomer solution containing silicate sturcture, 75g acrylamides, 22g 2- acrylamides
Base -2- methyl propane sulfonic acid sodium is added in the wolf bottle equipped with agitator, logical nitrogen pipe and thermometer, is 8 by temperature control
DEG C, pH is adjusted to 8.5, stirs and is passed through nitrogen to water-soluble monomer and is completely dissolved, then sequentially add 2mg sodium citrates,
0.15mg ferrous sulfate, 0.3mg tetramethylethylenediamines, 5mg 4,4'- azos double (4- cyanopentanoic acids), 0.5mg ammonium persulfates and
0.25mg hydrogen peroxide, reacts 4h, then temperature is increased into 60 DEG C, reacts 1.5h, product is dried, crushed, is obtained containing silicon
The flooding polymers of hydrochlorate structure.
Embodiment 2, temperature-resistant anti-salt flooding polymers of the preparation containing silicate sturcture
It is identical with the preparation method of the embodiment of the present invention 1, except that the Na in step (1)2SiO3·9H2O dosages are
5g, obtains the flooding polymers containing silicate sturcture.
Embodiment 3, temperature-resistant anti-salt flooding polymers of the preparation containing silicate sturcture
It is identical with the preparation method of the embodiment of the present invention 1, except that the methacryloxypropyl three in step (1)
Methoxy silane dosage is 4.5g, Na2SiO3·9H2O dosages are 10g, obtain the flooding polymers containing silicate sturcture.
Embodiment 4, temperature-resistant anti-salt flooding polymers of the preparation containing silicate sturcture
It is identical with the preparation method of the embodiment of the present invention 1, except that monomer is vinyl triethoxyl silicon in step (1)
Alkane, obtains the flooding polymers containing silicate sturcture.
Embodiment 5, temperature-resistant anti-salt flooding polymers of the preparation containing silicate sturcture
It is identical with the preparation method of the embodiment of the present invention 1, except that acrylamide dosage is 85g, 2- third in step (2)
Acrylamide base -2- methyl propane sulfonic acids sodium is 12g, obtains the flooding polymers containing silicate sturcture.
Embodiment 6, temperature-resistant anti-salt flooding polymers of the preparation containing silicate sturcture
It is identical with the preparation method of the embodiment of the present invention 1, except that remaining monomer is styrene sulfonic acid in step (2)
Sodium, obtains the flooding polymers containing silicate sturcture, obtains the flooding polymers containing silicate sturcture.
Embodiment 7, temperature-resistant anti-salt flooding polymers of the preparation containing silicate sturcture
It is identical with the preparation method of the embodiment of the present invention 1, except that remaining monomer is vinyl sulfonic acid in step (2)
Sodium, obtains the flooding polymers containing silicate sturcture.
Embodiment 8, temperature-resistant anti-salt flooding polymers of the preparation containing silicate sturcture
It is identical with the preparation method of the embodiment of the present invention 1, except that sodium citrate dosage is 3mg, sulfuric acid in step (2)
Ferrous dosage is 0.2mg, obtains the flooding polymers containing silicate sturcture.
Embodiment 9, temperature-resistant anti-salt flooding polymers of the preparation containing silicate sturcture
It is identical with the preparation method of the embodiment of the present invention 1, except that tetramethylethylenediamine dosage is in step (2)
0.2mg, double (4- cyanopentanoic acids) dosages of 4,4'- azos are 7mg, obtain the flooding polymers containing silicate sturcture.
Embodiment 10, temperature-resistant anti-salt flooding polymers of the preparation containing silicate sturcture
Identical with the preparation method of the embodiment of the present invention 1, except that (2) 10 DEG C of reaction time of step are 6h, 60 DEG C anti-
It is 1h between seasonable, obtains the flooding polymers containing silicate sturcture.
Comparative example 1, prepare flooding polymers
It is identical with the preparation method of the embodiment of the present invention 1, except that not adding the monomer containing silicate sturcture.
Comparative example 2, certain flooding polymers
Comparative example 2 is certain Oil Field flooding polymers (Tianjin Bo Hong petrochemical industries Co., Ltd, BHKY-3).
The embodiment of the present invention and comparative example properties of product are evaluated：
With the polymer solution that mineralized water prepared polymer concentration is 0.2%, stirred 20 seconds with the gear of WARRING agitators 1,
Under conditions of 90 DEG C, aging 90 days is tested with Brookfield DV3T types viscosimeter and shears polymer before and after front and rear, aging
The viscosity of solution, test temperature is 90 DEG C, and test rotating speed is 6r/min.The composition of mineralized water as shown in table 1, comment by anti-shear performance
As shown in table 2, high-temperature aging resisting Evaluation results are as shown in table 3 for valency result.From table 2-3, preparation method of the present invention is obtained
To the flooding polymers containing silicate sturcture have anti-shearing, anti-aging the characteristics of.
The mineralized water of table 1 is constituted
The anti-shear performance evaluation result of table 2
The high-temperature aging resisting Evaluation results of table 3
The polymer prepared using the embodiment of the present invention 1 carries out improving recovery ratio laboratory experiment, oil displacement experiment moisture content/adopt
The relation curve of yield and solution injected slurry volume is as shown in Figure 1.Obtained polymer is configured to 0.2% polymerization with mineralized water
Thing solution, (fill out sand tube sectional area 4.91cm in one-dimensional sandpack column is injected by the solution2, length 30cm) and initial oil saturation
For 75%, water drive is to moisture content 98%, and (crude oil used is in 90 DEG C, shear rate 7.34s-1Under the conditions of viscosity be 61.5mPas)
Injection rate is 1mL/min, and after the aqueous solutions of polymers for injecting 0.35PV, continuation water drive to moisture content reaches 98%, measures
Recovery ratio improves 19.6%.
Claims (9)
1. a kind of preparation method containing silicate sturcture monomer, comprises the following steps：The molten of silicate structure monomer will be contained
Drop is added in aqueous silicate solution, hybrid reaction, obtains the aqueous solution containing silicate sturcture monomer, and separation is contained
Silicate sturcture monomer.
2. preparation method according to claim 1, it is characterised in that：The solution containing silicate structure monomer be containing
There is silicate structure monomer to be dissolved in the solution of organic solvent configuration；The organic solvent include n-hexane, hexamethylene, normal heptane,
At least one of acetone, ether, ethyl acetate and benzene.
3. preparation method according to claim 1 or 2, it is characterised in that：It is described containing silicate structure monomer with it is described
SiO in aqueous silicate solution3 2-Mol ratio be 1：0.5~5.
4. the preparation method according to any one of claim 1-3, it is characterised in that：It is described to contain silicate structure monomer
Solution concentration be 400~800g/L；
The concentration of the aqueous silicate solution is 10~150g/L.
5. the preparation method according to any one of claim 1-4, it is characterised in that：It is described to contain silicate structure monomer
Selected from vinyltrimethoxy silane, VTES, methacryloxypropyl trimethoxy silane and first
At least one of base acryloxypropyl triethoxysilane；
The cation of silicate is selected from sodium and/or potassium in the aqueous silicate solution.
6. the preparation method according to any one of claim 1-5, it is characterised in that：It is described to contain silicate structure monomer
Solution be added dropwise speed be 0.1~0.4mL/min.
7. the preparation method according to any one of claim 1-6, it is characterised in that：The temperature of the reaction is room temperature；
The time of the reaction is 2~8h.
What 8. the preparation method any one of claim 1-7 was prepared contains silicate sturcture monomer.
9. the application described in claim 8 containing silicate sturcture monomer in flooding polymers are prepared.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111662408A (en) * | 2020-07-14 | 2020-09-15 | 中海石油(中国)有限公司 | Oil displacement system suitable for high-temperature high-salt oil reservoir |
| WO2021045136A1 (en) * | 2019-09-06 | 2021-03-11 | 株式会社カネカ | Water-soluble (meth)acrylic resin and use thereof |
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