CN105085838A - Preparation method of modified nanometer SiO2-AA-AM copolymer - Google Patents
Preparation method of modified nanometer SiO2-AA-AM copolymer Download PDFInfo
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- CN105085838A CN105085838A CN201410750934.7A CN201410750934A CN105085838A CN 105085838 A CN105085838 A CN 105085838A CN 201410750934 A CN201410750934 A CN 201410750934A CN 105085838 A CN105085838 A CN 105085838A
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Abstract
The invention relates to a preparation method of a modified nanometer SiO2-AA-AM copolymer. The preparation method comprises that a modified nanometer SiO2 functional nanometer, acrylamide and acrylic acid are mixed, pH of the mixed solution is adjusted to 6.0-7.5 by sodium hydroxide, distilled water is added into the mixed solution so that an aqueous solution with the monomer total mass concentration of 20.0-26.0% is obtained, an initiator is added into the aqueous solution, the mixed solution undergoes a reaction at a temperature of 36.0-42.0 DEG C in a nitrogen protective atmosphere to produce a reaction product, and the reaction product is washed, crushed and dried to form the copolymer. The nanometer SiO2 is introduced into the copolymer, and an amino group is connected to the surface of the nanometer SiO2 so that a double bond is connected to the surface of the nanometer SiO2 and thus the nanometer SiO2, acrylic acid and acrylamide undergo a polymerization reaction to produce the copolymer. The copolymer has a spatial network structure. Through control of a modification degree of the surface of a modified nanometer SiO2 functional monomer, copolymer viscosity-increasing performances are improved.
Description
Technical field
The present invention relates to technical field prepared by polymer materials, more particularly, the present invention relates to a kind of modified Nano SiO
2the preparation method of-AA-AM multipolymer.
Background technology
Oil, as Nonrenewable resources, has very important critical role in the fields such as industry, national defence.In order to improve mining term, the raising field output in oil field, employing polymer flooding is an important technology.Polymer flooding refers to and adds a small amount of polymkeric substance at injection water, relies on to increase aqueous viscosity and reduce reservoir permeability to play and improve sweep efficiency and improve the effect of recovery ratio.At present, polymer flooding enters industrialization phase in the Daqing oil field of China, Shengli Oil Field, Dagang Oilfield, Jilin Oil Field, Henan Oil Field, obtains good oil increasing effect.
At present, the widely used polymkeric substance of polymer flooding is polyacrylamide and derivative thereof.This base polymer desirable oil increasing effect can be obtained for when low temperature, low mineralization oil reservoir, but for during high temperature and high salinity oil reservoir, it improves recovery ratio effect and significantly reduces.Hyperbranched polymer has stronger anti-shear ability, can set up higher resistance coefficient and residual resistance factor in porous medium.At present, main organism is that kernel carrys out synthesis of super branched polymkeric substance, and the side chain number of synthesized hyperbranched polymer is less.Although can be increased the number of side chain by the algebraically increasing organism kernel, the algebraically of kernel is higher, and molecular dimension will be larger, and the injection of hyperbranched polymer is poorer; In addition, the algebraically of kernel is higher, and side reaction is more, and the alignment degree of kernel will be difficult to control, even if adopt a series of Separation & Purification technology can obtain more regular kernel, but the production cost of kernel also can be very high.
Summary of the invention
In order to solve the above-mentioned technical problem existed in prior art, the object of the present invention is to provide a kind of modified Nano SiO
2the preparation method of-AA-AM multipolymer.
To achieve these goals, present invention employs following technical scheme:
A kind of modified Nano SiO
2the preparation method of-AA-AM multipolymer, is characterized in that described preparation method comprises the following steps: (1) is by modified Nano SiO
2function monomer, acrylamide and vinylformic acid mix, and with sodium hydroxide adjust ph to 6.0 ~ 7.5, add distilled water and be made into the aqueous solution that monomer total mass concentration is 20.0 ~ 26.0%; Add initiator, logical nitrogen protection, reacts under temperature is 36.0 ~ 42.0 DEG C of conditions; Reaction product can obtain described multipolymer after washing, pulverizing, drying.
Wherein, the structural formula of described multipolymer is as follows:
Wherein, described initiator is the mixture of ammonium persulphate and sodium bisulfite, and the mol ratio of the two is 1: 1.
Wherein, the quality of described initiator is 0.10 ~ 0.30wt% of described monomer total mass.
Wherein, in described monomer, acrylamide and acrylic acid mass ratio are 1.86 ~ 4.00, modified Nano SiO
2the content of function monomer is 0.1 ~ 0.8wt%.
Wherein, described modified Nano SiO
2function monomer adopts the method comprised the following steps to prepare: (1) utilizes Nano-meter SiO_2
2with 3-aminopropyl triethoxysilane in the anhydrous toluene solution of 80 ~ 100 DEG C, reaction more than 12h obtains amino modified Nano-meter SiO_2
2, and control Nano-meter SiO_2 by the addition of control 3-aminopropyl triethoxysilane
2the content of surface amino groups; (2) excessive MALEIC ANHYDRIDE and amino modified Nano-meter SiO_2 is utilized
2be obtained by reacting the modified Nano SiO with carbon-carbon double bond
2function monomer.
Wherein, following operation is comprised in step (2): 1. in DMF solution, add MALEIC ANHYDRIDE, stirring and dissolving obtains mixing solutions completely; 2. at amino modified Nano-meter SiO_2
2in add DMF and stir and obtain dispersion liquid; 3. be then added in the mixing solutions that 1. operation obtain by operating the dispersant liquid drop that 2. obtains, then complete at 70 ~ 80 DEG C of stirring reactions, the reaction product obtained through washing, filter, the modified Nano SiO with carbon-carbon double bond can be grafted with after drying
2.
Wherein, described amino modified Nano-meter SiO_2
2surface amino groups molar weight is Nano-meter SiO_2 before modified
225 ~ 40% of surface hydroxyl molar weight.
Compared with prior art, terpolymer oil-displacing agent of the present invention has following beneficial effect:
Multipolymer of the present invention is by Nano-meter SiO_2
2be incorporated in multipolymer, at Nano-meter SiO_2
2surface connects amino and then connects double bond, and make itself and vinylformic acid and acrylamide polymerization, the multipolymer synthesized has spacial framework, and by controlling modified Nano SiO
2the modification degree on function monomer surface optimizes the increasing stickiness energy of multipolymer.
Accompanying drawing explanation
Fig. 1 is Nano-meter SiO_2
2modification degree increases the impact of stickiness energy to multipolymer.
Fig. 2 is modified Nano SiO
2the infrared line of-AM-AA multipolymer.
Fig. 3 is the hydrogen spectrum of copolymer 1.
Fig. 4 is the hydrogen spectrum of multipolymer 2.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearly understand, below in conjunction with drawings and Examples, the present invention is described in further detail.Should be appreciated that specific embodiment described herein only for setting forth technical scheme of the present invention, and be not used in the protection domain limiting invention.
Embodiment 1 modified Nano SiO
2the preparation of function monomer
Modified Nano SiO described in the present embodiment
2function monomer adopts the method comprised the following steps to prepare: (1) utilizes Nano-meter SiO_2
2with 3-aminopropyl triethoxysilane (KH540) in the anhydrous toluene solution of 80 DEG C, reaction 12h obtains amino modified Nano-meter SiO_2
2, and control Nano-meter SiO_2 by the addition of control 3-aminopropyl triethoxysilane
2the content of surface amino groups; (2) excessive MALEIC ANHYDRIDE and amino modified Nano-meter SiO_2 is utilized
2be obtained by reacting the modified Nano SiO with carbon-carbon double bond
2function monomer.Following operation is comprised: 1. in DMF solution, add MALEIC ANHYDRIDE, stirring and dissolving obtains mixing solutions completely in step (2); 2. at amino modified Nano-meter SiO_2
2in add DMF and stir and obtain dispersion liquid; 3. be added in the mixing solutions that 1. operation obtain by operating the dispersant liquid drop that 2. obtains, then complete at 75 DEG C of stirring reactions, the reaction product obtained through washing, filter, the modified Nano SiO with carbon-carbon double bond can be grafted with after drying
2.Wherein, hydrochloric acid-ethanol nonaqueous titrations can be utilized in step (2) to judge amino modified Nano-meter SiO_2
2whether the amino on surface reacts completely.Grignard reagent titration measuring Nano-meter SiO_2 was adopted before the reaction of step (1)
2surface hydroxyl quantity, and measure Nano-meter SiO_2 by hydrochloric acid-ethanol nonaqueous titrations after reacting
2the content of surface amino groups.The Nano-meter SiO_2 of different modification degree can be prepared by embodiment 1
2function monomer (can utilize amino modified Nano-meter SiO_2
2the molar weight of surface amino groups accounts for Nano-meter SiO_2 before modified
2the per-cent of the molar weight of surface hydroxyl represents).
Embodiment 2 modified Nano SiO
2the preparation of-AA-AM multipolymer
The modified Nano SiO of the present embodiment
2the preparation method of-AA-AM multipolymer, comprises the following steps: (1) is by modified Nano SiO
2function monomer, acrylamide and vinylformic acid mix, and by sodium hydroxide adjust ph to 7.0, add distilled water and be made into the aqueous solution that monomer total mass concentration is 25.0%; When temperature is increased to 40 DEG C, add initiator, logical nitrogen protection, reacts under temperature is 40.0 DEG C of conditions; Reaction product can obtain described multipolymer after washing, pulverizing, drying.Wherein, the quality of initiator is the 0.20wt% of described monomer total mass, and described initiator is the mixture of ammonium persulphate and sodium bisulfite, and the mol ratio of the two is 1: 1.In described monomer, acrylamide and acrylic acid mass ratio are 3.2, modified Nano SiO
2the content of function monomer is 0.50wt%.By using the Nano-meter SiO_2 of different modification degree
2function monomer prepares different multipolymers to investigate its impact on performance of copolymer.Take the copolymer powder obtained, the polymers soln that concentration is 2000mg/L is mixed with respectively with deionized water and 5000mg/L sodium chloride solution, 20s is sheared with agitator (3600r/min), then at 70.0 DEG C, measure the Polymer Solution Viscosity after shearing with BrookfiledDV-III viscosmeter, result as shown in Figure 1.As shown in Figure 1, Nano-meter SiO_2
2modification degree when being 30% and 35%, with the copolymer solution of deionized water and the preparation of 5000mg/L sodium chloride solution, there is after shearing higher viscosity, work as Nano-meter SiO_2 as seen
2modification degree when being 30% and 35%, synthesized multipolymer has and better increases stickiness energy.
Modified Nano SiO
2the sign of-AA-AM multipolymer
1. Infrared spectroscopy
1. the polymkeric substance vacuum-drying 48h at 40.4 DEG C will synthesized; 2. take a morsel dried KBr, uses infrared tabletting machine; 3. Infrared spectrum scanning is carried out, acquisition instrument background with WQF-520 type infrared spectrometer; 4. take a morsel polymer samples, mixes after adding KBr, and the mass ratio of KBr and sample is about 50: 1; 5. the infrared tabletting machine of the KBr being added with sample; 6. the sample strip WQF-520 type infrared spectrometer made is carried out Infrared spectrum scanning.Modified Nano SiO
2-AM-AA copolymer 1 (Nano-meter SiO_2
2modification degree be 30%) and multipolymer 2 (Nano-meter SiO_2
2modification degree be 35%) infrared spectrum as shown in Figure 2.At 3409.2cm
-1neighbouring absorption peak is the characteristic peak of hydroxyl; At 2931.4cm
-1neighbouring absorption peak is the characteristic peak of methylene radical; At 1653.8cm
-1neighbouring absorption peak is the characteristic peak of carbonyl; At 1112.1cm
-1neighbouring absorption peak is the asymmetric stretching vibration peak of Si-O-Si, at 769.2cm
-1neighbouring absorption peak is the symmetrical stretching vibration peak of Si-O-Si.Above result shows to have synthesized subject copolymers.
2. nuclear magnetic resonance spectroscopy
1. the multipolymer synthesized is joined in nuclear magnetic tube; 2. in nuclear magnetic tube, add heavy water, be placed to and dissolve completely; 3. by the hydrogen spectrum of BrukerAC-E200 nuclear magnetic resonance spectrometer scanning product, frequency is 200Hz.Modified Nano SiO
2-AM-AA copolymer 1 (Nano-meter SiO_2
2modification degree be 30%) and multipolymer 2 (Nano-meter SiO_2
2modification degree be 35%) hydrogen spectrum respectively as shown in Figure 3 and Figure 4,1.5ppm is-CH
2-CH (COONa)-,-CH
2-CH (CONH
2-CH (COONa)-CH)-, (CONH-)-,-CH
2-CH
2-CH
2the chemical shift of-NH-proton; 2.1ppm is-CH
2-CH (COONa)-,-CH
2-CH (CONH
2the chemical shift of-CH (COONa)-CH)-, (CONH-)-proton; 3.4ppm is-CH
2-CH
2-CH
2the chemical shift of-NH-proton.Above result shows to have synthesized subject copolymers.
3. the absolute weight average molecular of multipolymer measures
Static light scattering measures molecular weight of copolymer
(1) experimental procedure of static light scattering
1. with the polymers soln of 0.8 μm of membrane filtration preparation, carry out dust removal process to polymers soln, obtained sample, places 24h; 2. open BI-200SM extensive angle dynamic/static laser light scattering instrument and water-bath (25.0 DEG C), and allow instrument more than preheating 30min; 3. open treater and laser transmitter, if find that impurity is more, opened frit impurity to meeting requirement of experiment, and adjusts laser intensity; 4., after preparation work completes, adopt toluene as calibration solution, and deduct the impact of solvent, the polymers soln sample then putting into different concns is successively tested.
(3) molecular weight of multipolymer
With 0.8 μm of membrane filtration deionized water, dust removal process is carried out to deionized water; Again with the deionized water through dust removal process prepare a series of different concns (30,40,50,60,70mg/L) polymers soln, then use 0.8 μm of membrane filtration dedusting.Polymkeric substance is AA/AM multipolymer (HPAM), modified Nano SiO
2-AM-AA copolymer 1 and multipolymer 2.At 25.0 DEG C, by absolute weight average molecular and the cyclotron radius of static light scattering measuring polymkeric substance, utilize dual extrapotation, when the concentration of incident angle of light and polymers soln all level off to zero time, the inverse of the intersection point on Zimm figure is the absolute weight average molecular of multipolymer.Absolute weight average molecular and the cyclotron radius of multipolymer the results are shown in Table 1.
Table 1
| Polymkeric substance | Cyclotron radius (nm) | Absolute weight average molecular (10 7g/mol) |
| HPAM | 129 | 1.24 |
| Copolymer 1 | 98 | 0.98 |
| Multipolymer 2 | 95 | 0.95 |
Claims (8)
1. a modified Nano SiO
2the preparation method of-AA-AM multipolymer, is characterized in that described preparation method comprises the following steps: (1) is by modified Nano SiO
2function monomer, acrylamide and vinylformic acid mix, and with sodium hydroxide adjust ph to 6.0 ~ 7.5, add distilled water and be made into the aqueous solution that monomer total mass concentration is 20.0 ~ 26.0%; Add initiator, logical nitrogen protection, reacts under temperature is 36.0 ~ 42.0 DEG C of conditions; Reaction product can obtain described multipolymer after washing, pulverizing, drying.
2. modified Nano SiO according to claim 1
2the preparation method of-AA-AM multipolymer, is characterized in that the structural formula of described multipolymer is as follows:
3. modified Nano SiO according to claim 1
2the preparation method of-AA-AM multipolymer, is characterized in that: described initiator is the mixture of ammonium persulphate and sodium bisulfite, and the mol ratio of the two is 1: 1.
4. modified Nano SiO according to claim 3
2the preparation method of-AA-AM multipolymer, is characterized in that: the quality of described initiator is 0.10 ~ 0.30wt% of described monomer total mass.
5. modified Nano SiO according to claim 1
2the preparation method of-AA-AM multipolymer, is characterized in that: in described monomer, acrylamide and acrylic acid mass ratio are 1.86 ~ 4.00, modified Nano SiO
2the content of function monomer is 0.1 ~ 0.8wt%.
6. modified Nano SiO according to claim 1
2the preparation method of-AA-AM multipolymer, is characterized in that: described modified Nano SiO
2function monomer adopts the method comprised the following steps to prepare: 1) utilize Nano-meter SiO_2
2with 3-aminopropyl triethoxysilane in the anhydrous toluene solution of 80 ~ 100 DEG C, reaction more than 12h obtains amino modified Nano-meter SiO_2
2, and control Nano-meter SiO_2 by the addition of control 3-aminopropyl triethoxysilane
2the content of surface amino groups; 2) excessive MALEIC ANHYDRIDE and amino modified Nano-meter SiO_2 is utilized
2be obtained by reacting the modified Nano SiO with carbon-carbon double bond
2function monomer.
7. modified Nano SiO according to claim 6
2the preparation method of-AA-AM multipolymer, is characterized in that: in step 2) comprise following operation: 1. in DMF solution, add MALEIC ANHYDRIDE, stirring and dissolving obtains mixing solutions completely; 2. at amino modified Nano-meter SiO_2
2in add DMF and stir and obtain dispersion liquid; 3. be then added in the mixing solutions that 1. operation obtain by operating the dispersant liquid drop that 2. obtains, then complete at 70 ~ 80 DEG C of stirring reactions, the reaction product obtained through washing, filter, the modified Nano SiO with carbon-carbon double bond can be grafted with after drying
2.
8. modified Nano SiO according to claim 7
2the preparation method of-AA-AM multipolymer, is characterized in that: described amino modified Nano-meter SiO_2
2surface amino groups molar weight is Nano-meter SiO_2 before modified
225 ~ 40% of surface hydroxyl molar weight.
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| CN111406754A (en) * | 2020-04-28 | 2020-07-14 | 浙江禾本科技股份有限公司 | Hexythiazox water suspending agent and preparation method thereof |
| CN111548782A (en) * | 2020-04-30 | 2020-08-18 | 长江大学 | Nano-enhanced supermolecule clean fracturing fluid and preparation method thereof |
| 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 |
| CN113185657A (en) * | 2021-03-31 | 2021-07-30 | 宁波锋成先进能源材料研究院有限公司 | Nano material and preparation method and application thereof |
| CN114592689A (en) * | 2022-02-11 | 2022-06-07 | 瑞洲建设集团有限公司 | Fabricated building construction method |
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| CN111548782B (en) * | 2020-04-30 | 2023-01-24 | 长江大学 | Nano-enhanced supermolecule clean fracturing fluid and preparation method thereof |
| 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 |
| CN113185657A (en) * | 2021-03-31 | 2021-07-30 | 宁波锋成先进能源材料研究院有限公司 | Nano material and preparation method and application thereof |
| CN114592689A (en) * | 2022-02-11 | 2022-06-07 | 瑞洲建设集团有限公司 | Fabricated building construction method |
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Application publication date: 20151125 |