CN110041904B - Humic acid and alkylamine compound type thick oil viscosity reducer and preparation method and application thereof - Google Patents
Humic acid and alkylamine compound type thick oil viscosity reducer and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a humic acid and alkylamine compound thick oil viscosity reducer and a preparation method and application thereof. The viscosity reducer for thickened oil provided by the invention consists of two effective components. The effective component I is sodium humate polycondensate (HA) N, and the effective component II is polyacrylic acyloxy ethyl-N, N, N-dimethyl ammonium bromide (ASC). The viscosity reducing rate of the high-efficiency thick oil viscosity reducer reaches more than 80 percent at 40 ℃, 60 ℃ and 80 ℃, in particular to (HA)nWhen the mass ratio of (n-25) to ASC (n is about 500) is 5:5, the viscosity reduction rate at 40 ℃, 60 ℃ and 80 ℃ is 90.86%, 95.62% and 98.63% respectively, which shows that the heavy oil viscosity reducer of the invention has good heavy oil viscosity reduction performance under the conditions of higher temperature and mineralization degree.
Description
Technical Field
The invention belongs to the technical field of petroleum processing, and particularly relates to a humic acid and alkylamine compound thick oil viscosity reducer as well as a preparation method and application thereof.
Background
With the reduction of the recoverable reserves of light oil and the improvement of oil exploitation technology, the proportion of heavy oil is continuously increased. The thickened oil is a complex mixture rich in asphaltene and colloid, and has the characteristics of high viscosity, small oil-water density difference, poor liquidity and the like. The colloid and asphaltene in the thickened oil have surface activity, and when the thickened oil is mixed with formation water, the viscosity of the thickened oil is easily increased due to emulsification. Therefore, the viscosity reduction of the thick oil is an indispensable link in the oil field production.
The chemical viscosity reduction technology is one of the most economic measures for reducing the viscosity of the thick oil at present, and is widely used in various thick oil fields. The chemical viscosity reducer can effectively disperse and emulsify the thick oil, obviously reduce the viscosity of the thick oil and reduce the flow resistance of the thick oil in a stratum and a shaft, and has important significance for reducing the energy consumption in the exploitation process, reducing the emission pollution and improving the recovery ratio of the thick oil.
Humic Acid (HA) is a product of natural plant residues after decomposition, is a complex natural macromolecular organic matter, contains a plurality of active functional groups such as carbonyl, carboxyl, alcoholic hydroxyl and phenolic hydroxyl in molecules, and HAs acidity, hydrophilicity, interfacial activity, cation exchange capacity, complexation and adsorption and dispersion capacities, so that humic acid substances have wide application in the fields of environmental protection, oil exploitation, agriculture, forestry and horticulture, medicine, analytical chemistry, battery industry and the like.
Disclosure of Invention
The invention aims to provide a humic acid and alkylamine compound thick oil viscosity reducer and a preparation method and application thereof.
The active ingredients of the thick oil viscosity reducer provided by the invention comprise polymers shown in a formula a and a formula c;
in the formula a, HA is sodium humate;n is 1 to 100; specifically 25-75, 25-50, 50-75, 25, 50 or 75; the polymer represented by formula a is abbreviated as (HA)n；
The structural formula of the sodium humate can be shown as a formula b, and the sodium humate is obtained by reacting humic acid with sodium hydroxide; at present, the universally accepted international humic acid two-dimensional structure model is a Stevenson structure model, and the structural formula of the product obtained by reacting the Stevenson structure model with sodium hydroxide is shown as a formula b.
The polymer represented by formula a is sodium humate polycondensate (HA)nCan be prepared by the following method: with triphenyl phosphine (PPh)3) And diethyl azodicarboxylate (DEAD) as catalyst, and under the action of concentrated sulfuric acid, the sodium humate is subjected to polycondensation reaction at 50-180 ℃ for 3-10 hours to obtain the sodium humate.
In the formula c, R is- (CH)2)XCH3X is an integer of 5 to 22; m is 5 to 1000, and specifically can be 100-. The polymer shown in the formula c is called ASC for short;
the thick oil viscosity reducer also comprises a solvent.
Specifically, the solvent is at least one selected from water, methanol and ethanol.
In the thick oil viscosity reducer, the mass ratio of the polymers shown in the formulas a and c is 20-50: 50-80 parts; specifically (3-5) to (5-7); more specifically, it may be 3:7, 4:6 or 5: 5.
Specifically, the thick oil viscosity reducer consists of polymers shown in a formula a and a formula c and the solvent.
In the viscosity reducer, the polymers shown in the formula a and the formula c account for 40-60% of the total mass of the thick oil viscosity reducer;
the polymer shown in the formula a accounts for 20-50% of the total mass of the polymers shown in the formula a and the formula c; in particular 30 to 50 percent;
the polymer shown in the formula c accounts for 50-80% of the total mass of the polymers shown in the formula a and the formula c; in particular 50 to 70 percent.
The molar ratio of the total mass of the polymer represented by formula a and the polymer represented by formula c to the solvent may specifically be 5: 2.
The method for preparing the thick oil viscosity reducer comprises the following steps: and (3) uniformly mixing the polymers shown in the formulas a and c and a solvent to obtain the polymer.
The method may further comprise: before the blending step, acidifying the polymer of formula a with sulfuric acid to make it positively charged.
In addition, the application of the thick oil viscosity reducer provided by the invention in thick oil exploitation also belongs to the protection scope of the invention. Specifically, in the process of thick oil exploitation, the use temperature of the thick oil viscosity reducer is 40-80 ℃;
the volume ratio of the thickened oil viscosity reducer to the thickened oil is 1: 0.5-10; specifically 1: 1;
the thick oil viscosity reducer is diluted before use.
In the diluting step, the diluent is seawater; the concentration after dilution is 500mg/L-2500 mg/L.
The polymer of formula c, namely polyacryloyloxyethyl-N, N, N-dimethylalkylammonium bromide (ASC), can be prepared as follows:
1) reacting bromoalkane (R-Br, wherein R is- (CH)2)XCH3X is an integer of 5-22) and N, N-dimethylaminoethyl acrylate in a solvent, and obtaining a product M after rotary evaporation, filtration and recrystallization;
2) the product M is polymerized to give the polyacryloyloxyethyl-N, N, N-dimethylalkylammonium bromide (ASC).
Wherein, in the step 1), the molar ratio of the alkyl bromide to the N, N-dimethylaminoethyl acrylate is 1: 0.5-1.
In the reaction step, the temperature is 30-50 ℃ and the time is 2-36 hours.
In the step 2), the temperature is 50-80 ℃ and the time is 2-6 hours in the polymerization reaction step; the polymerization system is redox initiation system ammonium persulfate and ferrous ammonium sulfate; the mass ratio of the oxidant to the reducing agent is 1.2-2: 1; specifically 1.2:1, 1.5:1 or 2: 1; the polymerization is carried out in water and an inert atmosphere; the inert atmosphere is specifically a nitrogen atmosphere.
The efficient thick oil viscosity reducer provided by the invention has good interface participation capacity and viscosity reduction effect, enters between colloid and asphaltene flaky molecules by virtue of strong permeation and dispersion effects, partially disassembles an aggregate formed by plane overlapping and stacking, and forms an aggregate which is formed by the colloid, the asphaltene molecules and the viscosity reducer molecules and has a random stacking and a loose structure, so that the viscosity of thick oil is reduced. Experimental data show that the viscosity reduction rate of the high-efficiency thick oil viscosity reducer reaches more than 80% at 40 ℃, 60 ℃ and 80 ℃, in particular to (HA)nWhen the mass ratio of (n-25) to ASC (m is about 500) is 5:5, the viscosity reduction rate at 40 ℃, 60 ℃ and 80 ℃ is 90.86%, 95.62% and 98.63% respectively, which shows that the heavy oil viscosity reducer of the invention has good heavy oil viscosity reduction performance under the conditions of higher temperature and mineralization degree.
Detailed Description
The present invention will be further illustrated with reference to the following specific examples, but the present invention is not limited to the following examples. The method is a conventional method unless otherwise specified. The starting materials are commercially available from the open literature unless otherwise specified.
The polymer of formula a used in the following examples, namely, the sodium humate polycondensate (HA)nIs prepared by the following steps: mixing sodium humate and triphenyl phosphorus (PPh)3) And diethyl azodicarboxylate (DEAD) are added into a water separator containing a certain amount of toluene, reflux is carried out for water separation, concentrated sulfuric acid is slowly dripped into the mixture through a constant-pressure dropping funnel, the mixture is stirred at the temperature of 60 ℃ for 1 hour, then the temperature is raised to 180 +/-5 ℃, and the reaction is terminated after 3 hours. Filtering, washing with water, separating, recrystallizing to obtain condensed polymer (HA)nThe degree of condensation is 2 to 100.
In particular, with a degree of condensation of 25 (HA)nIs prepared by the following steps: 24.16g of sodium humate and 5.4g of triphenyl phosphine (PPh)3) 2.173g diethyl azodicarboxylate (DEAD) is added into a water separator containing 100mL toluene, reflux is carried out to separate water, concentrated sulfuric acid is slowly counted by a constant pressure dropping funnel, the total volume is 30mL, the mixture is stirred at the temperature of 60 ℃ for 1 hour, then the temperature is raised to 180 +/-5 ℃, the reaction is terminated after 3 hours of reaction. Filtration, washing with water, separation, recrystallization to give (HA) having a degree of condensation of 25n。
Degree of condensation 50 (HA)nIs prepared by the following steps: 30.16g of sodium humate and 1.3g of triphenyl phosphine (PPh)3) And 4.773g of diethyl azodicarboxylate (DEAD) were added to a water separator containing 100mL of toluene, water was separated by refluxing, concentrated sulfuric acid was slowly metered through a constant pressure dropping funnel, 30mL in total, stirred at 60 ℃ for 1 hour, then heated to 180. + -. 5 ℃ and reacted for 3 hours, and then terminated. Filtering, washing with water, separating, recrystallizing to obtain (HA) with condensation degree of 50n。
Degree of condensation 75 (HA)nIs prepared by the following steps: 38.261g of sodium humate, 5.71g of triphenyl phosphine (PPh)3) And 8.682g of diethyl azodicarboxylate (DEAD) were added to a water separator containing 200mL of toluene, water was separated by refluxing, concentrated sulfuric acid was slowly metered through a constant pressure dropping funnel, 30mL in total, stirred at 60 ℃ for 1 hour, then heated to 180. + -. 5 ℃, and the reaction was terminated after 5 hours. Filtration, washing with water, separation, recrystallization to give (HA) having a degree of condensation of 75n。
The polymer of formula c used in the following examples, namely polyacryloyloxyethyl-N, N, N-dimethylalkylammonium bromide (ASC), was prepared by the following procedure:
(1) mixing N, N-dimethylaminoethyl acrylate and bromoalkane according to the molar ratio of 1:1, dissolving in 100mL acetone, adding hydroquinone accounting for 0.5% of the mass of the bromoalkane, stirring for 24 hours at 35-40 ℃, adding KI accounting for 4% of the mass of the bromoalkane, continuing to react for 72 hours, evaporating part of acetone under reduced pressure, adding excessive diethyl ether into the reaction liquid to separate out solid, filtering out the solid, evaporating the solvent after obtaining the filtrate, repeatedly washing with diethyl ether for 3 times, collecting the filtrate, and evaporating the solvent under reduced pressure to obtain the product (M).
(2) Adding a certain amount of product (M) into a reaction container, dissolving in 200mL of deionized water, carrying out ice bath and introducing nitrogen for more than 30min, polymerizing the product by using an oxidation-reduction initiation system ammonium persulfate and ferrous ammonium sulfate (the mass ratio of an oxidant to a reducing agent is 1.2:1, 1.5:1 and 2:1 respectively), dialyzing, and filtering to obtain a product of polyacrylic acyloxy ethyl-N, N, N-dimethyl alkyl ammonium bromide (ASC).
Respectively dissolving the sodium humate polycondensate and polyacryloyloxyethyl-N, N, N-dimethyl alkyl ammonium bromide (ASC) in water to prepare a polymer solution, mixing the polymer solution and the polymer solution according to the mass ratio of 1:1, and carrying out performance index screening test.
Example 1: preparation of novel composite thickened oil viscosity reducer A
30g of sodium humate polycondensate (HA) as active ingredient In(N-25), 70g of Polyacryloxyethyl-N, N, N-dimethylalkylammonium bromide (ASC) (m is about 500) and 100g of ethanol were mixed well to give a high performance viscosity reducer for thick oils, designated A, where (HA)nAnd ASC in a mass ratio of 3:7 (HA)nAnd the mass ratio of the total mass of the ASC and the ethanol is 1: 1.
Example 2: preparation of novel composite thickened oil viscosity reducer B
40g polycondensate (HA) of sodium humate as active ingredient In(N-25), 60g of Polyacryloxyethyl-N, N, N-dimethylalkylammonium bromide (ASC) (m is about 500) and 100g of ethanol were mixed well to give a high performance viscosity reducer for thick oils, designated B, where (HA)nAnd ASC in a mass ratio of 4:6 (HA)nAnd the mass ratio of the total mass of the ASC and the ethanol is 1: 1.
Example 3: preparation of novel composite thickened oil viscosity reducer C
50g polycondensate (HA) of sodium humate as active ingredient In(N-25), 50g of Polyacryloxyethyl-N, N, N-dimethylalkylammonium Bromide (ASC) (m is about 500) and 100g of ethanol were mixed well to give a high performance viscosity reducer for thick oils, designated C, where (HA)nAnd ASC in a mass ratio of 5:5 (HA)nAnd the mass ratio of the total mass of the ASC and the ethanol is 1: 1.
Example 4: preparation of novel composite thickened oil viscosity reducer D
50g polycondensate (HA) of sodium humate as active ingredient In(N-50), 50g of Polyacryloxyethyl-N, N, N-dimethylalkylammonium bromide (ASC) (m is about 500) and 100g of ethanol were mixed well to give a high performance viscosity reducer for thick oils, designated D, where (HA)nAnd ASC in a mass ratio of5:5，(HA)nAnd the mass ratio of the total mass of the ASC and the ethanol is 1: 1.
Example 5: preparation of novel composite thickened oil viscosity reducer E
50g polycondensate (HA) of sodium humate as active ingredient In(N-50), 50g of Polyacryloxyethyl-N, N, N-dimethylalkylammonium bromide (ASC) (m is about 500) and 100g of ethanol were mixed well to give a high performance viscosity reducer for thick oils, designated E, where (HA)nAnd ASC in a mass ratio of 4:6 (HA)nAnd the mass ratio of the total mass of the ASC and the ethanol is 1: 1.
Example 6: preparation of novel composite thickened oil viscosity reducer F
50g polycondensate (HA) of sodium humate as active ingredient In(N-50), 50g of Polyacryloxyethyl-N, N, N-dimethylalkylammonium bromide (ASC) (m is about 500) and 100g of ethanol were mixed well to give a high performance viscosity reducer for thick oils, designated F, where (HA)nAnd ASC in a mass ratio of 3:7 (HA)nAnd the mass ratio of the total mass of the ASC and the ethanol is 1: 1.
Example 7: preparation of novel composite thickened oil viscosity reducer G
50g polycondensate (HA) of sodium humate as active ingredient In(N-75), 50G of Polyacryloxyethyl-N, N, N-dimethylalkylammonium bromide (ASC) (m is about 500) and 100G of ethanol were mixed well to give a high performance viscosity reducer for thick oils, designated G, where (HA)nAnd ASC in a mass ratio of 5:5 (HA)nAnd the mass ratio of the total mass of the ASC and the ethanol is 1: 1.
Example 8: preparation of novel composite thickened oil viscosity reducer H
50g polycondensate (HA) of sodium humate as active ingredient In(N-75), 50g of Polyacryloxyethyl-N, N, N-dimethylalkylammonium bromide (ASC) (m is about 500) and 100g of ethanol were mixed well to give a high performance viscosity reducer for thick oils, designated H, where (HA)nAnd ASC in a mass ratio of 4:6 (HA)nAnd the mass ratio of the total mass of the ASC and the ethanol is 1: 1.
Example 9: preparation of novel composite thickened oil viscosity reducer I
50g of active ingredient I humicPolycondensates of sodium acid (HA)n(N-75), 50g of Polyacryloxyethyl-N, N, N-dimethylalkylammonium bromide (ASC) (m is about 500) and 100g of ethanol were mixed well to give a high performance viscosity reducer for thick oils, designated I, where (HA)nAnd ASC in a mass ratio of 3:7 (HA)nAnd the mass ratio of the total mass of the ASC and the ethanol is 1: 1.
Viscosity reduction effect test of composite type thickened oil viscosity reducer A, B, C, D, E, F, G, H of example 10 and examples 1-9 and I
And (3) reducing the viscosity of the thick oil sample by a bottle test method, wherein the viscosity of the thick oil is 11000mPa & s at 30 ℃. The results of the experiments are shown in tables 1 to 3.
The specific experimental steps are as follows:
the viscosity reducers for thick oil (A-I) prepared in examples 1 to 9 were used with a degree of mineralization of 3X 104Preparing a thick oil viscosity reducer solution by using mg/L saline, and respectively adding the thick oil viscosity reducer into test tubes with plugs, wherein 50mL of dehydrated and degassed thick oil samples are filled with the viscosity reducer, the concentration of the viscosity reducer is 1200mg/L, and the volume ratio of the thick oil viscosity reducer solution to the thick oil samples is 1: 1. After the test tube plug is tightly covered, the test tube is placed in an oscillation box and horizontally oscillated for 80-100 times, and the amplitude is larger than 20 cm. After thorough mixing, the viscosity of the mixed system was measured using a Brookfield viscometer (shear rate 7.34 s) at 40 deg.C, 60 deg.C, 80 deg.C, respectively-1). The viscosity reduction results for thick oil are shown in tables 1 to 3.
TABLE 1 results of viscosity reduction test of samples of the viscosity reducer for thickened oils at 40 ℃ in examples 1 to 9
TABLE 2 results of viscosity reduction experiments on samples of thickened oils at 60 ℃ for the thickened oil viscosity reducers of examples 1 to 9
TABLE 3 results of viscosity reduction experiments on samples of the thick oil viscosity reducers of examples 1 to 9 at 80 deg.C
The results show that the viscosity reducer for thick oil has good viscosity reducing performance aiming at thick oil, the viscosity reducing rate at 40 ℃, 60 ℃ and 80 ℃ reaches more than 80%, particularly the viscosity reducing rate at 40 ℃, 60 ℃ and 80 ℃ of the viscosity reducer C is 90.86%, 95.62% and 98.63%, respectively, and good viscosity reducing capability is shown.
Claims (11)
1. The active ingredients of the viscosity reducer for the thickened oil comprise a sodium humate polycondensate and a polymer shown as a formula c;
the sodium humate polycondensate is prepared by a method comprising the following steps of: taking triphenyl phosphine and diethyl azodicarboxylate as catalysts, and carrying out polycondensation reaction on sodium humate at 50-180 ℃ for 3-10 hours under the action of concentrated sulfuric acid;
in the formula c, R is- (CH)2)XCH3X is an integer of 5 to 22; m is 100 to 800.
2. The viscosity reducer for thick oil according to claim 1, characterized in that: the thick oil viscosity reducer also comprises a solvent.
3. The viscosity reducer for thick oil according to claim 2, characterized in that: the solvent is at least one selected from water, methanol and ethanol.
4. The thick oil viscosity reducer according to any one of claims 1 to 3, characterized in that: in the heavy oil viscosity reducer, the mass ratio of the sodium humate polycondensate to the polymer shown in the formula c is 20-50: 50-80.
5. The thick oil viscosity reducer according to claim 2 or 3, characterized in that: the thickened oil viscosity reducer consists of a sodium humate polycondensate, a polymer shown in a formula c and the solvent.
6. The viscosity reducer for thick oil according to claim 5, characterized in that: in the viscosity reducer, the sodium humate polycondensate and the polymer shown in the formula c account for 40-60% of the total mass of the viscosity reducer;
the sodium humate polycondensate accounts for 20-50% of the total mass of the sodium humate polycondensate and the polymer shown in the formula c;
the polymer shown in the formula c accounts for 50-80% of the total mass of the sodium humate polycondensate and the polymer shown in the formula c.
7. A process for preparing the thick oil viscosity reducer of any one of claims 1-6, comprising: and (3) uniformly mixing the sodium humate polycondensate, the polymer shown in the formula c and the solvent to obtain the sodium humate polycondensate.
8. Use of the thick oil viscosity reducer of any one of claims 1-6 in thick oil recovery.
9. Use according to claim 8, characterized in that: in the process of thick oil exploitation, the using temperature of the thick oil viscosity reducer is 40-80 ℃;
the volume ratio of the thickened oil viscosity reducer to the thickened oil is 1: 0.5-10;
the thick oil viscosity reducer is diluted before use.
10. Use according to claim 9, characterized in that: the volume ratio of the thickened oil viscosity reducer to the thickened oil is 1: 1.
11. Use according to claim 9 or 10, characterized in that: in the diluting step, the diluent is seawater; the concentration after dilution is 500mg/L-2500 mg/L.
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