CN103666414A - Polyamide amine flowing modifier for mineral oil based drilling fluid and preparation method of modifier - Google Patents
Polyamide amine flowing modifier for mineral oil based drilling fluid and preparation method of modifier Download PDFInfo
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- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/02—Well-drilling compositions
- C09K8/03—Specific additives for general use in well-drilling compositions
- C09K8/035—Organic additives
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/02—Well-drilling compositions
- C09K8/32—Non-aqueous well-drilling compositions, e.g. oil-based
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Abstract
The invention discloses a polyamide amine flowing modifier for mineral oil based drilling fluid and a preparation method of the modifier. The modifier is prepared in such way that dimer fatty acid and polybasic amine are subjected to amidation reaction at 120-160 DEG C and then a reaction product is homogeneously mixed with a solvent; the content of dimer in the dimer fatty acid is greater than 78wt%; the polybasic amine is a homolog of polyethylene polyamine containing 2-5 amido groups; the molar ratio of the carboxylic groups in the dimer fatty acid to the amido groups in the polybasic amine is 1 to (0.2-1.2). The preparation process is fulfilled in a reaction vessel connected with a Dean-Stark receiver. The polyamide amine flowing modifier has high molecular weight and multiple active functional groups, can form multi-point adsorption, is hard to desorb from the surface of organic soil, and is continuously effective and stable in performance at high temperature; the preparation process is simple and reaction conditions are easy to control.
Description
Technical field
The present invention relates to a kind of oil and natural gas industry drilling fluid, particularly polyamide-based amine flow pattern regulator and preparation method thereof for a kind of mineral oil based drilling fluid.
Background technology
Along with the development of modern drilling technology, oil base drilling fluid because it has that oilness is good, strong inhibition capability, the primary selection to premium properties the becomes various complex stratigraphic drillings such as formation damage is little.But oil base drilling fluid suspension is poor, may form cutting bed, therefore, suspending power is one of parameter determining oil base drilling fluid performance, directly has influence on effect of hole cleaning, high-density weighting material sedimentation, equivalent circulating density, pressure excitement and swabbing pressure etc.Only have suitable suspending power and keep it stable, could successfully drill the narrow well section of Holes of Complicated Wells, especially deep well, hp-ht well and ' Safe Density Windows.
As glutinous the carrying of increasing of oil base drilling fluid, cut agent in early days--organophilic clay is widely used.But, the easy multiviscosisty of organophilic clay high temperature, the work-ing life of reducing oil base drilling fluid, reduce the solid content of oil base drilling fluid, pollute low permeability reservoir.Increasingly stringent along with environmental protection requirement; low/without the mineral oil of aromatic hydrocarbons and synthetic base oil, to replace after diesel oil; conventional organophilic clay dispersion suspension performance in this class environmental protection base oil is lower; the organophilic clay that often needs higher concentration; just can reach the effect of suspension high-density weighting material and hole cleaning, through shaft bottom high temperature, cause environment-friendly oil-based/synthetic base drilling fluid plastic viscosity to increase; rate of penetration reduces, and in the bad ground of many cover pressure systems, causes down-hole accident.
Study and think in early days, the suspending power that improves drilling fluid realizes by increasing Drilling Fluid Viscosity, and has developed the oil soluble macromolecular materials such as styrene-butadiene rubber(SBR).Along with going deep into of industrial practice and scientific research, there are some new viewpoints and progressively in oil drilling industry, be applied: in mineral oil and synthetic base drilling fluid, adding the oil-soluble polar organic matter matter of a class low viscosity (low-molecular-weight), can significantly improve the gelling behavior of organophilic clay, the yield value of raising system, low-shear rate viscosity etc., oil base drilling fluid reaches the state of " the fast weak gel " of " low sticky height is cut ".
At present, domestic mineral oil based drilling liquid technology is in developmental stage, has larger gap with comparing abroad.In order to reach required suspension character, often added the organophilic clay of excessive concentrations, under the hot conditions of shaft bottom, organophilic clay degree of scatter increases, and drilling fluid multiviscosisty is serious, and plastic viscosity is increased sharply; And for addressing this problem, in site operation, add polyalcohols, as ethylene glycol, glycerine and polyoxyethylene glycol etc.; Ethers, as Diethylene Glycol and dimethyl ether; Small molecules amides, as materials such as methane amide, ethanamides.These small-molecule substances at high temperature can be attached from organophilic clay surface desorption, thereby reduce the jelling structure of drilling fluid.
Summary of the invention
The object of the present invention is to provide polyamide-based amine flow pattern regulator for a kind of mineral oil based drilling fluid, its molecular weight is large, and active function groups is many, can form multipoint adsorption, be difficult to from organophilic clay surface desorption attached, continuous and effective at high temperature, stable performance.
Another object of the present invention is to provide the preparation method of a kind of mineral oil based drilling fluid with polyamide-based amine flow pattern regulator, the method technological process is simple, can meticulous control reaction conditions; Under the prerequisite that does not affect result of use, adopt double solvents, reduce the usage quantity of polar solvent, reduce costs; And product characteristics and the stable performance of the polyamide-based amine flow pattern regulator finally making.
For this reason, technical scheme of the present invention is:
A polyamide-based amine flow pattern regulator for mineral oil based drilling fluid carries out amidate action by dimer (fatty acid) yl and polyamine under 120～160 ℃ of conditions, after having reacted, the product making is mixed and is made according to mass ratio 0.5～1.5:1 with solvent; In described dimer (fatty acid) yl, dimeric content is greater than 78wt%; Described polyamine is the homologue of the polyethylene polyamine that contains 2～5 amidos; In described dimer (fatty acid) yl, in carboxyl and polyamine, the mol ratio of amido is 1:0.2～1.2, preferably 1:0.4～0.8, more preferably 1:0.7; Described solvent is diethylene glycol monomethyl ether, diethylene glycol dimethyl ether, Dipropylene glycol mono-n-butyl Ether or DPGME, or any one and the mixture of any ratio of mineral oil in these four kinds of materials.
Described dimer (fatty acid) yl is the mixing acid of monomer acids, dimer (fatty acid) yl and three polyglycerol fatty acids, and the content of wherein said monomer acids is 2～22wt%, and the content of dimer (fatty acid) yl is 78%～98wt%, and the content of three polyglycerol fatty acids is 0～12wt%.
Described polyamine is for being quadrol, diethylenetriamine, triethylene tetramine or tetraethylene pentamine.
The mass ratio that described amidate action makes product and solvent is 0.8～1.2:1, preferably 1:1.
Described mineral oil is 5# industrial white oil, and described solvent is the double solvents that glycol monomethyl ether is mixed with mass ratio 10～90:90～10 with 5# industrial white oil; Both mass ratioes are 30～80:70～20 preferably, most preferably are 60:40.
A preparation method for polyamide-based amine flow pattern regulator for mineral oil based drilling fluid, comprises the steps:
1) take in dimer (fatty acid) yl the mol ratio of amido in carboxyl and polyamine takes respectively dimer (fatty acid) yl and the polyamine that dimer content is greater than 78wt% as 1:0.2～1.2;
2) material step 1) being taken is inserted in the reaction vessel that is connected with Dean-Stark receptor, stirring, 120～160 ℃, be connected with under condition of nitrogen gas and react 1～3h, obtain just finished product; This step temperature of reaction is preferably 140～160 ℃, more preferably 150～155 ℃.
3) described just finished product is mixed according to mass ratio 0.5～1.5:1 with solvent, obtain polyamide-based amine flow pattern regulator for described mineral oil based drilling fluid; Wherein said solvent is diethylene glycol monomethyl ether, diethylene glycol dimethyl ether, Dipropylene glycol mono-n-butyl Ether or DPGME, or in these four kinds of materials any one with mineral oil with arbitrarily than mixture.
Polyamide-based amine flow pattern regulator prepared by the present invention is the non-nylon material class polyamide materials that a class is prepared by dimer (fatty acid) yl and multi-element organic amine condensation, the feature of condensation reaction has determined that primary amine groups, secondary amine and amide group isopolarity functional group are uniformly distributed in polymer molecule, this class active function groups can form multipoint adsorption on organophilic clay surface, strengthened the interaction of organophilic clay in nonpolar environment, improved gelating property, under high temperature, be difficult for desorption, at shaft bottom high temperature, still can keep certain jelling structure.In addition, in preparation method, the present invention is at the enterprising one-step optimization in the basis of the disclosed method of patent CN103012180A, by three kinds of raw materials, change two kinds of raw materials into, by two steps, feed intake and change a step into and feed intake, by two step pyroreactions, change a step pyroreaction into, reduced the control difficulty of technological process, save energy consumption, reduced labour intensity.
Embodiment
Mineral oil based drilling fluid of the present invention is mainly made by carboxylic acyloxy amination reaction with polyamide-based amine flow pattern regulator, and the functional group of generation is mainly acid amides, generates water in reaction process.But in lipid acid and polyamine reaction process, can the higher cross-linking products of generating portion molecular weight.If under hot conditions the reaction times long, can there is part crosslinking reaction, but not affect the performance that makes product.If excessively crosslinked, cross-linking products is difficult to dissolve, disperse so, can not be applied.
In order to obtain the product of excellent performance, not only need to control the type of reactant, also need strictly to control the reaction times.
Below in conjunction with embodiment, describe the present invention.
Embodiment 1
Diethylenetriamine and dimer (fatty acid) yl (78wt% dimeracid, 10wt% monomer acids and 12wt% trimer acid) that in the four-hole reactor with agitator, thermometer, logical nitrogen device (protection of inert gas is also carried steam) and Dean-Stark receptor, to add by the ratio of amido quantity and carboxyl quantity be 0.4:1.0; with constant temperature oil bath, be heated to 110 ℃ of reaction 0.5h; be warming up to 150 ℃, reaction 3.0h obtains polyamide-based amine flow pattern regulator for mineral oil based drilling fluid of the present invention again.The mineral oil based drilling fluid obtaining is mixed with mass ratio 1:1 with solvent with polyamide-based amine flow pattern regulator, obtain product P AA-1; Wherein: solvent is that mass ratio is the dipropylene glycol monomethyl ether of 60:40 and the mixture of 5# industrial white oil.
Embodiment 2
Triethylene tetramine and dimer (fatty acid) yl (92wt% dimeracid, 2.5% monomer acids and 5.5% trimer acid) that in the four-hole reactor with agitator, thermometer, logical nitrogen device (protection of inert gas is also carried steam) and Dean-Stark receptor, to add by the ratio of amido quantity and carboxyl quantity be 0.7:1.0; with constant temperature oil bath, be heated to 110 ℃ of reaction 0.5h; be warming up to 160 ℃, reaction 2.0h obtains polyamide-based amine flow pattern regulator for mineral oil based drilling fluid of the present invention again.The mineral oil based drilling fluid obtaining is mixed with mass ratio 1:1 with solvent with polyamide-based amine flow pattern regulator, obtain product P AA-2; Wherein: solvent is that mass ratio is the dipropylene glycol monomethyl ether of 60:40 and the mixture of 5# industrial white oil.
Embodiment 3
Triethylene tetramine and dimer (fatty acid) yl (98wt% dimeracid and 2wt% monomer acids) that in the four-hole reactor with agitator, thermometer, logical nitrogen device (protection of inert gas is also carried steam) and Dean-Stark receptor, to add by the ratio of amido quantity and carboxyl quantity be 0.8:1.0; with constant temperature oil bath, be heated to 110 ℃ of reaction 0.5h; be warming up to 160 ℃, reaction 1.5h obtains polyamide-based amine flow pattern regulator for mineral oil based drilling fluid of the present invention again.The mineral oil based drilling fluid obtaining is mixed with mass ratio 1:1 with solvent with polyamide-based amine flow pattern regulator, obtain product P AA-3; Wherein: solvent is that mass ratio is the dipropylene glycol monomethyl ether of 60:40 and the mixture of 5# industrial white oil.
Embodiment 4
Tetraethylene pentamine and dimer (fatty acid) yl (98wt% dimeracid and 2wt% monomer acids) that in the four-hole reactor with agitator, thermometer, logical nitrogen device (protection of inert gas is also carried steam) and Dean-Stark receptor, to add by the ratio of amido quantity and carboxyl quantity be 0.8:1.0; with constant temperature oil bath, be heated to 110 ℃ of reaction 0.5h; be warming up to 150 ℃, reaction 1.5h obtains polyamide-based amine flow pattern regulator for mineral oil based drilling fluid of the present invention again.The mineral oil based drilling fluid obtaining is mixed with mass ratio 1:1 with solvent with polyamide-based amine flow pattern regulator, obtain product P AA-4; Wherein: solvent is that mass ratio is the dipropylene glycol monomethyl ether of 60:40 and the mixture of 5# industrial white oil.
Embodiment 5
Quadrol and dimer (fatty acid) yl (98wt% dimeracid and 2wt% monomer acids) that in the four-hole reactor with agitator, thermometer, logical nitrogen device (protection of inert gas is also carried steam) and Dean-Stark receptor, to add by the ratio of amido quantity and carboxyl quantity be 0.8:1.0; with constant temperature oil bath, be heated to 110 ℃ of reaction 0.5h; be warming up to 155 ℃, reaction 1.5h obtains polyamide-based amine flow pattern regulator for mineral oil based drilling fluid of the present invention again.The mineral oil based drilling fluid obtaining is mixed with mass ratio 1:1 with solvent with polyamide-based amine flow pattern regulator, obtain product P AA-5; Wherein: solvent is that mass ratio is the dipropylene glycol monomethyl ether of 60:40 and the mixture of 5# industrial white oil.
Note: described in embodiment, three kinds of dimer (fatty acid) yls are respectively dimer (fatty acid) yl (78wt% dimeracid, 10wt% monomer acids and 12wt% trimer acid), dimer (fatty acid) yl (92wt% dimeracid, 2.5% monomer acids and 5.5% trimer acid) and dimer (fatty acid) yl (98wt% dimeracid and 2wt% monomer acids), its trade name is dimer (fatty acid) yl or dimeracid, being that concrete content is different, is concrete technical indicator in bracket.
Application experiment: preparation mineral oil based drilling fluid
Formula forms:
5# white oil: mineral oil based drilling fluid base oil;
Organobentonite: tackifier;
Calcium oxide: alkalinity control agent;
BZ-OFL-II: pitch class fluid loss agent;
PAA: the polyamide-based amine flow pattern regulator that the present invention makes;
SPAN-80: wetting agent;
Limestone powder: high-density weighting material;
Barite: high-density weighting material;
Layoutprocedure: SPAN-80, flow pattern regulator PAA are joined in 5# white oil, and high-speed stirring 5～10min, then adds organobentonite, calcium oxide, stirs 30～40min; Add fluid loss agent BZ-OFL-II to stir 15min, add limestone powder and barite, stir 40～60min.
According to the method described above, the polyamide-based amine flow pattern regulator preparation mineral oil based drilling fluid that utilizes embodiment 1～3 to make, as shown in table 1:
The polyamide-based amine flow pattern regulator preparation mineral oil based drilling fluid that table 1 utilizes embodiment 1～3 to make
| Component | Formula-1 | Formula-2 | Formula-3 |
| 5# white oil, mL | 400 | 400 | 400 |
| SPAN-80，g | 8 | 8 | 8 |
| PAA-1，g | 6 | — | — |
| PAA-3，g | — | 6 | — |
| PAA-5，g | — | — | 6 |
| Organophilic clay, g | 18 | 18 | 18 |
| Calcium oxide, g | 10 | 10 | 10 |
| BZ-OFL-II，g | 16 | 16 | 16 |
| Limestone powder, g | 170 | 170 | 170 |
| Barite, g | 150 | 150 | 150 |
The performance of the full oil base drilling fluid making by table 1 formula is as shown in table 2.
The performance of full oil base drilling fluid in table 2 table 1
Note: 1. rheological parameter probe temperature is 50 ℃;
2. aging condition is 150 ℃ * 16h;
3. High Temperature High Pressure leak-off FL
hTHPcondition is 150 ℃, and pressure reduction is 3.5MPa.
4. Φ wherein
600, Φ
300, Φ
200, Φ
100, Φ
6, Φ
3represent respectively the reading of 600 revs/min, 300 revs/min, 200 revs/min, 100 revs/min, 6 revs/min, 3 revs/min.
Above result shows, add after polyamide-based amine flow pattern regulator, the yield value (YP) of full oil base drilling fluid system, the low-shear rate viscosity reading of 6 revs/min and 3/ minute while turning () all increase substantially, and plastic viscosity (PV) is not subject to remarkably influenced, and good with other treatment agent compatiblenesies.After 150 ℃ of high temperature ageings, the performance of the product of three kinds of different material proportion of composing has greatly changed, wherein, ingressing after the full oil base drilling fluid system that contains the product P AA-3 that amido and carboxyl ratio are 0.7:1.0 is aging, egress difference is less, and the full oil base drilling fluid system that contains other two kinds of product P AA-1 and PAA-5 is ingressed, egress difference is larger, illustrate that product P AA-3 has preferably temperature stability, make full oil base drilling fluid system have more the characteristic of " weak gel strength fast " and inductile viscosity, be conducive to improve drilling speed and hole cleaning efficiency.
Claims (10)
1. polyamide-based amine flow pattern regulator for a mineral oil based drilling fluid, it is characterized in that: by dimer (fatty acid) yl and polyamine, under 120～160 ℃ of conditions, carry out amidate action, after having reacted, the product making is mixed and made according to mass ratio 0.5～1.5:1 with solvent;
In described dimer (fatty acid) yl, dimeric content is greater than 78wt%;
Described polyamine is the homologue of the polyethylene polyamine that contains 2～5 amidos;
In described dimer (fatty acid) yl, in carboxyl and polyamine, the mol ratio of amido is 1:0.2～1.2;
Described solvent is diethylene glycol monomethyl ether, diethylene glycol dimethyl ether, Dipropylene glycol mono-n-butyl Ether or DPGME, or any one and the mixture of any ratio of mineral oil in these four kinds of materials.
2. polyamide-based amine flow pattern regulator for mineral oil based drilling fluid as claimed in claim 1, is characterized in that: in described dimer (fatty acid) yl, in carboxyl and polyamine, the mol ratio of amido is 1:0.4～0.8, is preferably 1:0.7.
3. polyamide-based amine flow pattern regulator for mineral oil based drilling fluid as claimed in claim 1, is characterized in that: described dimer (fatty acid) yl is the mixing acid of monomer acids, dimer (fatty acid) yl and three polyglycerol fatty acids.
4. polyamide-based amine flow pattern regulator for mineral oil based drilling fluid as claimed in claim 3, is characterized in that: the content of described monomer acids is 2～22wt%, and the content of dimer (fatty acid) yl is 78%～98wt%, and the content of three polyglycerol fatty acids is 0～12wt%.
5. polyamide-based amine flow pattern regulator for mineral oil based drilling fluid as claimed in claim 1, is characterized in that: described polyamine is for being quadrol, diethylenetriamine, triethylene tetramine or tetraethylene pentamine.
6. polyamide-based amine flow pattern regulator for mineral oil based drilling fluid as claimed in claim 1, is characterized in that: the mass ratio that described amidate action makes product and solvent is 0.8～1.2:1, preferably 1:1.
7. polyamide-based amine flow pattern regulator for mineral oil based drilling fluid as claimed in claim 1, is characterized in that: described mineral oil is 5# industrial white oil.
8. polyamide-based amine flow pattern regulator for mineral oil based drilling fluid as claimed in claim 7, is characterized in that: described solvent is the double solvents that glycol monomethyl ether is mixed with mass ratio 10～90:90～10 with 5# industrial white oil; Both mass ratioes are 30～80:70～20 preferably, most preferably are 60:40.
9. the preparation method of polyamide-based amine flow pattern regulator for mineral oil based drilling fluid as described in claim 1, is characterized in that: comprise the steps:
1) take in dimer (fatty acid) yl the mol ratio of amido in carboxyl and polyamine takes respectively dimer (fatty acid) yl and the polyamine that dimer content is greater than 78wt% as 1:0.2～1.2;
2) material step 1) being taken is inserted in the reaction vessel that is connected with Dean-Stark receptor, stirring, 120～160 ℃, be connected with under condition of nitrogen gas and react 1～3h, obtain just finished product;
3) described just finished product is mixed according to mass ratio 0.5～1.5:1 with solvent, obtain polyamide-based amine flow pattern regulator for described mineral oil based drilling fluid; Wherein said solvent is diethylene glycol monomethyl ether, diethylene glycol dimethyl ether, Dipropylene glycol mono-n-butyl Ether or DPGME, or in these four kinds of materials any one with mineral oil with arbitrarily than mixture.
10. preparation method as claimed in claim 9, is characterized in that: step 2) temperature of reaction be 140～160 ℃, preferably 150～155 ℃.
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| CN104818004A (en) * | 2015-05-20 | 2015-08-05 | 中国海洋石油总公司 | Tackifying and shear strength improving agent as well as preparation method and application of tackifying and shear strength improving agent |
| CN104974721A (en) * | 2014-04-11 | 2015-10-14 | 中国石油化工集团公司 | Preparation used in high-temperature-resistant oil-based drilling fluid and preparation method thereof |
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