CN101671438A - Titanium and nano fluorine-containing poly (aryl ether ketone) copolymer, coating made thereof and manufacturing method thereof - Google Patents
Titanium and nano fluorine-containing poly (aryl ether ketone) copolymer, coating made thereof and manufacturing method thereof Download PDFInfo
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- CN101671438A CN101671438A CN200810198419A CN200810198419A CN101671438A CN 101671438 A CN101671438 A CN 101671438A CN 200810198419 A CN200810198419 A CN 200810198419A CN 200810198419 A CN200810198419 A CN 200810198419A CN 101671438 A CN101671438 A CN 101671438A
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Abstract
The invention makes further technical innovation in the prior invention and obtains a titanium and nano fluorine-containing poly (aryl ether ketone) macromolecular alloy copolymer by copolymerizationof a nano organic titanium polymer and a nano alumina-modified fluorine-containing poly (aryl ether ketone) polymer. The novel material has a series of excellent physicochemical characteristics and isextremely suitable to meet the special protection requirements of exploitation equipment of underground deep crude oil and natural gas such as high hardness, corrosion resistance, high temperature resistance, high-pressure hot vapor penetrability resistance, dirt picking up and scale deposition prevention, aging resistance, durability and other properties. A nano organic titanium macromolecular alloy coating manufactured by using the novel chemical material of the invention as a substrate film forming material resin is used in anticorrosion coatings of oil-gas field well exploitation drillingtools and well pipes and has the advantages of prolonging the protection life of a nano ceramic film coating and an organic titanium special anticorrosion coating by several times, greatly reducing oil and natural gas exploitation cost and equipment maintenance cost and obviously improving comparable relative production efficiency compared with the product of the prior invention.
Description
Technical field
The invention belongs to chemosynthesis and chemical composition technical field, what relate to is a kind of nano organic titanium fluorinated poly arylene ether ketone copolymers and nano organic titanium high polymer alloy coating thereof; Be mainly used in oil-gas field deep-well drill tool and oil recovery pipeline and under the high temperature pressure corrosion envrionment conditions, have the special anticorrosive erosion resisting coating protection of special technical requirement.
Background technology
Underground deep layer crude oil or gas extraction, geological condition and corrosive environment very complicated (shown in table-1).Because (＞3MPa) the strong osmotic effect of hot steam, all kinds of corrosive mediums in crude oil and the sewage are (as SO for high temperature (80～250 ℃) and high pressure in addition
4 2-, NO
3 -, Cl
-, F
-, CN
-, Ba
+, Ca
+Deng) and the erosion of unwanted bacteria, oil gas down-hole equipment, tubing string, pipeline and the chemical corrosion and the deposition fouling of oil/gas pipe line, container basin have on the ground been quickened, not only shortened the work-ing life of winning apparatus, cause increasing of exploitation of oil-gas field cost, and seriously influence the ordinary production of enterprise.Introduce according to " coatings industry " 2006 the 36th volumes 2 phases (total the 259th phase), Liu Yuqin, Feng Yantao, people's such as Peng Xuan investigation shows: underground deep layer oil recovery pipeline is subjected to the influence of tectonic structure and reservoir condition, corrode very serious, the average corrosion rate of buried oil pipe line is up to 1.5～3.3mm/a, and spot corrosion speed is up to 5～15mm/a, and corrosion condition is perforation in 3～6 months, just needed overhaul in 6～12 months, promptly scrapped in 1～2 year.Oil recovery does not wait at 9～18 months with the mean lifetime of underground oil pipe, and the shortest only has 3 months.Deep layer underground pipeline protection against corrosion problem becomes the normal key of recovering the oil and reducing cost for oil production in oil field.
In petroleum industry, it is more more complex than buried oil pipeline road, the face of land with the Working environment of underground pipeline to recover the oil, and therefore, the anticorrosive work of the underground oil recovery pipeline of deep layer is also much bigger than the difficulty of face of land oil pipeline.Though oilfield applications is paid much attention to the corrosion and protection of oil recovery pipeline at present, to existing oil pipe anti-corrosive erosion technology
Table 1 recovers the oil with small-bore pipeline underground deep layer Working environment and corrosion factor
[1]
| Environmental factors | Content | Remarks |
| Pipe laying depth of stratum/m | ??0～5000 | The common degree of depth＞the 2000m of oil well |
| The pipe laying formation temperature/℃ | ??100～250 | Whenever go deep into 100m and increase by 1 ℃ |
| Oil pipe bears pressure/MPa | ??＞10 | Inject high-pressure steam pressure＞3 |
| Underground water water type | ??CaCl 2、MgCl 2、NaHCO 3、Na 2SO 4 | Different tectonic structures are all variant |
| Underground water | ??Cl -、SO 4 2-、HCO 3 -、F - | The acid attack medium |
| Dissolved ions | ??K +、Na +、Ca 2+、Mg 2+ | The alkaline corrosion medium |
| Contained element in the oil | C, H, N, O, S and trace metal thereof and non-metallic element | ??H 2S、CO 2、O 2、H 2O |
| Phreatic salinity | ??3*103 -1*105mg/L | Different tectonic structures are all variant |
| Bacterium | Sulphate reducing bacteria (SRB) |
Constantly improve and perfect, to seek the breakthrough of new anticorrosion technique.But because the restriction of the anticorrosive that is fallen behind, the heavy corrosion problem of solution oil recovery pipeline has become the anxious century difficult problem that alleviate oil crisis and quickens the energy industry development world today.
Summary of the invention
The objective of the invention is to overcome above-mentioned the deficiencies in the prior art, prepare a kind of high-performance polymer and provide a kind of by the modification technology that adopts nano material, and with this speciality coating product, for opening up a new way in industrial antisepsis erosion field as base-material exploitation series; As, for the oil-gas field well provides a kind of protection against corrosion type material with the protection of drilling tool and oil recovery pipeline.
The object of the present invention is achieved like this:
The technological line that is adopted is to adopt the mechanochemistry principle, grind the heat energy accumulation that is produced by special national patented product " planetary type ball-milling reactor " by Nanjing Univ. Instrument Factory's invention, make solvent carrier under hot environment, begin vaporization, and in airtight reactor, form High Temperature High Pressure, this moment is under the effect of nano aluminium oxide as catalyzer, nano organic titanium polymer and nanometer alumina modified fluorinated poly arylene ether ketone polymer generation copolyreaction, obtain the thermoplastic organic polymer alloy of a kind of linear structure attitude multipolymer novel material, with the nano fluorine-contained polyaryletherketone high polymer alloy of its called after titanium hybrid copolymers, be called for short the nano fluorine-contained poly (aryl ether ketone) copolymer of titanium at this; Its skeleton symbol is abbreviated as (T_PAEK_F)
XNMP nIts chemical structural formula is:
Polymerization degree n in the formula 〉=8;
Be nano aluminium oxide; In its skeleton symbol (T_PAEK_F)
x nBe polymkeric substance, NMP is a solvent carrier.(T_PAEK_F)
XNMP nSolids content be about about 65%.(T_PAEK_F)
x nBe a kind of novel thermoplastic high molecule alloy material, can be used for the exotic materials of space flight and aviation industrial circle.The present invention mainly is the anticorrosive coating with its a kind of special purpose of developing as the oilfield drilling pipeline protection.
The preparation method of the synthetic and nano organic titanium high polymer alloy coating of the nano fluorine-contained poly (aryl ether ketone) copolymer of titanium described in the present invention, its feature may further comprise the steps:
The first step takes by weighing each component according to formula ratio, in the closed planetary ball mill reactor of packing into special in order.Then by sealed tank cap behind the Stainless Steel Ball of proportioning adding different-grain diameter.
Second step started the ball-milling reaction device and enters normal operation, ground must not be less than 5h working time.Behind the operation 3h, shutdown inspection.Later every upper end metallic thermometer of operation 1h shutdown inspection record and barometric data.Prepolymer is under the effect of carrier NMP or tetramethylene sulfone and catalyst, and through grind heating up, (when jar interior temperature＞180 ℃, pressure for vaporization＞0.6MPa), copolyreaction begins to the required temperature and pressure of reaction for temperature in jar, accumulation of pressure.Allowing the ball milling reaction times continue 1h more then can shut down.
After the 3rd step, the question response jar naturally cooled to normal temperature, open jar and filter out Stainless Steel Ball, obtain the polymerisate of black mud shape, its particle diameter is about 50～80nm, solids content 〉=65%.
The 4th step took by weighing each component by formulation for coating material amount and order and places in the sand milling cylinder, earlier after disperseing 20 minutes on the high speed dispersor, transfer to the laboratory again and grind, require fineness until being ground to basket type sand mill, with 300 order screen cloths filter promptly to nano organic titanium high polymer alloy coating.
Beneficial effect of the present invention is as follows:
(1) The present invention be directed to an oil-gas field deep-well drill tool and a underground defeated Corrosion of Pipeline and the protection difficult problem of adopting, two patents of invention of having applied for before the applicant, its number of patent application is respectively: 200610122225.X and 200810029936.1 relates to nano aluminium oxide, fluorinated poly arylene ether ketone, nano modifier, nano organic titanium polymer, the nano fluorine-contained polyaryletherketone high polymer alloy of titanium hybrid copolymers, matrix resin, nano organic titanium high polymer alloy coating (coating), oil gas well drilling tool or pipeline, speciality coating, extraordinary application; It with nano organic titanium polymer and nanometer alumina modified fluorinated poly arylene ether ketone polymer reformation copolymerization, has prepared the nano fluorine-contained polyaryletherketone high-molecular copolymer of a kind of titanium novel material by adopting previous patent of invention achievement; The nano organic titanium high polymer alloy coating that makes with this novel material has obtained successful application in the corrosion-proof coating protection engineering of oil-gas field well drilling tool and well casing again; The performance of the comparable previous patent of invention product of this novel material " nano ceramic film coating and organic titanium special anticorrosive erosion coating " is excellent more, the protection life-span prolongs several times, spoke reduces the cost of winning and the maintenance of equipment expense of oil and natural gas greatly, thereby has improved the comparability relative productivity significantly;
(2) the present invention is intended to prepare a kind of high-performance polymer by the modification technology that adopts nano material, and with this speciality coating product as base-material exploitation series, for opening up a new way in industrial antisepsis erosion field; Experiment product of the present invention is breathed out field use test (wouldn't externally disclose) at Xinjiang Karamay oilfield, oil field, Tarim Basin, soil, obtained the very satisfied effect of user, for technical barrier has been captured in the protection of underground high sulfur content exploitation of oil-gas field equipment, also for China's oil and natural-gas field deep mining equipment selected high-performance protective coating production domesticization, provide novel material for special anticorrosive erosion coating project field.
Embodiment
The preparation method of the nano fluorine-contained poly (aryl ether ketone) copolymer of titanium of the present invention comprises that the chemosynthesis reaction course is shown in following reaction formula:
Polymerization degree n in the formula 〉=8;
Be nano aluminium oxide.
For finishing above chemosynthesis reaction, concrete implementation step is as follows:
The first step prepares the nano fluorine-contained poly (aryl ether ketone) copolymer required equipment of titanium and the detailed row of starting material are as follows:
1. major equipment: 1. QM-1SP4 closed planetary ball mill reactor; 2. LBM-T1 type frequency-conversion high-speed dispersion machine; 3. LBM-T2 frequency conversion basket type sand mill.
2. main raw material(s): 1. base-material raw material: nano organic titanium high molecular polymer (HTH); Nanometer alumina modified fluorinated poly arylene ether ketone polymer [(PAEK_F-Al
2O
3)
n x].2. auxiliary agent class: (Al
2O
2)
XNMP 2-The nano modification catalyzer; The PBT catalyzer; ZD-401, SF-560 coupling agent; Coatings additive(s)s such as F108S, F118C, F881B, ADP, L612P, L613P, PTFE-2U.3. color stuffing: Mitsubishi's carbon black; Iron mica.4. grinding medium: Stainless Steel Ball: four kinds of ф 20mm, ф 15mm, ф 10mm, ф 5mm; Its cooperation ratio is: 10: 20: 30: 40 (wt, %).
The nano fluorine-contained poly (aryl ether ketone) copolymer of the second step preparation titanium: take by weighing HTH 600g, NMP 230g, MEK 70g, (PAEK_F-Al
2O
3)
n x220g, PBT catalyzer 40g, (Al
2O
2)
XNMP 2-40g, ZD-401 auxiliary agent 10g, SF-560 auxiliary agent 10g add up to 1200g, are respectively charged into by equivalent in 4 jars of closed planetary ball mill reactor, add 3/4ths places of Stainless Steel Ball to jar internal volume by proportioning, screw the bolt seal cover then.Start the ball-milling reaction device and enter normal operation, the reaction times of grinding operation approximately needs 5～6h.Behind the operation 3h, the airtight situation of shutdown inspection also writes down vertical metallic thermometer of grinding pot and barometric data.Later every operation 1h shutdown inspection also writes down a secondary data.When temperature in the jar reaches required temperature (about 180 ℃) of reaction and pressure (about 0.6MPa), allow the ball milling reaction times continue 1h and shut down.After the question response jar naturally cools to normal temperature, open jar and filter out steel ball, the particle diameter that obtains black mud shape is about " the nano fluorine-contained poly (aryl ether ketone) copolymer of titanium " of 60～80nm, solids content 〉=65%.It is a body material of making nano organic titanium high polymer alloy coating.
(trade name is the 3rd step preparation nano organic titanium high polymer alloy base coat: oil-gas field well specific drilling tool pipeline special anticorrosive priming paint): take by weighing (T_PAEK_F)
XNMP n270g, (PAEK_F-Al
2O
3)
n x80g, NMP 120g, MEK 30g, F108S (dispersion agent) 5g, F118C (anti-settling agent) 5g, F881B (thixotropic agent) 10g, ADP (adhesive agent) 10g, 1250 order super-fine zinc dust 500g, add up to 1030g to put into abrading cylinder, high speed dispersion 60min on LBM-T1 type dispersion machine, reach requirement fineness (≤40 μ m) and viscosity (be coated with-4 glasss 〉=80s), promptly available 300 mesh filter screen cloth filter, packing.
(trade name is the 4th step preparation nano organic titanium high polymer alloy top coat: oil-gas field well specific drilling tool pipeline special anticorrosive finish paint): take by weighing (T_PAEK_F)
XNMP n300g, (PAEK_F-Al
2O
3)
n x150g, NMP 200g, MEK 40g, (Al
2O
2)
XNMP 2-50g, F108S 10g, F118C 10g, F881B10g, ADP 10g, PTFE-2U (tetrafluoroethylene wax powder) 20g, the carbon black 20g of Mitsubishi, iron mica (ash) 200g, L612P (flow agent) 5g, L613P (defoamer) 5g, add up to 1030g to put into abrading cylinder, the high speed dispersion 20min on LBM-T1 type dispersion machine of elder generation, move to then be ground on the LBM-T2 type basket type sand mill require fineness (≤15 μ m) and viscosity (be coated with-4 glasss 〉=80s), promptly available 300 mesh filter screen cloth filter, packing.
The check of coating products physicochemical property of the present invention, still not having national standard and industry standard at present can reference, so rely on cooperative enterprise with reference to the special technical requirement of oil field to the oil country tubular good erosion shield, has worked out corresponding company standard.
Claims (7)
1. nano fluorine-contained poly (aryl ether ketone) copolymer of titanium is characterized in that its molecular structural formula is as follows:
Polymerization degree n in the formula 〉=8;
Be nano aluminium oxide.
2. make the method that aforesaid right requires the nano fluorine-contained poly (aryl ether ketone) copolymer of 1 described titanium for one kind, it is characterized in that, comprise following making step:
The first step takes by weighing each component by formula ratio, adds the nano organic titanium oligopolymer in the closed planetary ball mill reactor of packing into special in order, adds nano aluminium oxide fluorinated poly arylene ether ketone again, then by sealed tank cap behind the Stainless Steel Ball of proportioning adding different-grain diameter;
Second step started the ball-milling reaction device and enters normal operation, grind and to be less than 3h working time, behind the operation 1h, shutdown inspection, later every upper end metallic thermometer of operation 1h shutdown inspection record and barometric data, prepolymer is under the effect of carrier NMP or tetramethylene sulfone and catalyst, heat up through grinding, temperature, accumulation of pressure be to the required temperature and pressure of reaction in jar, that is: jar in when temperature＞180 ℃, pressure for vaporization＞20MPa, polycondensation begins; Then, allowing the ball milling reaction times continue 1h again can shut down;
After the 3rd step, the question response jar naturally cooled to normal temperature, open jar and filter out Stainless Steel Ball, obtain the polymerisate of black mud shape, its particle diameter is about 50～80nm.
3. according to the method for the nano fluorine-contained poly (aryl ether ketone) copolymer of the described manufacturing titanium of claim 3, it is characterized in that, described making method is called " TFPK method ", and with the chemical product called after " the nano fluorine-contained poly (aryl ether ketone) copolymer of titanium " that this method makes, skeleton symbol is (T_PAEK_F)
XNMP n, (T_PAEK_F) wherein
x nBe polymkeric substance, NMP is a solvent carrier.
4. purposes of the nano fluorine-contained poly (aryl ether ketone) copolymer of titanium according to claim 1, it is characterized in that, with the nano fluorine-contained poly (aryl ether ketone) copolymer of titanium is the film forming matrix resin, compositely process speciality coating with anti-corrosion property with coatings additive(s), pigment and/or rust-stabilising pigment, functional stuffing, polar solvent etc., this speciality coating is called the nano fluorine-contained polyaryletherketone high polymer alloy of titanium polymer coating, is abbreviated as " TPFK ".
5. according to the purposes of the nano fluorine-contained poly (aryl ether ketone) copolymer of the described titanium of claim 4, it is characterized in that, above-mentioned speciality coating with anti-corrosion property, it specifically is applied to the coating protection of oil-gas field deep-well drill tool or pipeline.
6. according to the purposes of the nano fluorine-contained poly (aryl ether ketone) copolymer of the described titanium of claim 4, it is characterized in that, the nano fluorine-contained poly (aryl ether ketone) copolymer of described titanium is the film forming matrix resin, composite with it and color stuffing, chemical assistant and polar solvent, use the general-purpose equipment and the conventional working method of producing coating, produce the extraordinary industrial antisepsis coating of different purposes.
7. one kind is utilized the nano fluorine-contained poly (aryl ether ketone) copolymer of titanium as the film forming matrix resin material of making speciality coating as described in claim 4, and the reaction formula of its manufacturing processed is as follows:
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|---|---|---|---|
| CN200810198419A CN101671438A (en) | 2008-09-08 | 2008-09-08 | Titanium and nano fluorine-containing poly (aryl ether ketone) copolymer, coating made thereof and manufacturing method thereof |
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|---|---|---|---|
| CN200810198419A CN101671438A (en) | 2008-09-08 | 2008-09-08 | Titanium and nano fluorine-containing poly (aryl ether ketone) copolymer, coating made thereof and manufacturing method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103819683A (en) * | 2014-02-28 | 2014-05-28 | 江苏金陵特种涂料有限公司 | A novel titanium nanometer polymer alloy material and a preparation method thereof |
| CN103881106A (en) * | 2014-02-28 | 2014-06-25 | 江苏金陵特种涂料有限公司 | Preparation method for titanium nanometer high-polymer alloy oilwell pipe coating material |
| CN103881109A (en) * | 2014-03-26 | 2014-06-25 | 江苏金陵特种涂料有限公司 | Titanium nano macromolecule alloy base material as well as preparation method and equipment thereof |
| CN103881563B (en) * | 2014-03-03 | 2017-04-26 | 江苏金陵特种涂料有限公司 | Titanium nanometer polymer alloy coating material and application method thereof |
-
2008
- 2008-09-08 CN CN200810198419A patent/CN101671438A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103819683A (en) * | 2014-02-28 | 2014-05-28 | 江苏金陵特种涂料有限公司 | A novel titanium nanometer polymer alloy material and a preparation method thereof |
| CN103881106A (en) * | 2014-02-28 | 2014-06-25 | 江苏金陵特种涂料有限公司 | Preparation method for titanium nanometer high-polymer alloy oilwell pipe coating material |
| CN103881563B (en) * | 2014-03-03 | 2017-04-26 | 江苏金陵特种涂料有限公司 | Titanium nanometer polymer alloy coating material and application method thereof |
| CN103881109A (en) * | 2014-03-26 | 2014-06-25 | 江苏金陵特种涂料有限公司 | Titanium nano macromolecule alloy base material as well as preparation method and equipment thereof |
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