CN106830930B - Zirconium oxide ceramic for oil-gas well and preparation method thereof - Google Patents
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Abstract
The invention provides a zirconia ceramic for an oil-gas well and a preparation method thereof, wherein the zirconia ceramic comprises the following raw materials in parts by weight: 60-70 parts of zirconium oxide, 1.5-2.5 parts of hundred million oxide, 0.4-1.2 parts of lanthanum oxide, 0.5-1.5 parts of samarium oxide, 0.5-1.5 parts of graphite, 2-4 parts of molybdenum carbide, 1-2 parts of adhesive and 1-2 parts of dispersant. The preparation method comprises the following steps: 1) pretreatment: soaking graphite and molybdenum carbide in dilute nitric acid, and then carrying out solid-liquid separation to obtain pretreated graphite and molybdenum carbide; 2) ball-milling each component to obtain slurry; 3) and (3) granulation: carrying out spray granulation on the slurry; 4) manufacturing a sheath; 5) cold isostatic pressing; 6) and sintering the blank. The friction coefficient of the ceramic is low, and the problems that the zirconia ceramic material is high in sintering temperature and easy to damage an expansion pipe due to overlarge friction coefficient at high temperature are solved.
Description
Technical Field
The invention belongs to the technical field of ceramics, and particularly relates to zirconia ceramics for an oil-gas well and a preparation method thereof.
Background
The expansion pipe technology is widely applied to drilling, well completion and well repairing operations of oil and gas fields, and particularly has obvious technical advantages in aspects of subsiding casing leakage or corroding well sections, subsiding reinforcement after channeling of casing deformation wells, blocking perforation intervals, blocking high water-yielding intervals, adding deep wells, completing side drilling wells and the like. The expansion pipe technology is that under the action of hydraulic or mechanical force, an expansion core head is driven to move longitudinally in an expansion pipe, and an expansion section of the expansion core head extrudes the inner wall of the expansion pipe to cause the expansion pipe to generate permanent plastic deformation so as to be tightly attached to the inner wall of a casing or an open hole well section. In the operation process of a high-sulfur gas field, the operation needs to be carried out in an environment with the temperature of 120 ℃ and high sulfur and carbon dioxide, and a high-temperature-resistant, wear-resistant and sulfur-resistant expansion core head is urgently needed.
At present, the materials of the expansion core heads adopted by expansion pipe patching and well completion are mostly common carbon steel materials. The plug-in type expansion head disclosed by ZL201110343666.3 and the expansion tool disclosed by ZL200920164454.7 both adopt high-hardness steel materials and are designed in an integrated mode, but the plug-in type expansion head and the expansion tool do not have the sulfur resistance. The sintering temperatures of the zirconia ceramic materials are 1550-1600 ℃ and 1650-1800 ℃ respectively, and the sintering temperature of the zirconia ceramic is too high to be beneficial to production and operation; simultaneously, in the expansion pipe work progress, the expansion core head can produce very big frictional force to the expansion pipe, and then produces the damage to the expansion pipe, is unfavorable for later stage production.
Disclosure of Invention
The invention provides a zirconia ceramic for an oil-gas well, which is low in friction coefficient and solves the problems that a zirconia ceramic material is high in sintering temperature and high in friction coefficient at high temperature and easily damages an expansion pipe.
The technical scheme of the invention is realized as follows:
the zirconia ceramic for the oil-gas well comprises the following raw materials in parts by weight:
60-70 parts of zirconium oxide, 1.5-2.5 parts of hundred million oxide, 0.4-1.2 parts of lanthanum oxide, 0.5-1.5 parts of samarium oxide, 0.5-1.5 parts of graphite, 2-4 parts of molybdenum carbide, 1-2 parts of adhesive and 1-2 parts of dispersant; wherein, the graphite and the molybdenum carbide need to be soaked by dilute nitric acid and then subjected to solid-liquid separation.
Preferably, in some embodiments of the present invention, the concentration of the dilute nitric acid is 0.5 to 3 mol/L.
Preferably, in some embodiments of the present invention, the binder is methyl cellulose or ethyl cellulose.
Preferably, in some embodiments of the present invention, the dispersant is a polyacrylate.
Preferably, in some embodiments of the present invention, the polyacrylate salt is ammonium polymethacrylate or ethyl polymethacrylate.
The invention also aims to provide a preparation method of the zirconia ceramic for the oil-gas well, which comprises the following steps:
1) pretreatment: soaking graphite and molybdenum carbide in dilute nitric acid, and then carrying out solid-liquid separation to obtain pretreated graphite and molybdenum carbide;
2) ball milling powder: weighing zirconium oxide, hundred million oxide, lanthanum oxide and samarium oxide according to a ratio, mixing the zirconium oxide, the hundred million oxide, the lanthanum oxide and the samarium oxide with pretreated graphite and molybdenum carbide, adding the mixture into a ball mill to form mixed powder, respectively adding an adhesive and a dispersant into the mixed powder, and then starting the ball mill to obtain slurry;
3) and (3) granulation: spray drying the slurry obtained in the step 2) in a granulation spray tower to remove water in the slurry to obtain granulated powder;
4) manufacturing a sheath: manufacturing a steel mould according to the size of an expansion section of the expansion core head, heating the steel mould to 190 ℃ in an oven, putting the heated steel mould into a prepared polyvinyl chloride material, putting the steel mould into the oven at 190 ℃ again for heating after the outer surface of the steel mould is uniformly hung, taking out the steel mould after 10-15 min, putting the steel mould into water, and quickly taking off a sheath from the mould;
5) cold isostatic pressing: placing the granulated powder obtained in the step 3) into a prepared sheath, performing preforming pressing and cold isostatic pressing to obtain a blank of an expansion section of the expansion core head, wherein the preforming working pressure is 280-330 kg/cm2The cold isostatic pressing working pressure is 1500-1700 kg/cm2After pressing, carrying out secondary processing on the blank to ensure that the size of the expansion section meets the manufacturing requirement;
6) sintering a blank: sintering the green body in the step 5), wherein the sintering temperature is 1150-1260 ℃, and preserving heat for 6-8 hours to obtain the zirconium oxide ceramic for the oil-gas well.
Preferably, in some embodiments of the present invention, the binder is methyl cellulose or ethyl cellulose.
Preferably, in some embodiments of the present invention, the dispersant is a polyacrylate.
Preferably, in some embodiments of the present invention, the polyacrylate salt is ammonium polymethacrylate or ethyl polymethacrylate.
The invention has the beneficial effects that:
1. the compactness of the zirconia ceramic is obviously improved by the composite addition of yttrium oxide, lanthanum oxide and samarium oxide, and the rare earth oxide is a very good surface active substance, so that the wettability of the material can be improved, the sintering temperature can be reduced finally, and the processing difficulty and the processing cost of the zirconia ceramic expansion core head are reduced.
2. Through multiple experiments, the inventor finds that graphite and molybdenum carbide are subjected to dilute nitric acid soaking treatment, the graphite and the molybdenum carbide are completely soaked in the soaking treatment, the traditional lubricating additives such as molybdate, magnesium oxide and the like are replaced, the friction coefficient of zirconia ceramics at the temperature of 120 ℃ can be remarkably reduced, the porosity of the material is rapidly reduced, the density of the material is increased, and the sintering temperature of a tetragonal polycrystalline zirconia (TZP) material is greatly reduced.
Detailed Description
Example 1
The zirconia ceramic for the oil-gas well comprises the following raw materials in parts by weight:
62 parts of zirconium oxide, 2 parts of hundred million oxide, 0.5 part of lanthanum oxide, 1.5 parts of samarium oxide, 1 part of graphite, 2 parts of molybdenum carbide, 1 part of methyl cellulose and 1 part of ammonium polymethacrylate; wherein, the graphite and the molybdenum carbide need to be soaked by dilute nitric acid and then subjected to solid-liquid separation.
The preparation method comprises the following steps:
1) pretreatment: soaking graphite and molybdenum carbide in 1mol/L dilute nitric acid for 30min, and then carrying out solid-liquid separation to obtain pretreated graphite and molybdenum carbide;
2) ball milling powder: weighing zirconium oxide, hundred million oxide, lanthanum oxide and samarium oxide according to a ratio, mixing the zirconium oxide, the hundred million oxide, the lanthanum oxide and the samarium oxide with pretreated graphite and molybdenum carbide, adding the mixture into a ball mill to form mixed powder, respectively adding methylcellulose and ammonium polymethacrylate into the mixed powder, and then starting the ball mill to obtain slurry;
3) and (3) granulation: spray drying the slurry obtained in the step 2) in a granulation spray tower to remove water in the slurry to obtain granulated powder;
4) manufacturing a sheath: manufacturing a steel mould according to the size of an expansion section of the expansion core head, heating the steel mould to 190 ℃ in an oven, putting the heated steel mould into a prepared polyvinyl chloride material, putting the steel mould into the oven at 190 ℃ again for heating after the outer surface of the steel mould is uniformly hung, taking out the steel mould after 10min, putting the steel mould into water, and quickly taking off a sheath from the mould;
5) cold isostatic pressing: putting the granulation powder in the step 3) into the prepared productPerforming pre-forming pressing and cold isostatic pressing treatment in the sheath to obtain a blank of an expansion section of the expansion core head, wherein the pre-forming working pressure is 300kg/cm2The cold isostatic pressing working pressure is 1600kg/cm2After pressing, carrying out secondary processing on the blank to ensure that the size of the expansion section meets the manufacturing requirement;
6) sintering a blank: sintering the green body obtained in the step 5), wherein the sintering temperature is 1200 ℃, and keeping the temperature for 7 hours to obtain the zirconium oxide ceramic for the oil-gas well.
Example 2
The zirconia ceramic for the oil-gas well comprises the following raw materials in parts by weight:
70 parts of zirconium oxide, 1.5 parts of hundred million oxide, 0.4 part of lanthanum oxide, 0.5 part of samarium oxide, 1.5 parts of graphite, 4 parts of molybdenum carbide, 2 parts of ethyl cellulose and 2 parts of ammonium polymethacrylate; wherein, the graphite and the molybdenum carbide need to be soaked by dilute nitric acid and then subjected to solid-liquid separation.
The preparation method comprises the following steps:
1) pretreatment: soaking graphite and molybdenum carbide in 0.5mol/L dilute nitric acid for 40min, and performing solid-liquid separation to obtain pretreated graphite and molybdenum carbide;
2) ball milling powder: weighing zirconium oxide, hundred million oxide, lanthanum oxide and samarium oxide according to a ratio, mixing the zirconium oxide, the hundred million oxide, the lanthanum oxide and the samarium oxide with pretreated graphite and molybdenum carbide, adding the mixture into a ball mill to form mixed powder, respectively adding ethyl cellulose and ammonium polymethacrylate into the mixed powder, and then starting the ball mill to obtain slurry;
3) and (3) granulation: spray drying the slurry obtained in the step 2) in a granulation spray tower to remove water in the slurry to obtain granulated powder;
4) manufacturing a sheath: manufacturing a steel mould according to the size of an expansion section of the expansion core head, heating the steel mould to 190 ℃ in an oven, putting the heated steel mould into a prepared polyvinyl chloride material, putting the steel mould into the oven at 190 ℃ again for heating after the outer surface of the steel mould is uniformly hung, taking out the steel mould after 15min, putting the steel mould into water, and quickly taking off a sheath from the mould;
5) cool equal quietPressing: placing the granulated powder obtained in the step 3) into a prepared sheath, performing preforming pressing and cold isostatic pressing to obtain a blank of an expansion section of the expansion core head, wherein the preforming working pressure is 330kg/cm2The cold isostatic pressing working pressure is 1500kg/cm2After pressing, carrying out secondary processing on the blank to ensure that the size of the expansion section meets the manufacturing requirement;
6) sintering a blank: sintering the green body obtained in the step 5), wherein the sintering temperature is 1150 ℃, and preserving heat for 6 hours to obtain the zirconium oxide ceramic for the oil-gas well.
Example 3
The zirconia ceramic for the oil-gas well comprises the following raw materials in parts by weight:
60 parts of zirconium oxide, 2.5 parts of hundred million oxide, 1.2 parts of lanthanum oxide, 1.5 parts of samarium oxide, 0.5 part of graphite, 2 parts of molybdenum carbide, 1.5 parts of ethyl cellulose and 1.5 parts of ammonium polymethacrylate; wherein, the graphite and the molybdenum carbide need to be soaked by dilute nitric acid and then subjected to solid-liquid separation.
The preparation method comprises the following steps:
1) pretreatment: soaking graphite and molybdenum carbide in 3mol/L dilute nitric acid for 20min, and performing solid-liquid separation to obtain pretreated graphite and molybdenum carbide;
2) ball milling powder: weighing zirconium oxide, hundred million oxide, lanthanum oxide and samarium oxide according to a ratio, mixing the zirconium oxide, the hundred million oxide, the lanthanum oxide and the samarium oxide with pretreated graphite and molybdenum carbide, adding the mixture into a ball mill to form mixed powder, respectively adding ethyl cellulose and ammonium polymethacrylate into the mixed powder, and then starting the ball mill to obtain slurry;
3) and (3) granulation: spray drying the slurry obtained in the step 2) in a granulation spray tower to remove water in the slurry to obtain granulated powder;
4) manufacturing a sheath: manufacturing a steel mould according to the size of an expansion section of the expansion core head, heating the steel mould to 190 ℃ in an oven, putting the heated steel mould into a prepared polyvinyl chloride material, putting the steel mould into the oven at 190 ℃ again for heating after the outer surface of the steel mould is uniformly hung, taking out the steel mould after 12min, putting the steel mould into water, and quickly taking off a sheath from the mould;
5) cold isostatic pressing: placing the granulated powder obtained in the step 3) into a prepared sheath, performing preforming pressing and cold isostatic pressing to obtain a blank of an expansion section of the expansion core head, wherein the preforming working pressure is 280kg/cm2The cold isostatic pressing working pressure is 1700kg/cm2After pressing, carrying out secondary processing on the blank to ensure that the size of the expansion section meets the manufacturing requirement;
6) sintering a blank: sintering the green body obtained in the step 5), wherein the sintering temperature is 1260 ℃, and keeping the temperature for 8 hours to obtain the zirconia ceramics for the oil-gas well.
Comparative example 1
(1) Adding zirconium oxide, magnesium oxide, aluminum oxide, yttrium oxide, lanthanum oxide and samarium oxide into a ball mill according to the following weight to form mixed powder, wherein ZrO is2，74kg；MgO，16kg；Al2O3，4.4kg；Y2O3，2kg；La2O3，1kg；Sm2O30.6 kg. Adding 0.8kg of ethyl cellulose and 1.2kg of ammonium polymethacrylate into the mixed powder, and then performing ball milling on the mixture by using a ball mill to obtain slurry;
(2) spray-drying the slurry obtained in the step (1) in a granulation spray tower, and removing water in the slurry to obtain granulated powder;
(3) the sheath is made of polyvinyl chloride materials, and the proportion of the polyvinyl chloride materials is as follows: 49kg of polyvinyl chloride resin; 49kg of dioctyl phthalate; 1.85kg of tribasic lead sulfate; 0.15kg of stearic acid, heating the manufactured steel mould to 180 ℃ in an oven, putting the heated mould into the prepared polyvinyl chloride material, putting the mould subjected to material hanging into the oven at 180 ℃ again for heating, taking out the mould after the slurry turns yellow after 10min, putting the mould into water, and quickly taking off the sheath from the mould;
(4) and (3) putting the prefabricated granulation powder into the prepared sheath, and then performing preforming pressing and cold isostatic pressing to obtain a blank of the expansion section of the expansion core head. The preforming pressure is 300kg/cm2. The cold isostatic pressing working pressure is 1500kg/cm2. After pressing the blank, processing the blank to the size of the expansion section according to requirements;
(5) and sintering the blank. And sintering the green body at 1350 ℃ for 7 hours.
The mechanical properties of examples 1-3 were compared with comparative example 1, and the specific results are shown in Table 1:
TABLE 1 mechanical Properties of examples 1-3 and comparative example 1
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (8)
1. The zirconia ceramic for the oil-gas well is characterized by comprising the following raw materials in parts by weight:
60-70 parts of zirconium oxide, 1.5-2.5 parts of hundred million oxide, 0.4-1.2 parts of lanthanum oxide, 0.5-1.5 parts of samarium oxide, 0.5-1.5 parts of graphite, 2-4 parts of molybdenum carbide, 1-2 parts of adhesive and 1-2 parts of dispersant; wherein, the graphite and the molybdenum carbide need to be soaked by dilute nitric acid and then subjected to solid-liquid separation.
2. The zirconia ceramic for oil and gas wells according to claim 1, wherein the binder is methyl cellulose or ethyl cellulose.
3. The zirconia ceramic for oil and gas wells of claim 1, wherein the dispersant is a polyacrylate.
4. The zirconia ceramic for oil and gas wells according to claim 3, wherein the polyacrylate is ammonium polymethacrylate or polyethylmethacrylate.
5. The method for preparing the zirconia ceramic for oil and gas wells according to claim 1, comprising the steps of:
1) pretreatment: soaking graphite and molybdenum carbide in dilute nitric acid, and then carrying out solid-liquid separation to obtain pretreated graphite and molybdenum carbide;
2) ball milling powder: weighing zirconium oxide, hundred million oxide, lanthanum oxide and samarium oxide according to a ratio, mixing the zirconium oxide, the hundred million oxide, the lanthanum oxide and the samarium oxide with pretreated graphite and molybdenum carbide, adding the mixture into a ball mill to form mixed powder, respectively adding an adhesive and a dispersant into the mixed powder, and then starting the ball mill to obtain slurry;
3) and (3) granulation: spray drying the slurry obtained in the step 2) in a granulation spray tower to remove water in the slurry to obtain granulated powder;
4) manufacturing a sheath: manufacturing a steel mould according to the size of an expansion section of the expansion core head, heating the steel mould to 190 ℃ in an oven, putting the heated steel mould into a prepared polyvinyl chloride material, putting the steel mould into the oven at 190 ℃ again for heating after the outer surface of the steel mould is uniformly hung, taking out the steel mould after 10-15 min, putting the steel mould into water, and quickly taking off a sheath from the mould;
5) cold isostatic pressing: placing the granulated powder obtained in the step 3) into a prepared sheath, performing preforming pressing and cold isostatic pressing to obtain a blank of an expansion section of the expansion core head, wherein the preforming working pressure is 280-330 kg/cm2The cold isostatic pressing working pressure is 1500-1700 kg/cm2After pressing, carrying out secondary processing on the blank to ensure that the size of the expansion section meets the manufacturing requirement;
6) sintering a blank: sintering the green body in the step 5), wherein the sintering temperature is 1150-1260 ℃, and preserving heat for 6-8 hours to obtain the zirconium oxide ceramic for the oil-gas well.
6. The method of producing a zirconia ceramic for oil and gas wells according to claim 5, wherein the binder is methyl cellulose or ethyl cellulose.
7. The method of manufacturing a zirconia ceramic for oil and gas wells according to claim 5, wherein the dispersant is polyacrylate.
8. The method for preparing a zirconia ceramic for oil and gas wells according to claim 7, wherein the polyacrylate is ammonium polymethacrylate or polyethylmethacrylate.
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