CN104403644A - Self-dissolving material and preparation method thereof - Google Patents
Self-dissolving material and preparation method thereof Download PDFInfo
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- CN104403644A CN104403644A CN201410609926.0A CN201410609926A CN104403644A CN 104403644 A CN104403644 A CN 104403644A CN 201410609926 A CN201410609926 A CN 201410609926A CN 104403644 A CN104403644 A CN 104403644A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- 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
- C09K8/60—Compositions for stimulating production by acting on the underground formation
- C09K8/62—Compositions for forming crevices or fractures
- C09K8/66—Compositions based on water or polar solvents
- C09K8/665—Compositions based on water or polar solvents containing inorganic compounds
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- 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
- C09K8/60—Compositions for stimulating production by acting on the underground formation
- C09K8/84—Compositions based on water or polar solvents
- C09K8/845—Compositions based on water or polar solvents containing inorganic compounds
Abstract
The invention discloses a self-dissolving material and a preparation method thereof, and the preparation method comprises the following steps: (1) providing at least two metal materials and ceramic powder with porous or multilayer microstructure as raw materials; and (2) compounding the raw materials to from the self-dissolving material by powder metallurgy process or melting and casting forming process. The self-dissolving material not only has high mechanical strength, but also can be automatically dissolved in an electrolyte solution, so that the self-dissolving material can be widely applied to the development of oil and gas and other mineral resources, can be completely soluble underground without returning operation, and greatly improves the production efficiency.
Description
Technical field
The present invention relates to a kind of from dissolved material and preparation method thereof.
Background technology
When mineral products (such as oil gas) mining operations, often need to drop into some material with specific function (such as bridging plug, pressure break ball) to down-hole.These materials can hinder the operation of next step operation after completing mission, and the past adopts the row's of returning operation to be returned to ground usually, and this just increases operating cost greatly, reduces production efficiency.
Summary of the invention
The object of the present invention is to provide a kind of from dissolved material and preparation method thereof, prepared from dissolved material can in electrolyte solution automatic dissolving.
According to an aspect of the present invention, a kind of preparation method from dissolved material is provided, comprises the following steps:
(1) at least two kinds of raw metals are provided and there is the ceramic powder of porous or multilayer microtexture as raw material;
(2) powder metallurgical technique or melting casting molding process is adopted to be compounded to form above-mentioned raw materials from dissolved material.
Under preferable case, two or more in raw metal chosen from Fe, magnesium, aluminium, copper, silicon, calcium, nickel, zinc, titanium.
Under preferable case, ceramic powder be selected from diatomite, zeolite, white carbon black, mica, vermiculite one or more.
Under preferable case, wherein ceramic powder raw material before combination first by chemical plating technology at its Surface coating skim metal.Particularly, chemical plating technology adopts ceramic powder raw material to join in the ammonia solution of metal-salt, then obtain the ceramic powder of metallic cover by pressurized hydrogen reducing process.Particularly, coated sheet metal is identical with at least one in raw metal.
Under preferable case, also comprise step:
(3) desired shape and size will be become from dissolving materials processing after shaping, forming inner core;
(4) in the coated layer of metal of interior core outer surface, shell is formed.
Under further preferable case, in identical electrolyte solution, the dissolution rate of shell is less than the dissolution rate of inner core.
According to a second aspect of the invention, provide prepared by a kind of above-mentioned preparation method from dissolved material.
By prepared by the present invention from dissolved material, not only there is higher mechanical strength, can also dissolve voluntarily in electrolyte solution.Thus can be widely applied in the exploitation of the Mineral resources such as oil gas, can be implemented in down-hole completely solvable, do not need to return operation, substantially increase production efficiency.
Embodiment
Below by specific embodiment, the preparation method from dissolved material of the present invention (process) is described, the metal used in its Raw is all commercially available industrial raw material, according to different moulding processs, can select bulk or powder, purity is generally at more than 97wt%.The diatomite used, zeolite, mica and vermiculite raw material all directly adopt natural mineral to form through pulverizing, particular requirement be there is no to its purity, in order to contrast, the ceramic powder illustrated in the examples below all adopts the particle diameter of below 325 orders, but it should be appreciated by those skilled in the art that in other embodiments also can for being greater than 325 object particle diameters.The white carbon black used is obtained by vapor phase process or the precipitator method, there is no particular requirement to its purity.The chemical plating technology adopted in embodiment carries out in autoclave, first metal-salt (such as single nickel salt, zinc sulfate) is dissolved in ammonia soln, again ceramic powder is joined in solution, pass into hydrogen, at the pressure of 1-5MPa, 80-200 DEG C, react after 1-4 hour, gained throw out is carried out washing, filter and drying, the ceramic powder of obtained metallic cover.The thickness of clad metal is between 5-30 micron.Powder metallurgical technique described herein or melting casting molding process are all technique means well-known to those skilled in the art, therefore no longer describe in detail.
embodiment 1
Magnesium powder, iron powder and kieselguhr micropowder are fully mixed according to mass ratio 4:4:2, the granularity of each powder is all below 325 orders.Add appropriate polyvinyl alcohol adhesive after mixing, then powder mix is loaded mould and be pressed into base substrate in advance on pressing machine.Base substrate is put into High Temperature Furnaces Heating Apparatus, at 1200 DEG C, sintering 2 hours under argon gas atmosphere protection, obtained fine and close finished product.
embodiment 2
Aluminium powder, iron powder and zeolite micro mist are fully mixed according to mass ratio 5:4:1, the granularity of each powder is all below 325 orders.Add appropriate polyvinyl alcohol adhesive after mixing, then powder mix is loaded mould and be pressed into base substrate in advance on pressing machine.Base substrate is put into High Temperature Furnaces Heating Apparatus, at 800 DEG C, sintering 2 hours under argon gas atmosphere protection, obtained fine and close finished product.
embodiment 3
Copper powder, iron powder, aluminium powder and Ultrafine Mica are fully mixed according to mass ratio 3:3:3:1, the granularity of each powder is all below 325 orders.Add appropriate polyvinyl alcohol adhesive after mixing, then powder mix is loaded mould and be pressed into base substrate in advance on pressing machine.Base substrate is put into High Temperature Furnaces Heating Apparatus, at 1000 DEG C, sintering 2 hours under nitrogen atmosphere protection, obtained fine and close finished product.
embodiment 4
Magnesium powder, silica flour and white carbon black micro mist are fully mixed according to mass ratio 4.5:4.5:1, the granularity of each powder is all below 325 orders.Powder mix is directly put in the mould of hot pressing furnace, 750 DEG C, under argon gas atmosphere protection pressurization (35MPa) sinter 2 hours, obtained fine and close finished product.
embodiment 5
First by kieselguhr micropowder (below 325 orders) by the coated layer of metal nickel of chemical plating technology, fully mixed according to mass ratio 1:5:4 with nickel powder, silica flour by the kieselguhr micropowder of coated nickel, wherein the granularity of nickel powder, silica flour is all below 325 orders again.Add appropriate polyvinyl alcohol adhesive after mixing, then powder mix is loaded mould and be pressed into base substrate in advance on pressing machine, base substrate is put into High Temperature Furnaces Heating Apparatus, at 1300 DEG C, sintering 2 hours under argon gas atmosphere protection, obtained fine and close finished product.
embodiment 6
First by white carbon black micro mist (below 325 orders) by the coated layer of metal zinc of chemical plating technology, fully mixed according to mass ratio 1:5:4 with zinc powder, calcium powder by the kieselguhr micropowder of coated zinc, wherein the granularity of zinc powder, calcium powder is all below 325 orders again.Add appropriate polyvinyl alcohol adhesive after mixing, then powder mix is loaded mould and be pressed into base substrate in advance on pressing machine, base substrate is put into High Temperature Furnaces Heating Apparatus, at 1300 DEG C, sintering 2 hours under argon gas atmosphere protection, obtained fine and close finished product.
embodiment 7
First by vermiculite micro mist (below 325 orders) by the coated layer of metal titanium of chemical plating technology, more fully mixed according to mass ratio 2:4:4 with titanium valve, magnesium powder by the kieselguhr micropowder of coated titanium, wherein the granularity of titanium valve, magnesium powder is all below 325 orders.Add appropriate polyvinyl alcohol adhesive after mixing, then powder mix is loaded mould and be pressed into base substrate in advance on pressing machine, base substrate is put into High Temperature Furnaces Heating Apparatus, at 1000 DEG C, sintering 2 hours under argon gas atmosphere protection, obtained fine and close finished product.
embodiment 8
MAG block, iron block and kieselguhr micropowder are weighed according to mass ratio 4:4:2, wherein the granularity of kieselguhr micropowder is below 325 orders; Then MAG block is melted together with iron block in vacuum melting furnace; Add diatomite powder after having melted, after carrying out suitable stirring, dissolving liquid is cast in the mould designed in advance, after cooling, form the finished product of desired shape.
embodiment 9
Spelter, calcium block and white carbon black micro mist are weighed according to mass ratio 5:4:1, wherein the granularity of white carbon black micro mist is below 325 orders; Then spelter is melted together with calcium block in vacuum melting furnace; Add white carbon black powder after having melted, after carrying out suitable stirring, dissolving liquid is cast in the mould designed in advance, after cooling, form the finished product of desired shape.
comparative example 1
First titanium valve, magnesium powder are fully mixed according to mass ratio 5:5, wherein the granularity of titanium valve, magnesium powder is all below 325 orders.Add appropriate polyvinyl alcohol adhesive after mixing, then powder mix is loaded mould and be pressed into base substrate in advance on pressing machine, base substrate is put into High Temperature Furnaces Heating Apparatus, at 1000 DEG C, sintering 2 hours under argon gas atmosphere protection, obtained fine and close finished product.
comparative example 2
MAG block, iron block are weighed according to mass ratio 5:5; Then MAG block is melted together with iron block in vacuum melting furnace; After having melted, dissolving liquid is cast in the mould designed in advance, after cooling, forms the finished product of desired shape.
Prepared by above-described embodiment 1-7 can by being machined to desired shape and size from dissolved material.In order to performance test needs, the finished product of above-described embodiment and comparative example gained is processed into the spheroid that diameter is 100mm.Carry out from dissolving performance test in electrolyte solution to spheroid, test is containing 25wt%NaCl, 2wt%MgCl
2with the CaCl of 3wt%
2the aqueous solution in the fracturing liquid of oil-gas mining (simulation) carry out, temperature is 60 DEG C.Start timing to put into electrolyte solution, until spheroid dissolves end (metal ingredient is dissolved into solution, and ceramics component becomes the powder of dispersion) completely, test result is as shown in table 1.
Table 1: spheroid certainly dissolve the performance test results
| Numbering | From dissolution time (minute) |
| Embodiment 1 | 43 |
| Embodiment 2 | 51 |
| Embodiment 3 | 45 |
| Embodiment 4 | 45 |
| Embodiment 5 | 58 |
| Embodiment 6 | 55 |
| Embodiment 7 | 42 |
| Embodiment 8 | 45 |
| Embodiment 9 | 59 |
| Comparative example 1 | 102 |
| Comparative example 2 | 121 |
Performance as can be seen from table 1, spheroid prepared by embodiment 1-9 be all less than 60 minutes from dissolution time, and spheroid prepared by comparative example 1 and 2 be all greater than 100 minutes from dissolution time.Comparative example 1-2 is compared with embodiment 1-9, and raw material is entirely metal, does not adopt ceramic, and other raw material, proportioning and preparation technology are all identical with embodiment 1-7 or close.Thus can find out, the present invention has the ceramic powder of porous or multilayer microtexture owing to have employed in the feed, make prepared greatly accelerating from the dissolution rate of dissolved material, its reason be from dissolved material dissolve time, electrolyte solution can enter into micropore or the microbedding of ceramic composition, greatly accelerates the speed of electrochemical reaction.
Being not limited to from dissolved material prepared by the present invention is dissolved voluntarily in the electrolyte solution of above-mentioned test, it can dissolve voluntarily in the plurality of inorganic salt class aqueous solution, such as sodium-chlor and/or potassium chloride solution, dissolution rate is accelerated along with the temperature rising of electrolyte solution.
In addition, contriver is also unexpected in test to be found, when other preparation technologies are identical, when the proportioning that proportioning is identical, ceramic powder accounts for raw material total mass that two or more the metal adopted in raw material accounts for raw material total mass is separately 10-20%, obtained from dissolved material from dissolution time (see embodiment 1,3,4,7,8, from dissolve all be less than 50 minutes) will faster than other proportionings from dissolved material (see embodiment 2,5,6,9, being all greater than 50 minutes from dissolution time).This may be due under said ratio, and each component from dissolved material formed is the distribution in even dispersion on microcosmic, thus facilitates the carrying out of electrochemical reaction.
Prepare skim metal on ceramic powder surface by chemical plating technology, can protect the porous of ceramic powder or multilayered structure, when ceramic powder and metal-powder can be made to sinter, porous or multilayered structure are not destroyed; The effect in middle layer can also be played simultaneously, promote the sintering between ceramic powder and metal-powder and combination, when particularly coated sheet metal is identical with at least one in the metal-powder in raw material, because consistency is good between same metal.
In some cases (such as during oil gas pressure break production practice), what use during earlier machine bears certain mechanical strength from dissolving material require, just needs its rapid solution to fall after fulfiling assignment.In order to meet the need, present invention also offers a kind of double-deck from dissolved material, it, by becoming desired shape and size by what make in above-described embodiment from dissolving materials processing, forms inner core; Then in the coated layer of metal of interior core outer surface, shell is formed.Wherein, in identical electrolyte solution, the dissolution rate of shell is less than the dissolution rate of inner core.Coated metal different from the metal in kernel (or incomplete same) can be such as one or more in aluminium, titanium, iron, zinc.Cladding process can adopt known plating or gas-phase deposition.The thickness of clad metal rationally can be determined according to the earlier machine time.
It should be appreciated by those skilled in the art that above-described embodiment is only exemplary and list some embodiments.Under spirit according to the invention, other embodiment any can also be adopted to realize the present invention.
Claims (9)
1., from a preparation method for dissolved material, comprise the following steps:
(1) at least two kinds of raw metals are provided and there is the ceramic powder of porous or multilayer microtexture as raw material;
(2) powder metallurgical technique or melting casting molding process is adopted to be compounded to form above-mentioned raw materials from dissolved material.
2. the preparation method from dissolved material according to claim 1, two or more wherein in raw metal chosen from Fe, magnesium, aluminium, copper, silicon, calcium, nickel, zinc, titanium.
3. the preparation method from dissolved material according to claim 1, wherein ceramic powder is selected from one or more in diatomite, zeolite, white carbon black, mica, vermiculite.
4. the preparation method from dissolved material according to claim 1, wherein ceramic powder raw material before combination first by chemical plating technology at its Surface coating skim metal.
5. the preparation method from dissolved material according to claim 4, wherein chemical plating technology adopts ceramic powder raw material to join in the ammonia solution of metal-salt, then obtain the ceramic powder of metallic cover by pressurized hydrogen reducing process.
6. the preparation method from dissolved material according to claim 4, wherein coated sheet metal is identical with at least one in raw metal.
7. the preparation method from dissolved material according to claim 1, also comprises step:
(3) desired shape and size will be become from dissolving materials processing after shaping, forming inner core;
(4) in the coated layer of metal of interior core outer surface, shell is formed.
8. the preparation method from dissolved material according to claim 7, wherein, in identical electrolyte solution, the dissolution rate of shell is less than the dissolution rate of inner core.
9. one kind prepared by the arbitrary described preparation method of claim 1-8 from dissolved material.
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| CN201410609926.0A CN104403644B (en) | 2014-11-03 | 2014-11-03 | From dissolved material and preparation method thereof |
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| CN105001620A (en) * | 2015-07-10 | 2015-10-28 | 北京中科金腾科技有限公司 | Self-dissolving functional material for making well drilling bridge plug rubber packer and preparation method therefor |
| CN106285557A (en) * | 2015-06-05 | 2017-01-04 | 中国石油天然气股份有限公司 | A kind of bridging plug |
| CN108571295A (en) * | 2018-02-09 | 2018-09-25 | 北京中科金腾科技有限公司 | A kind of manufacturing method of solvable slips and the solvable slips manufactured by this method |
| CN112004650A (en) * | 2019-03-25 | 2020-11-27 | 宝洁公司 | Multilayer dissolvable solid article and method of making same |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106285557A (en) * | 2015-06-05 | 2017-01-04 | 中国石油天然气股份有限公司 | A kind of bridging plug |
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| CN112004650A (en) * | 2019-03-25 | 2020-11-27 | 宝洁公司 | Multilayer dissolvable solid article and method of making same |
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| CN104403644B (en) | 2017-03-01 |
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Effective date of registration: 20170524 Address after: Zheng Fu Zhuang village 102607 Beijing city Daxing District anding town north 800 meters Patentee after: BEIJING ZHONGKE JINTENG TECHNOLOGY CO., LTD. Address before: 100035 Beijing city Xicheng District Banbi Street No. 6 Patentee before: Xi Junjie |