CN103408264B - Method for preparing low-density cement testing block for oil well cementation by using tantalum carbide microbeads - Google Patents
Method for preparing low-density cement testing block for oil well cementation by using tantalum carbide microbeads Download PDFInfo
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- CN103408264B CN103408264B CN201310388537.5A CN201310388537A CN103408264B CN 103408264 B CN103408264 B CN 103408264B CN 201310388537 A CN201310388537 A CN 201310388537A CN 103408264 B CN103408264 B CN 103408264B
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Abstract
The invention provides a method for preparing a low-density cement testing block for oil well cementation by using closed hollow tantalum carbide microbeads. The method comprises the following steps of: preparing the hollow tantalum carbide microbeads; burdening; mixing; stirring and slurrying; mold testing; and carrying out a strength test. The method is characterized by comprising the following steps of: stirring and slurrying 55wt% to 65wt% (weight percentage) of G-grade oil well cement, 25wt% to 35wt% of the closed hollow tantalum carbide microbeads with the particle diameter from 10 to 150 mu m, 5wt% to 7wt% of coal ash with the ignition loss being 1.1%, 1.5wt% to 2wt% of calcium oxide with the purity being 99.9%, 0.5wt% to 1.0wt% of sodium sulfate and 1wt% to 3wt% of micro-silicon in a stirrer for 40 seconds according to the water-cement ratio being from 0.5 to 0.7 (W/C); pouring the mixture into a group of testing molds (comprising the two testing molds respectively having 53mm, 53mm and 53mm in length, width and height); maintaining the testing molds in a water bath maintenance box for 24 hours and 48 hours at the constant temperature of 52 DEG C; demolding and soaking in cold water for 1 hour; and then performing the strength test.
Description
Technical field
The present invention relates to a kind of method that tantalum carbide closed pore cenosphere prepares the cement briquette of low density oil well cementing, belong to field of material technology.
Background technology
Current domestic well cementation light-weight additive adopts the drift pearl in flyash, and comprise heavy pearl and drift pearl at flyash, heavy pearl density is at 1.1 ~ 2.8g/cm
3between, content accounts for flyash 30 ~ 70%, and drift pearl is the glass microballon being less than water-mass density in flyash, and drift pearl mainly comprises aluminosilicate glass microballon and porous carbon granule, drift pearl after removing carbon granule mainly comprises Thin-walled Aluminum silex glass microballon, surfaces externally and internally is smooth, and volume is large, is that one is rounded, light weight, closed pore are hollow, wear-resisting, high temperature resistant, thermal conductivity is little, intensity is high, drift pearl amount accounts for 0.5 ~ 1% of flyash total amount, and aluminosilicate glass microballon is hollow spherosome.
Drift pearl wherein in flyash it be coal dust in thermal power plant boiler when 1100 ~ 1500 ° of C burning, clayey material melts becomes microlayer model, in stove turbulent flow hot air acting under at a high speed spin, form perfectly round sial spheroid, the gases such as nitrogen, hydrogen and carbonic acid gas that burning and scission reaction produce, undergoes rapid expansion in the high temperature aluminum silicon spheroid of melting, under capillary effect, form the glass envelope of hollow, then enter flue to cool rapidly, after sclerosis, become the vitreous state cenosphere of high vacuum, i.e. fly ash float.
Flyash is put into water stir, leave standstill for some time, because drift pearl density is less than water-mass density, will swim in the water surface pulls out and dry, and be and float pearl.
In recent years, due to the impact of haze weather, the big-and-middle-sized thermal power generation of China adopts the desulfurization technology of environmental protection, and not containing in flyash floats pearl, causes in short supply.
Different according to the well cementation degree of depth, usually being less than the oil well of 2000 meters low hot-well, with highdensity grout, (, between 70 ~ 90 ° of C, namely the density of grout is at 1.8 g/cm for the temperature in oil well in low temperature oil-well well cementation
3~ 1.9 g/cm
3); Be middle hot-well between 2000 ~ 4000 meters, (, between 90 ~ 150 ° of C, namely cement slurry density is at 1.6 g/cm for the temperature in oil well for the grout of middle temperature oil well cementing Midst density
3~ 1.7 g/cm
3); Be greater than 4000 meters for hot hole, with low-density grout, (, between 150 ~ 240 ° of C, namely cement slurry density is at 1.0 g/cm for the temperature in oil well in high-temperature oil well well cementation
3~ 1.5 g/cm
3).
Summary of the invention
The object of the invention is to the defect overcoming prior art existence, provide a kind of cost low, excellent property, can replace the pearl of wafing in flyash, make tantalum carbide closed pore cenosphere by the method for organic synthesis, density range is at 0.5 g/cm
3~ 0.7g/cm
3between, and then configuration low density 1.2 g/cm
3~ 1.5g/cm
3oil well cementing cement briquette, meets the well cementing material requirement of different depths.
its technical scheme is.
Comprise the preparation of tantalum carbide microballon, batching, mixing, stirring is sized mixing, die trial, strength trial, it is characterized in that: by G level oil well cement 55 ~ 65 wt%, particle diameter is closed pore hollow tantalum carbide microballon 25 ~ 35 wt% of 10 ~ 150 μm, flyash 5 ~ 7 wt% of loss on ignition 1.1%, purity 99.9% calcium oxide 1.5 ~ 2 wt%, sodium sulfate 0.5 ~ 1.0 wt% and micro-silicon 1 ~ 3 wt%, with 0.5 ~ 0.7(W/C) water cement ratio stir in stirrer and size mixing 40 seconds, pour die trial (one group of two block length into, wide, high 53mm*53mm*53mm respectively), maintenance 24 hours in the water-bath maintaining box of constant temperature 52 ° of C, 48 hours, soak 1 hour in cold water after the demoulding, make a strength test.
Described a kind of tantalum carbide closed pore cenosphere prepares the method for low density oil well cementing cement briquette, it is characterized in that: particle diameter 1 ~ 30 μm of tantalum oxide is become powder mix than 1:0.8 ~ 1 in stirrer for mixing with phenolic resin weight, solidify at the temperature of 40 ~ 100 ° of C, and then make 50 ~ 100 μm of powder, by 50 ~ 100 μm of powder mixs at 1 ~ 3Mpa briquetting press upper holder block, on the electric furnace of 1300 ~ 1800 ° of C, sintering obtains tantalum carbide block in 5 ~ 8 hours, and the tantalum carbide of bulk is made 5 ~ 30 μm of circular solids microballoons by balling machine.
Described a kind of tantalum carbide closed pore cenosphere prepares the method for low density oil well cementing cement briquette, it is characterized in that: the weight percent of tantalum carbide liquid slurry consists of: 5 ~ 30 μm of tantalum carbide 60 ~ 70 wt%, water 30 ~ 40 wt%.
Described a kind of tantalum carbide closed pore cenosphere prepares the preparation method of low density oil well cementing cement briquette, it is characterized in that: in tantalum carbide liquid slurry, add whipping agent is one in calcium carbonate, potassium sulfate or sodium sulfate, and concentration is 1 ~ 3g/L.
Described tantalum carbide closed pore cenosphere prepares the preparation method of low density oil well cementing cement briquette, it is characterized in that: tantalum carbide liquid is starched abundant agitation and filtration, adopt high speed centrifugation rotary spraying technique, form microballoon, through dehydration expansion, sintering, melting, balling-up on four district's electric furnaces, obtain 10 ~ 150 μm of tantalum carbide closed pore cenospheres through classification.
Described a kind of tantalum carbide closed pore cenosphere prepares the preparation method of low density oil well cementing cement briquette, it is characterized in that: the tantalum carbide closed pore cenosphere its floatability of preparation is greater than 90%.
Described a kind of tantalum carbide closed pore cenosphere prepares the preparation method of low density oil well cementing cement briquette, it is characterized in that: the cement briquette 8 hours ultimate compression strength of preparation is greater than 10MPa, and within 24 hours, ultimate compression strength is greater than 20MPa.
The present invention has the following advantages.
1, lightening material needed for oil well cementing can be made by methodology of organic synthesis.
2, not by the restriction of envrionment conditions, the high-activity carbon that resol can be utilized to be formed prepares tantalum carbide for the complete reduction-oxidation tantalum of carbon source, does not produce impurity.
3, change high-pressure injector head, aperture can change, size tunable, and the particle diameter of particle is determined according to actual needs.
4, this technical matters is advanced, and product performance are stablized, and production cost is low, and output is high, and performance is good.
Embodiment
Embodiment 1.
(1) 1. the preparation of tantalum carbide closed pore cenosphere is prepared: particle diameter 1 ~ 10 μm of tantalum oxide is become powder mix than 1:0.8 in stirrer for mixing with phenolic resin weight, solidify at the temperature of 40 ° of C, and then make 50 μm of powder, by 50 μm of powder mixs at 1Mpa briquetting press upper holder block, on the electric furnace of 1300 degree, sintering obtains tantalum carbide block in 5 hours, and the tantalum carbide of bulk is made 5 μm of circular solids microballoons by balling machine.2. dosing: the weight percent of tantalum carbide liquid slurry consists of: particle diameter 5 μm of tantalum carbide 60 wt%, water 40 wt%, in tantalum carbide liquid slurry, add whipping agent is light calcium carbonate, concentration is 1g/L, 3. stirs: tantalum carbide solution good for proportioning is put into agitator and stirs; 4. filter: by macrobead and Impurity removal; 5. fire: adopt high pressure spraying high speed centrifugation rotary spraying technique, form microballoon, through dehydration expansion, sintering, melting, balling-up on four district's electric furnaces, obtain 50 μm of tantalum carbide closed pore cenospheres through classification.
(2) low density oil well cementing cement briquette batching: get G level oil well cement 65 wt%, 10 ~ 50 μm closed pore hollow tantalum carbide microballon 25 wt%, flyash 5 wt% of loss on ignition 1.1%, purity 99.9% calcium oxide 1.5 wt%, sodium sulfate 0.5 wt% and micro-silicon 3.0 wt%.
(3) mix: get G level oil well cement 65 wt%, closed pore hollow tantalum carbide microballon 25 wt%, flyash 5 wt% of loss on ignition 1.1%, purity 99.9% calcium oxide 1.5 wt%, sodium sulfate 0.5 wt% and micro-silicon 3.0 wt% of 10 ~ 50 μm mix.
(4) get in (3) and mix sample a little, pour in beaker, by the water cement ratio modulation grout of 0.7, stir with glass stick, pour in mud scale and weigh density.
(5) under temperature 28 ° of C ± 1 ° C, with 0.7(W/C) water cement ratio pour corrugation agitator into, under even low speed, all mixed in 20 seconds, then build the lid of agitator, continue to stir 40 seconds under the speed of 4000r/min, leave standstill 5 minutes and observe grout homogeneity.
(6) poured into by the grout be stirred in the die trial of a group two pieces, the specification of die trial is long 53mm, wide 53mm height 53mm.
(7) maintenance 24 hours in the water-bath maintaining box of constant temperature 52 ° of C, soaks 1 hour after the demoulding in cold water, carries out ultimate compression strength and folding strength test and rate of change of the density experiment by the regulation of GB GB/T 177.
(8) maintenance 48 hours in the water-bath maintaining box of constant temperature 52 ° of C, soaks 1 hour after the demoulding in cold water, carries out ultimate compression strength and folding strength test and rate of change of the density experiment by the regulation of GB GB/T 177.
Embodiment 2.
(1) 1. the preparation of tantalum carbide closed pore cenosphere is prepared: particle diameter 10 ~ 20 μm of tantalum oxide are become powder mix than 1:0.9 in stirrer for mixing with phenolic resin weight, solidify at the temperature of 70 ° of C, and then make 70 μm of powder, by 70 μm of powder mixs at 2Mpa briquetting press upper holder block, on the electric furnace of 1500 ° of C, sintering obtains tantalum carbide block in 6 hours, and the tantalum carbide of bulk is made 20 μm of circular solids microballoons by balling machine.2. dosing: the weight percent of tantalum carbide liquid slurry consists of: particle diameter 20 μm of tantalum carbide 65 wt%, water 35 wt%, in tantalum carbide liquid slurry, add whipping agent is potassium sulfate, concentration is 2g/L, 3. stirs: tantalum carbide solution good for proportioning is put into agitator and stirs; 4. filter: by macrobead and Impurity removal; 5. fire: adopt high pressure spraying high speed centrifugation rotary spraying technique, form microballoon, through dehydration expansion, sintering, melting, balling-up on four district's electric furnaces, obtain 60 ~ 100 μm of tantalum carbide closed pore cenospheres through classification.
(2) low density oil well cementing cement briquette batching: G level oil well cement 60 wt%, closed pore hollow tantalum carbide microballon 30 wt%, flyash 6 wt% of loss on ignition 1.1%, purity 99.9% calcium oxide 2.0 wt%, sodium sulfate 0.5 wt% and micro-silicon 1.5 wt% of 60 ~ 100 μm are fully mixed.
(3) mix: G level oil well cement 60 wt%, closed pore hollow tantalum carbide microballon 30 wt%, flyash 6 wt% of loss on ignition 1.1%, purity 99.9% calcium oxide 2.0 wt%, sodium sulfate 0.5 wt% and micro-silicon 1.5 wt% of 60 ~ 100 μm are fully mixed.
(4) get in (3) and mix sample a little, pour in beaker, by the water cement ratio modulation grout of 0.6, stir with glass stick, pour in mud scale and weigh density.
(5) under temperature 28 ° of C ± 1 ° C, with 0.6(W/C) water cement ratio pour corrugation agitator into, under even low speed, all mixed in 20 seconds, then build the lid of agitator, continue to stir 40 seconds under the speed of 4000r/min, leave standstill 5 minutes and observe grout homogeneity.
(6) poured into by the grout be stirred in the die trial of a group two pieces, the specification of die trial is long 53mm, wide 53mm height 53mm.
(7) maintenance 24 hours in the water-bath maintaining box of constant temperature 52 ° of C, soaks 1 hour after the demoulding in cold water, carries out ultimate compression strength and folding strength test and rate of change of the density experiment by the regulation of GB GB/T 177.
(8) maintenance 48 hours in the water-bath maintaining box of constant temperature 52 ° of C, soaks 1 hour after the demoulding in cold water, carries out ultimate compression strength and folding strength test and rate of change of the density experiment by the regulation of GB GB/T 177.
Embodiment 3.
(1) 1. the preparation of tantalum carbide closed pore cenosphere is prepared: particle diameter 20 ~ 30 μm of tantalum oxide are become powder mix than 1:1 in stirrer for mixing with phenolic resin weight, solidify at the temperature of 100 ° of C, and then make 100 μm of powder, by 100 μm of powder mixs at 3Mpa briquetting press upper holder block, on the electric furnace of 1800 ° of C, sintering obtains tantalum carbide block in 8 hours, and the tantalum carbide of bulk is made 30 μm of circular solids microballoons by balling machine.2. dosing: the weight percent of tantalum carbide liquid slurry consists of: particle diameter 30 μm of tantalum carbide 70 wt%, water 40 wt%, whipping agent sodium sulfate is added in tantalum carbide liquid slurry, concentration is 3g/L, 3. stirs: tantalum carbide solution good for proportioning is put into agitator and stirs; 4. filter: by macrobead and Impurity removal; 5. fire: adopt high pressure spraying high speed centrifugation rotary spraying technique, form microballoon, through dehydration expansion, sintering, melting, balling-up on four district's electric furnaces, obtain 110 ~ 150 μm of tantalum carbide closed pore cenospheres through classification.
(2) low density oil well cementing cement briquette batching: G level oil well cement 55 wt%, closed pore hollow tantalum carbide microballon 35 wt%, flyash 7 wt% of loss on ignition 1.1%, purity 99.9% calcium oxide 1.0 wt%, sodium sulfate 1.0 wt% and micro-silicon 1.0 wt% of 110 ~ 150 μm are fully mixed.
(3) mix: G level oil well cement 55 wt%, closed pore hollow tantalum carbide microballon 35 wt%, flyash 7 wt% of loss on ignition 1.1%, purity 99.9% calcium oxide 1.0 wt%, sodium sulfate 1.0 wt% and micro-silicon 1.0 wt% of 110 ~ 150 μm are fully mixed.
(4) get in (3) and mix sample a little, pour in beaker, by the water cement ratio modulation grout of 0.5, stir with glass stick, pour in mud scale and weigh density.
(5) under temperature 28 ° of C ± 1 ° C, with 0.5(W/C) water cement ratio pour corrugation agitator into, under even low speed, all mixed in 20 seconds, then build the lid of agitator, continue to stir 40 seconds under the speed of 4000r/min, leave standstill 5 minutes and observe grout homogeneity.
(6) poured into by the grout be stirred in the die trial of a group two pieces, the specification of die trial is long 53mm, wide 53mm height 53mm.
(7) maintenance 24 hours in the water-bath maintaining box of constant temperature 52 ° of C, soaks 1 hour after the demoulding in cold water, carries out ultimate compression strength and folding strength test and rate of change of the density experiment by the regulation of GB GB/T 177.
(8) maintenance 48 hours in the water-bath maintaining box of constant temperature 52 ° of C, soaks 1 hour after the demoulding in cold water, carries out ultimate compression strength and folding strength test by the regulation of GB GB/T 177.
Claims (3)
1. prepare the method for low density oil well cementing cement briquette with tantalum carbide closed pore cenosphere for one kind, comprise the preparation of tantalum carbide microballon, batching, mixing, stirring is sized mixing, die trial, strength trial, it is characterized in that: by G level oil well cement 55 ~ 65 wt%, particle diameter is closed pore hollow tantalum carbide microballon 25 ~ 35 wt% of 10 ~ 150 μm, flyash 5 ~ 7 wt% of loss on ignition 1.1%, purity 99.9% calcium oxide 1.5 ~ 2 wt%, sodium sulfate 0.5 ~ 1.0 wt% and micro-silicon 1 ~ 3 wt%, with 0.5 ~ 0.7(W/C) water cement ratio stir in stirrer and size mixing 40 seconds, pour die trial one group of two block length into, wide, high 53mm*53mm*53mm respectively, maintenance 24 hours in the water-bath maintaining box of constant temperature 52 ° of C, 48 hours, soak 1 hour in cold water after the demoulding, make a strength test,
Described a kind of tantalum carbide closed pore cenosphere prepares the method for low density oil well cementing cement briquette, particle diameter 1 ~ 30 μm of tantalum oxide is become powder mix than 1:0.8 ~ 1 in stirrer for mixing with phenolic resin weight, solidify at the temperature of 40 ~ 100 ° of C, and then make 50 ~ 100 μm of powder, by 50 ~ 100 μm of powder mixs at 1 ~ 3Mpa briquetting press upper holder block, on the electric furnace of 1300 ~ 1800 ° of C, sintering obtains tantalum carbide block in 5 ~ 8 hours, and the tantalum carbide of bulk is made 5 ~ 30 μm of circular solids microballoons by balling machine;
Described a kind of tantalum carbide closed pore cenosphere prepares the method for low density oil well cementing cement briquette, and the weight percent of tantalum carbide liquid slurry consists of: 5 ~ 30 μm of tantalum carbide 60 ~ 70 wt%, water 30 ~ 40 wt%;
Described a kind of tantalum carbide microballon prepares the preparation method of low density oil well cementing cement briquette, and in tantalum carbide liquid slurry, add whipping agent is one in calcium carbonate, potassium sulfate or sodium sulfate, and concentration is 1 ~ 3g/L;
Described a kind of tantalum carbide closed pore cenosphere prepares the method for low density oil well cementing cement briquette, tantalum carbide liquid is starched abundant agitation and filtration, adopt high pressure spraying high speed centrifugation rotary spraying technique, form microballoon, four district's electric furnaces obtain 10 ~ 150 μm of tantalum carbide closed pore cenospheres through dehydration expansion, sintering, melting, balling-up through classification.
2. a kind of tantalum carbide closed pore cenosphere according to claim 1 prepares the preparation method of low density oil well cementing cement briquette, it is characterized in that: the tantalum carbide closed pore cenosphere its floatability of preparation is greater than 90%.
3. a kind of tantalum carbide closed pore cenosphere according to claim 1 prepares the preparation method of low density oil well cementing cement briquette, it is characterized in that: the cement briquette 8 hours ultimate compression strength of preparation is greater than 10MPa, and within 24 hours, ultimate compression strength is greater than 20MPa.
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| CN103803883B (en) * | 2014-01-02 | 2015-05-06 | 山东理工大学 | Method for preparing oil well cementing cement briquette with silicon carbide/boron carbide hollow ceramic microbeads |
| CN103803888B (en) * | 2014-03-11 | 2015-07-29 | 山东理工大学 | A kind of silicon oxynitride Ceramic Composite microballon prepares the method for oil well cementing cement briquette |
| CN106187036B (en) * | 2016-07-05 | 2018-01-12 | 山东理工大学 | The method that heat-conducting type zeolite tantalum carbide ceramics microballon prepares the porous sponge brick that catchments |
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| CN102994059B (en) * | 2012-12-18 | 2014-10-15 | 中国石油化工股份有限公司 | low-density cement slurry |
| CN103224772B (en) * | 2013-04-08 | 2015-09-09 | 中国石油天然气股份有限公司 | A kind of cementing slurry, Preparation Method And The Use |
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