CN101696113B - Method for preparing low-density sintered ceramisite fracturing proppant with low cost - Google Patents
Method for preparing low-density sintered ceramisite fracturing proppant with low cost Download PDFInfo
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Abstract
The invention belongs to the technical field of petroleum fracturing proppants, and provides a method for preparing a low-density sintered ceramisite fracturing proppant with low cost. In the method, natural quartz is taken as a main raw material; one or more of bentonite, kaolin and clay are taken as a plasticizer, and a proper amount of one or more of magnesia, borax and boron oxide are taken as a sintering aid; and the low-density sintered ceramisite fracturing proppant is prepared through high-temperature sintering. The method is characterized by crushing the quartz, grinding the quartz into quartz powder with fine particles, adding the plasticizer, the sintering aid and an adhesive, then adding water into the mixture to roll into balls, and then sintering the balls at high temperature so as to obtain a silica fracturing proppant with low density, high sphericity and high flow conductivity. The cost for preparing the fracturing proppant by the method is far lower than that of a sintered bauxite fracturing proppant. The ceramisite proppant can be used as a solid proppant material for the fracture of oil and gas wells, thereby increasing the yield of the oil and gas wells.
Description
Technical field
The invention belongs to the petroleum fracturing propping agent technical field, propose a kind of low-cost preparation method of low-density sintered ceramisite fracturing proppant.
Background technology
In the recovery process of oil and gas; Because the Hyposmolality and the low flow conductivity of subterranean strata many times need make solid particulate inject subterranean strata by hydraulic fracturing technology, support formation fractures; Thereby improve the percent of pass of oil gas, these solid particulates are called fracturing propping agents.Early stage in hydraulic pressure technology, people adopt natural silica sand or nut-shell fragment as fracturing propping agents more.Along with the progress of hydraulic fracturing technology and material preparation technology, artificial fracturing propping agents such as sintered bauxite haydite and resin parcel haydite are used for the pressure break of oil gas well just increasingly extensively with its excellent performance.In the waterfrac treatment operation of oil gas well; Not only require propping agent to have suitable intensity; Simultaneously also require the density of propping agent low, degree of sphericity wants high; That low-density propping agent pumps into more easily is underground, reduce the propping agent consumption, and has higher porosity between the proppant particles of high degree of sphericity, helps improving flow conductivity.
The propping agent that Chinese patent CN02132988.5 has used when disclosing a kind of injection well pressure break, this propping agent is the mixtinite of nut-shell and silica sand, and the particle diameter of nut-shell is 1.0～3.0mm, and the volume ratio of nut-shell and silica sand is 0.8～1.2: 0.8～1.2.In use, this propping agent can not get into the inside of formation fracture fully, but rests on crack mouth or the downward a little space of crack mouth, makes the crack mouth can be too early closed because of lacking propping agent, thereby has improved the fracturing effect of injection well.
Chinese patent CN200410046711.9 discloses a kind of mesh propping agent; It is a main raw material with aluminum oxide, kaolin, clay, potassium felspar sand, talcum, as pore-forming material, adds water granulation balling-up with PS and rosin; Sintering at high temperature then, thus a kind of mesh propping agent obtained.This propping agent density is little, porosity is high, resistance to chemical corrosion good, as the catalyzer propping agent in the reactor drum time, can prolong the action time of catalyzer, enhances productivity.
Chinese patent CN200680049303.6 discloses a kind of composite proppant particle; It is made up of the glass of hollow and ceramic microsphere and resin glue; Adopt thermoplasticity or thermosetting resin to mix these potteries or glass microsphere, form the microballoon composite proppant of resin parcel.The composite proppant particle grain size is 5～1000 μ m, and density is 0.5～1.8g/cm
3, have crushing strength usually greater than 3.45MPa.In conjunction with hydraulic fracturing technology, the oil gas well yield can be improved in the crack of using this composite proppant to support in the oil gas well subsurface formations.
Chinese patent CN200710188410.3 discloses a kind of preparation technology of low-density propping agent; At first the plant fiber powder breakdown mill is become plant fiber particle; Then with modifier solution dipping, solidified plant fibre particle; Use the macromolecule resin enwrapped granule again, obtain low-density propping agent behind the last crushing screening.The sponge of selecting for use can be farm crop, also can be the fruit stone shell, and the volume density of gained propping agent is 0.65～1.1g/cm
3, volume density is 1.1～1.5g/cm
3
Natural silica sand and nut-shell propping agent are cheap, but their intensity is low, degree of sphericity is poor, therefore can only be used for the pressure break of shallow-layer well, and flow conductivity are not high.And, harsh as the silica sand selection of propping agent, can only select ground SiO such as Xinjiang, Gansu, Fujian for use
2The high-quality crude sedimentation sand that content is high, and a lot of geographic SiO
2The silica sand that content is low slightly is difficult to reach performance requriementss such as intensity, degree of sphericity.The sintered bauxite haydite has higher degree of sphericity, intensity and flow conductivity, and can be used for the pressure break of deep layer well, but production cost is higher.The price that is used to produce the natural bauxitic clay of bauxitic clay haydite is about 2～5 times of quartzite price, and sintering temperature also exceeds about 300 ℃ than the sintering temperature of quartz.And in the production process of sintering propping agent haydite, raw material and fuel cost account for 2/3rds of whole production cost.So, adopt quartzite to prepare the preparation cost that Z-prop fused ceramic will reduce propping agent greatly as raw material.The quartzy stone ore that extensively distributing in a lot of areas of Central and Western China, their application are demanded exploitation urgently, therefore, the present invention proposes a kind of method of utilizing natural quartzite to prepare low-density sintered ceramisite fracturing proppant as main raw material.
Summary of the invention
The objective of the invention is to develop a kind of low-cost preparation method of low-density sintered ceramisite propping agent, use this low-density sintered ceramisite fracturing proppant of the inventive method preparation can be used as the well fracturing Selid propping agent.
Core of the present invention is to select cheap quartzite as raw material; With the one or more combination thing in wilkinite, kaolin, the clay as plastic agent; One or more combination thing in adding magnesia, borax, the boron oxide is as sintering aid; And add one or more combination thing in Z 150PH, starch, the dextrin as sticker, and through batch mixing, moulding, drying, sintering, thus the petroleum fracturing propping agent of the low density of obtaining, high degree of sphericity, high flow conductivity.Operational path of the present invention and is implemented through following technological process shown in accompanying drawing 1:
(1) chooses the quartzy stone ore of dioxide-containing silica greater than 95wt%; After fragmentation, grinding, obtain having the quartz powder of 300 eye mesh screen percent of pass greater than 85% granularity; Choose one or more combination thing in wilkinite, kaolin, the clay as plastic agent; As sintering aid, and the granularity that guarantees these plastic agents and sintering aid is less than 200 orders, wherein with the one or more combination thing in magnesia, borax, the boron oxide; Content of magnesia in the magnesia is greater than 70wt%, and sticker is the one or more combination thing in Z 150PH, starch, the dextrin;
(2) with the quartzite powder: plastic agent: the weight ratio of sintering aid is 100 :≤20 :≤20 prepare burden, and add sticker, and add-on is 0.5～5% of a raw material powder weight, and powder is mixed in mixer;
(3) above-mentioned mixed powder is poured into carried out granulating and forming in the nodulizer, add entry in batches, make powder rotate balling-up, thereby obtain the propping agent haydite biscuit of spherical shape;
(4) propping agent haydite biscuit is dry in the environment of normal temperature to 300 ℃ under atmospheric environment or in the loft drier; Obtain dried haydite; Can be according to the needs of different propping agent particle diameters requirements; Dried haydite is carried out classification sieve,, dried haydite work in-process are carried out the control of size distribution so that remove excessive, the too small haydite of particle diameter;
(5) the propping agent biscuit after sieving in 1100～1450 ℃ of sintering, can select tunnel, rotary kiln or box kiln to carry out sintering in air, and in the sintering process, the temperature rate of propping agent should be less than 20 ℃/min; At last the propping agent behind the sintering is carried out classification, sieves, thereby obtain the propping agent product that different-grain diameter distributes.
According to China National Petroleum industry standard fracturing propping agents performance index and test recommend method SY/T5108-2006, use the fracturing propping agents performance of the present invention's preparation following, volume density is 0.7～1.4g/cm
3, volume density is 2.2～2.6g/cm
3, circularity and sphericity are about 0.9, and turbidity is less than 30FTU, and the percentage of damage of 20/40 order product under 28MPa pressure is less than 17%.And the minimum 2.2g/cm that reaches of volume density
3, far below the volume density (2.6～3.5g/cm of present sintered bauxite propping agent
3).Utilize the typical pattern of the propping agent that the present invention prepares as shown in Figure 2.
In sum, utilizing the present invention to prepare ceramic proppant has the following advantages:
(1) cheap, the easy acquisition of cost of material;
(2) the propping agent haydite of preparing is superior to the degree of sphericity and the intensity of silica sand, thereby in use has higher flow conductivity;
(3) compare with the sintered bauxite haydite, the production cost of present method is lower, and the density of ceramsite propping agent is also lower, is particularly useful for the pressure break exploitation of the high flow conductivity of Shallow Oil-Gas well.
Description of drawings
Preparation technology's flow process of Fig. 1 low-density silicon dioxide sintered ceramisite fracturing proppant.
The pattern of Fig. 2 low-density silicon dioxide sintered ceramisite fracturing proppant.
Embodiment
Through practical implementation the present invention is done explanation further below, but the present invention is confined to embodiment absolutely not.
Embodiment 1: get the 10Kg dioxide-containing silica and be 97.2% quartzy stone ore, behind the broken and jaw crushing, put into the ball mill ball milling through pair roller; Obtain 300 eye mesh screen percent of pass and be 95% quartz powder, then with 1Kg wilkinite, 1Kg magnesia (content of magnesia 82%), 0.1Kg starch adds in the silica powder; In mixer, mix, put into disk balling machine to the raw material powder that mixes, add water 1.5Kg; The granulation balling-up, the propping agent biscuit that obtains is placed into seasoning under the normal temperature in the air, sieves then and removes particle bigger than normal or less than normal; Obtain work in-process, work in-process are put into box-type furnace be warming up to 1300 ℃, be incubated 2 hours with the speed of 10 ℃/min; Speed with 15 ℃/min is cooled to normal temperature then, and the propping agent classification behind the sintering is sieved, and obtains 20/40 order ceramic fracturing propping agent product; According to the SY/T5108-2006 standard testing, performance is following, and volume density is 1.3g/cm
3, volume density is 2.5g/cm
3, circularity and sphericity are about 0.9, turbidity 20FTU, and the percentage of damage of product under 28MPa pressure is 12%.
Embodiment 2: get the 10Kg dioxide-containing silica and be 95.6% quartzy stone ore,, put into Raymond mill and grind behind the broken and jaw crushing through pair roller; Obtaining 300 eye mesh screen percent of pass is the quartz powder of 96wt%, then 0.8Kg kaolin, 1.2Kg borax, 0.08Kg Z 150PH is added in the silica powder, in mixer, mixes; Change the raw material powder that mixes in the high speed nodulizer over to, add water 1.3Kg, the granulation balling-up; The propping agent biscuit that obtains is placed in 100 ℃ the loft drier dry, sieves then and removes particle bigger than normal or less than normal, obtains work in-process; Work in-process are put into rotary kiln burn till in 1200 ℃, the propping agent classification after burning till is sieved, obtain 20/40 order ceramic fracturing propping agent product; According to the SY/T5108-2006 standard testing, performance is following, and volume density is 1.5g/cm
3, volume density is 2.4g/cm
3, circularity and sphericity are about 0.9, turbidity 12FTU, and the percentage of damage of product under 28MPa pressure is 11.2%.
Embodiment 3: get the 10Kg dioxide-containing silica and be 98.1% quartzy stone ore,, put into airflow milling and grind behind the broken and jaw crushing through pair roller; Obtain 300 eye mesh screen percent of pass and be 100% quartz powder, then 1.0Kg clay, 0.8Kg magnesia (content of magnesia 75%), 0.7Kg borax, 0.1Kg dextrin are added in the silica powder, in mixer, mix; Change the raw material powder that mixes in the high speed nodulizer over to, add water 1.8Kg, the granulation balling-up; The propping agent biscuit that obtains is placed in 150 ℃ the loft drier dry, sieves then and removes particle bigger than normal or less than normal, obtains work in-process; Work in-process are put into tunnel burn till in 1400 ℃, the propping agent classification after burning till is sieved, obtain 20/40 order ceramic fracturing propping agent product; According to the SY/T5108-2006 standard testing, performance is following, and volume density is 0.8g/cm
3, volume density is 2.3g/cm
3, circularity and sphericity are about 0.9, turbidity 8FTU, and the percentage of damage of product under 28MPa pressure is 6%.
Embodiment 4: get the 10Kg dioxide-containing silica and be 98.0% quartzy stone ore, after the pair roller fragmentation, put into vibration mill and grind; Obtain 300 eye mesh screen percent of pass and be 99% quartz powder, then 1.0Kg wilkinite, 1.0Kg kaolin, 0.8Kg boron oxide, 0.1Kg starch, 0.1Kg dextrin are added in the silica powder, in mixer, mix; Change the raw material powder that mixes in the high speed nodulizer over to, add water 1.6Kg, the granulation balling-up; The propping agent biscuit that obtains is placed in 200 ℃ the loft drier dry, sieves then and removes particle bigger than normal or less than normal, obtains work in-process; Work in-process are put into tunnel burn till in 1280 ℃, the propping agent classification after burning till is sieved, obtain 16/30 order ceramic fracturing propping agent product; According to the SY/T5108-2006 standard testing, performance is following, and volume density is 0.8g/cm
3, volume density is 2.4g/cm
3, circularity and sphericity are about 0.9, turbidity 20FTU, and the percentage of damage of product under 28MPa pressure is 5.5%.
Embodiment 5: get the 10Kg dioxide-containing silica and be 98.4% quartzy stone ore, after the pair roller fragmentation, put into vibration mill and grind; Obtain 300 eye mesh screen percent of pass and be 90% quartz powder, then 1.0Kg kaolin, 0.5Kg clay, 0.8Kg magnesia (content of magnesia 88%), 0.1Kg starch are added in the silica powder, in mixer, mix; Change the raw material powder that mixes in the high speed nodulizer over to, add water 1.3Kg, the granulation balling-up; The propping agent biscuit that obtains is placed in 130 ℃ the loft drier dry, sieves then and removes particle bigger than normal or less than normal, obtains work in-process; Work in-process are put into tunnel burn till in 1350 ℃, the propping agent classification after burning till is sieved, obtain 30/50 order ceramic fracturing propping agent product; According to the SY/T5108-2006 standard testing, performance is following, and volume density is 1.3g/cm
3, volume density is 2.3g/cm
3, circularity and sphericity are about 0.95, turbidity 24FTU, and the percentage of damage of product under 28MPa pressure is 17%.
Embodiment 6: get the 10Kg dioxide-containing silica and be 97.0% quartzy stone ore, after the pair roller fragmentation, put into vibration mill and grind; Obtain 300 eye mesh screen percent of pass and be 86% quartz powder, then 1.0Kg wilkinite, 0.5Kg magnesia (content of magnesia 88%), 0.3Kg boron oxide, 0.1Kg starch, 0.05Kg Z 150PH are added in the silica powder, in mixer, mix; Change the raw material powder that mixes in the high speed nodulizer over to, add water 1.6Kg, the granulation balling-up; The propping agent biscuit that obtains is placed in 170 ℃ the loft drier dry, sieves then and removes particle bigger than normal or less than normal, obtains work in-process; Work in-process are put into tunnel to be burnt till in 1330 ℃; Propping agent classification after burning till is sieved, obtain 40/70 order ceramic fracturing propping agent product, according to the SY/T5108-2006 standard testing; Performance is following, and volume density is 1.4g/cm
3, volume density is 2.5g/cm
3, circularity and sphericity are about 0.9, turbidity 26FTU, and the percentage of damage of product under 28MPa pressure is 4%.
Embodiment 7: get the 10Kg dioxide-containing silica and be 98.9% quartzy stone ore, after the pair roller fragmentation, put into vibration mill and grind; Obtain 300 eye mesh screen percent of pass and be 89% quartz powder, then 1.0Kg wilkinite, 0.5Kg kaolin, 0.5Kg clay, 0.3Kg magnesia (content of magnesia 95%), 0.2Kg borax, 0.1Kg boron oxide, 0.1Kg starch, 0.05Kg dextrin, 0.05Kg Z 150PH are added in the silica powder, in mixer, mix; Change the raw material powder that mixes in the high speed nodulizer over to, add water 1.7Kg, the granulation balling-up; The propping agent biscuit that obtains is placed in 80 ℃ the loft drier dry, sieves then and removes particle bigger than normal or less than normal, obtains work in-process; Work in-process are put into tunnel to be burnt till in 1290 ℃; Propping agent classification after burning till is sieved, obtain 8/16 order ceramic fracturing propping agent product, according to the SY/T5108-2006 standard testing; Performance is following, and volume density is 0.7g/cm
3, volume density is 2.2g/cm
3, circularity and sphericity are about 0.85, turbidity 6FTU, and the percentage of damage of product under 28MPa pressure is 16%.
Claims (6)
1. the low-cost preparation method of a low-density sintered ceramisite fracturing proppant comprises material choice, proportioning raw materials, moulding, drying and sintering, it is characterized in that:
(1) be main raw material with the natural stone diamond stone; With the one or more combination thing in wilkinite, the kaolin as plastic agent; With the one or more combination thing in magnesia, borax, the boron oxide is sintering aid; And adding one or more combination thing in Z 150PH, starch, the dextrin as sticker, raw material powder is with the quartzite powder: plastic agent: the weight ratio of sintering aid is 100 :≤20 :≤20 prepare burden, and the add-on of sticker is 0.5～5% of a raw material powder weight;
(2) in the raw material powder that is mixed with sticker, add suitable quantity of water, granulation balling-up in rolling balling machine or high speed nodulizer, the propping agent biscuit of formation spherical shape;
(3) dry propping agent biscuit, then in air in 1100～1450 ℃ of sintering, thereby obtain low-density ceramic fracturing propping agent.
2. press the low-cost preparation method of the described a kind of low-density sintered ceramisite fracturing proppant of claim 1; It is characterized in that: the quartzite of employing has the above dioxide-containing silica of 95wt%, and quartzite powder broken, after grinding has 300 eye mesh screen percent of pass greater than 85% granularity.
3. by the low-cost preparation method of the described a kind of low-density sintered ceramisite fracturing proppant of claim 1, it is characterized in that: the content of magnesia in the used magnesia is greater than 70wt%, and the granularity of magnesia is less than 200 orders.
4. by the low-cost preparation method of the described a kind of low-density sintered ceramisite fracturing proppant of claim 1, it is characterized in that: used borax and boron oxide have less than 200 purpose granularities.
5. by the low-cost preparation method of the described a kind of low-density sintered ceramisite fracturing proppant of claim 1, it is characterized in that: the propping agent biscuit of spherical shape is at the TR inner drying of normal temperature to 300 ℃.
6. by the low-cost preparation method of the described a kind of low-density sintered ceramisite fracturing proppant of claim 1, it is characterized in that: dried propping agent biscuit sintering in tunnel, rotary kiln or box furnace, and keep temperature rate less than 20 ℃/min.
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