CN103342881B - Degradable temporary plugging ball and preparation method thereof - Google Patents
Degradable temporary plugging ball and preparation method thereof Download PDFInfo
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- CN103342881B CN103342881B CN201310318038.9A CN201310318038A CN103342881B CN 103342881 B CN103342881 B CN 103342881B CN 201310318038 A CN201310318038 A CN 201310318038A CN 103342881 B CN103342881 B CN 103342881B
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Abstract
The invention discloses a degradable temporary plugging wall and a preparation method thereof. The method comprises the following steps: esterifying and polymerizing water, terephthalic acid, ethylene glycol, 1,4-succinic acid, 1,3-propylene glycol and 1,4-hydroquinone; processing and grinding into balls in later phase to obtain a finished product. According to the degradable temporary plugging ball prepared by the preparation method provided by the invention, a blasthole can be plugged, working fluid is enforced to turn to other reforming layers, so that the degradable temporary plugging ball has the remarkable advantage of remarkable turning effect, and is easy to operate. After the construction is completed, the temperature of the stratum can be recovered, the temporary plugging wall is hydrolyzed into water-soluble acid and alcohol, and is drained with other fluids, so that the clean reformation of the stratum can be achieved, and longitudinal physical layering reformation can be realized, and the risk of ground flow plugging can be reduced. The degradable temporary plugging ball can be used in testing and completion stages.
Description
Technical field
The invention belongs to formation testing field of engineering technology, be specifically related to a kind of Degradable temporary and block up ball and preparation method thereof.
Background technology
Along with the development of formation testing engineering, under enter simple completion tubular column when, the more and more steering mode of demand simple and fast, realizes three-dimensional transformation.
At present, process complicated reservoirs, the transformation problem that longitudinally upper nonuniformity is strong, the method for employing has: the solid that instrument physical layering, fibrous physics turn to, baton round physics turns to and turn to the means such as sour chemistry diversion to carry out is longitudinally transformed.
The advantage of instrument physical layering is that layering is accurate, but exists and can only realize the problems such as the complicated and subsequent job of large section (being greater than 10m) layering, tool tubular column is difficult; The advantage that fibrous physics turns to can realize turning to transformation to the reservoir inhaling sour pressure difference value and be less than 8MPa, but there is multilayered reservoir that stress difference is greater than 8MPa and be difficult to realization and turn to the shortcoming such as complicated with pumping technology; Baton round physics turns to be had plugged perforation and turns to obvious advantage, but this baton round is not degraded, and in the later stage, discharge opeing easily blocks flow process; Turn to sour chemistry diversion can realize turning to transformation to the reservoir inhaling sour pressure difference value and be less than 5MPa, but the multilayered reservoir that stress difference is greater than 5MPa is difficult to realization turns to.
Summary of the invention
For solving the problem, the invention provides the preparation method that a kind of Degradable temporary blocks up ball, the Degradable temporary prepared by this method blocks up ball, has easy construction, the temporarily stifled feature that performance is good, degradation speed is fast, success ratio is high.
The present invention adopts following technical scheme:
Degradable temporary blocks up a preparation method for ball, it is characterized in that comprising following content:
(1) preparation of degradation material:
A. in water, add terephthalic acid and ethylene glycol, heated and stirred, to dissolving, adds 1, 4-succinic acid and 1,3-PD, through over-churning and polycondensation, obtains copolyesters A;
In water, add terephthalic acid and ethylene glycol, be stirred to dissolving, add 1, 4-benzenediol, through over-churning and polycondensation, obtain copolyesters B;
B. by the copolyesters A that obtains in above-mentioned steps and copolyesters B, through polycondensation, copolyesters C is obtained;
C. melt spinning method is adopted namely to obtain described degradation material copolyesters C obtained above;
(2) preparation of degradable ball:
A. above-mentioned obtained degradation material is heated to molten state;
B. add iron trichloride, stir after 30 minutes, add paraformaldehyde, stir;
C. the mixture stirred in step b is poured in mould, after cooling, namely obtain degradable ball through polishing.
Further, in step (1), each substance weight part is: terephthalic acid 50-100 part; Ethylene glycol 50-100 part; 1, 4-succinic acid 10-20 part; 1,3-PD 1-10 part; 1, 4-benzenediol 1-10 part; Water 20-50 part.
Further, in step (2), substance weight part of b step is: iron trichloride 0.1-0.5 part; Paraformaldehyde 0.05-0.5 part.
Further, substance weight part that the middle a step of step (1) prepares copolyesters A is: 14 parts, water, terephthalic acid 30 parts, ethylene glycol 40 parts, 1, 4-succinic acid 14 parts, 1,3-PD 2 parts; Each substance weight part of preparing copolyesters B in step (1) a step is: 27 parts, water, terephthalic acid 34 parts, ethylene glycol 36 parts, 1, 4-benzenediol 3 parts.
Further, in step (2), b substance weight part can also be: iron trichloride 0.4 part, paraformaldehyde 0.2 part.
Further, reaction conditions and the time of preparing copolyesters A in step (1) are: 250 DEG C, reaction 3 hours under 150MPa; Reaction conditions and the time of preparing copolyesters B in step (1) are: 255 DEG C, reaction 3 hours under 150MPa; Reaction conditions and the time of preparing copolyesters C in step (1) are: 282 DEG C, reaction 3 hours under 80MPa.
Further, in step (2), the Heating temperature of a step is 200 DEG C; B step in step (2), carries out the operation being heated to 100 DEG C, being forced into 5MPa before cooling.
Further, the diameter of the degradable ball prepared is 13mm or 15mm or 18mm.
The invention has the beneficial effects as follows:
(1), when general acid carries out esterification and polycondensation with alcohol, all adopt the ratio of 1:1, and carry out when needing catalyzer.And Degradable temporary provided by the invention blocks up the preparation method of ball, when preparing copolyesters A in step (1), esterification and polyreaction generation copolyesters C adopt sour total amount excessive, this is done to obtain the copolyesters A that the end of the chain is carboxyl, can be carried out when next time is polymerized; And excessive acid also helps reaction to carry out towards esterification direction.In the present invention, when preparing copolyesters A, do not use catalyzer, reaction conditions is 250 DEG C, the High Temperature High Pressure of 150MPa, this is because at this temperature and pressure, do not need additionally to add catalyzer, esterification and polyreaction just can be made to carry out simultaneously, if change other temperature and pressure into, this reaction is difficult to carry out and can not obtains the copolyesters product of required diprotic acid and dibasic alcohol, and Degradable temporary obtained after making is blocked up ball and can not be reached good physical strength and elasticity, can not resistance to compression preferably and effectively degraded.
(2), when general acid carries out esterification and polycondensation with alcohol, all adopt the ratio of 1:1, and carry out when needing catalyzer.And Degradable temporary provided by the invention blocks up the preparation method of ball, when preparing copolyesters B in step (1), adopt alcohol total amount excessive, this is done to obtain the copolyesters B that the end of the chain is hydroxyl, can esterification be carried out when being polymerized with copolyesters A and polyreaction generates copolyesters C; And alcohol is excessive to be also conducive to reaction and to carry out towards esterification direction.In the present invention, the copolyesters B provided is at 255 DEG C, be prepared under the High Temperature High Pressure of 150MPa, under this temperature and pressure, do not need additionally to add catalyzer just can make esterification and polyreaction carry out simultaneously, if change other temperature and pressure into, this reaction is difficult to carry out and can not obtains required copolyesters product.
(3) Degradable temporary provided by the invention is blocked up in the preparation method of ball, copolyesters C is polymerized by the copolyesters B of the end of the chain to be the copolyesters A of carboxyl and the end of the chain be hydroxyl, not as the reaction of general esterifying polycondensation, with the direct disposable generation copolyesters C of the raw material of copolyesters A and copolyesters B.With method preparation provided by the invention stifled ball temporarily, reaction process is easy to control, can not produce a large amount of by products, easily obtains a large amount of target product, and makes this temporary stifled ball have good physical strength and elasticity, can resistance to compression preferably and effectively degraded.
(4) block up ball by Degradable temporary prepared by method provided by the invention, it, by forcing working fluid to turn to the temporary blocking of borehole, achieves interlayer from physics aspect and turns to, and solves a transformation difficult problem for Heterogeneous reservoir from physics aspect; New type high temperature turns to acid to be that force liquid to enter low permeability layer and realize turning in layer, chemically aspect solves a transformation difficult problem for Heterogeneous reservoir along with the rising viscosity of pH value increases stifled most permeable zone temporarily.So Degradable temporary provided by the invention is blocked up ball and new type high temperature steering technique and is achieved interlayer and turn to and the double combination that turns in layer, solves a transformation difficult problem for Heterogeneous reservoir from physics and chemistry two aspects.
(5) block up ball by Degradable temporary prepared by method provided by the invention, its lowering speed is directly proportional to the velocity magnitude of fluid, the square root of stifled spherical diameter, is directly proportional to the square root of density difference.By regulating density or the diameter of stifled ball temporarily, can make to block up ball temporarily under fluid driven and dropping to designated depth, carrying out shutoff stratum.Therefore with this temporarily stifled ball block up temporarily in formation testing engineering, easy and simple to handle and can carry out accurately stifled temporarily to specified location.
(6) ball is blocked up by Degradable temporary prepared by method provided by the invention, for a kind of based on the product of ester fibrid, 13mm is stifled ball energy resistance to compression 70MPa under 130 DEG C of conditions temporarily, 15mm is stifled ball energy resistance to compression 80MPa under 150 DEG C of conditions temporarily, 18mm blocks up ball energy resistance to compression 100MPa under 180 DEG C of conditions temporarily, above-mentioned stifled ball temporarily equal energy voltage stabilizing 4 hours.In addition, stifled ball pressure is rear indeformable temporarily for this, has certain elasticity, has good physical strength.So stifled ball temporarily provided by the invention blocks up temporarily, this kind of technique just can realize multiple reservoir reconstruction, and the multilayered reservoir of energy counter stress difference 0 ~ 100MPa carries out three-dimensional acidifying or pressure break.
(7) ball is blocked up by Degradable temporary prepared by method provided by the invention, before turning layer, use ball injector to throw this stifled ball temporarily, have the advantages that directly do not drop into instrument, after construction terminates, formation temperature is restored, stifled ball is hydrolyzed into water miscible acid and alcohol temporarily, and discharges with other liquid, and reaches the clean transformation of formation; This blocks up ball temporarily can realize longitudinally upper physical layering transformation, reduces the risk that ground flow blocks simultaneously, all can use in test and completion phase; Block up temporarily with stifled ball temporarily provided by the invention, do not need increase equipment, fixed tubular column, also there will not be and shut stratum, string layer accident; This blocks up ball temporarily and tests at mill small stream 10 well, mill small stream 12 well, high stone 2 well, high stone 3 well, and being constructed into power is 100%.Therefore temporarily stifled ball provided by the invention has the feature of " easy construction, stifled performance is good temporarily, degradation speed is fast, success ratio is high ".
Accompanying drawing explanation
Fig. 1: stifled ball preparation process block diagram temporarily; Fig. 2: mill small stream 10 well acidizing construction curve figure; Wherein, 1 in Fig. 2 represents oil pressure curve, and 2 represent discharge curve of displacement, and 3 represent casing pressure curves.
Embodiment
Below in conjunction with embodiment, the present invention is further described, but therefore protection scope of the present invention be not limited among scope of embodiments.
embodiment 1
A kind of Degradable temporary is blocked up ball and is made up of (calculating by weight) following formula:
Terephthalic acid 65 parts; Ethylene glycol 75 parts; 1, 4-succinic acid 15 parts; 1,3-PD 1 part; 1, 4-benzenediol 3 parts; Iron trichloride 0.4 part; Paraformaldehyde 0.2 part, 41 parts, water.
Degradable temporary blocks up the preparation method of ball, comprises following content (producing by batch 200kg):
(1) preparation process of ball is blocked up temporarily as shown in Figure 1: the preparation of degradation material: 1. weight part is the terephthalic acid of 32 parts and the ethylene glycol of 38 parts, at 250 DEG C, carry out esterification, add the 1, 4-succinic acid that weight part is 15 parts, stir, obtain esterification products; Add in esterification products weight part be 1 part 1, ammediol carries out copolymerization, controlling final vacuum tightness is 150MPa, reacts 3 hours, obtains the copolyesters A that limiting viscosity is about 0.4.2. weight part is the terephthalic acid of 33 parts and the ethylene glycol of 37 parts, adds the 1, 4-benzenediol that weight part is 3 parts, 255 DEG C, reaction 3 hours under 150MPa, obtains the copolyesters B that limiting viscosity is about 0.3.3. mixed under the temperature condition of 282 DEG C by copolyesters A and B, controlling final vacuum tightness is 80MPa, reacts 3 hours, obtains the copolyesters C of limiting viscosity 0.65.Copolyesters C cuts into slices, and to doing, section is moisture is less than 25ppm to warm air drying at 155 ~ 158 DEG C.4. dry copolyesters C cuts into slices by respective screw extruder melting, sets up through volume pump, spinning, extrusion moulding from Spray silk hole, through stretching together and heat setting type, obtains degradation material.
(2) Degradable temporary blocks up the synthesis of ball: 1. the degradation material made is melt into pulpous state under 200 DEG C of high temperature; 2. in these slurries, add the flocculation agent iron(ic) chloride that weight part is 0.4, and stir 30 minutes; 3. after flocculation agent stirs, add weight part be 0.2 solidifying agent paraformaldehyde stir 30 minutes again; 4. the above-mentioned slurries stirred slowly are poured in the spherical die of specifying; 5. 100 DEG C are heated to spherical die, are forced into 5MPa; 6. carrying out after cooling 1h polishes again can obtain the smooth globe of shaping.
Obtained Degradable temporary is blocked up ball and carries out engineering simulation test, under its resistance to compression effect is shown in:
1. 130 DEG C, 13 mm block up ball temporarily in clear water, resistance to compression 70MPa 4 hours;
2. 150 DEG C, 15 mm block up ball temporarily in clear water, resistance to compression 80MPa 4 hours;
3. 180 DEG C, 18 mm block up ball temporarily in clear water, resistance to compression 100MPa4 hour;
Dissolution time: 13 mm to 18mm are stifled ball temporarily, under differing temps pressure condition, in different media, can meet 1 hour solvable by 5 hours, dissolution time is adjustable.
Find out thus, this Degradable temporary is indeformable after blocking up ball pressure, have certain elasticity, there is good physical strength, the multilayered reservoir of counter stress difference 0 ~ 100MPa can carry out three-dimensional acidifying or pressure break.
embodiment 2
A kind of Degradable temporary is blocked up ball and is made up of (calculating by weight) following formula:
Terephthalic acid 64 parts; Ethylene glycol 76 parts; 1, 4-succinic acid 14 parts; 1,3-PD 2 parts; 1, 4-benzenediol 3 parts; Iron trichloride 0.4 part; Paraformaldehyde 0.2 part, 41 parts, water.
Degradable temporary blocks up the preparation method of ball, comprises following content (producing by batch 200kg):
The preparation process of stifled ball is as shown in Figure 1 temporarily:
1. the preparation of degradation material:
A. in clean reactor, 14kg clear water is first added, after being warming up to 30 ~ 40 DEG C, add 30kg terephthalic acid in stirring, 40kg ethylene glycol, control to add at 30min, be stirred to after adding and dissolve completely, add the 1, 4-succinic acid of 14 kg, be warming up to 250 DEG C, stir constant temperature, then add 1 of 2kg, ammediol, control vacuum tightness 150MPa, react 3 hours, obtain 100kg copolyesters A;
B. in clean reactor, 27kg clear water is first added, after being warming up to 30 ~ 40 DEG C, drop into 34kg terephthalic acid in stirring, 36kg ethylene glycol, control to add at 30 ~ 50 min, be stirred to after adding and dissolve completely, add 3 kg1,4-dihydroxy-benzene, be warming up to 255 DEG C, stir constant temperature, control vacuum tightness 150MPa, react 3 hours, obtain 100kg copolyesters B;
C. in clean reactor, slowly add a, the 100kg copolyesters A that b generates and 100kg copolyesters B, adds in control 20min, is warming up to 282 DEG C, controls vacuum tightness 80MPa, reacts 3 hours, obtain copolyesters C.
2. Degradable temporary blocks up the preparation of ball:
A. degradation material 200kg is melt into pulpous state under 200 DEG C of high temperature;
B. add 0.4kg flocculation agent iron trichloride, stir 30 minutes to after dissolving completely, then add 0.2kg solidifying agent paraformaldehyde and stir 30 minutes to dissolving completely;
C. the slurries stirred in step b are poured in spherical die and be heated to 100 DEG C, be forced into 5MPa, after cooling, namely obtain degradable ball through polishing.
Above-mentioned obtained Degradable temporary is blocked up the practice of ball:
Domesticly use temporarily stifled ball provided by the invention to be that this well belongs to mill small stream-shop, Anping covered structure, well temperature 134 DEG C, belongs to porosity reservoir, construction layer position Temple of the Dragon King group at mill small stream 10 well first, this well uses new type high temperature to turn to acid 400 cubes and 13mm to block up 200, ball temporarily.Construct 83 minutes, its acidizing treatment curve as shown in Figure 2, from oil pressure curve 1, curve of displacement 2, can find out by casing pressure curve 3: oil pressure 87 to 92 MPa, discharge capacity 5.0 cubes/point, casing pressure 20 to 25 MPa.As can be seen from construction curve figure, stifled ball physics turns to obviously temporarily, serves the object of shutoff lower floor.Test output 1,300,000 cubes/day after this well pressure, comparatively front 1,200,000 cubes of/day volume increase 100,000 cubes/day of pressure.This shows that new type high temperature turns to acid and Degradable temporary to block up being combined of ball and demonstrates the considerable prospect of blocking up ball interlayer physical temporarily and turning in the successful use of this reservoir.High stone 2 well, mill small stream 12 well, high stone 3 well etc. are also constructed subsequently, are constructed into power 100%.
Claims (7)
1. Degradable temporary blocks up a preparation method for ball, it is characterized in that comprising following content:
(1) preparation of degradation material:
A. in water, add terephthalic acid and ethylene glycol, heated and stirred, to dissolving, adds 1, 4-succinic acid and 1,3-PD, through over-churning and polycondensation, obtains copolyesters A; The end of the chain of described copolyesters A is carboxyl;
In water, add terephthalic acid and ethylene glycol, be stirred to dissolving, add 1, 4-benzenediol, through over-churning and polycondensation, obtain copolyesters B; The end of the chain of described copolyesters B is hydroxyl;
B. by the copolyesters A that obtains in above-mentioned steps and copolyesters B, through polycondensation, copolyesters C is obtained;
C. melt spinning method is adopted namely to obtain described degradation material copolyesters C obtained above;
(2) preparation of degradable ball:
A. above-mentioned obtained degradation material is heated to molten state;
B. add iron trichloride, stir after 30 minutes, add paraformaldehyde, stir;
C. the mixture stirred in step b is poured in mould, after cooling, namely obtain degradable ball through polishing.
2. Degradable temporary according to claim 1 blocks up the preparation method of ball, it is characterized in that in step (1), each substance weight part is: terephthalic acid 50-100 part; Ethylene glycol 50-100 part; 1, 4-succinic acid 10-20 part; 1,3-PD 1-10 part; 1, 4-benzenediol 1-10 part; Water 20-50 part.
3. Degradable temporary according to claim 1 blocks up the preparation method of ball, it is characterized in that substance weight part of b step in step (2) is: iron trichloride 0.1-0.5 part; Paraformaldehyde 0.05-0.5 part.
4. Degradable temporary according to claim 1 blocks up the preparation method of ball, it is characterized in that: in step (2), substance weight part of b step is: iron trichloride 0.4 part, paraformaldehyde 0.2 part.
5. Degradable temporary according to claim 1 blocks up the preparation method of ball, it is characterized in that, reaction conditions and the time of preparing copolyesters A in step (1) are: 250 DEG C, reaction 3 hours under 150MPa; Reaction conditions and the time of preparing copolyesters B in step (1) are: 255 DEG C, reaction 3 hours under 150MPa; Reaction conditions and the time of preparing copolyesters C in step (1) are: 282 DEG C, reaction 3 hours under 80MPa.
6. Degradable temporary according to claim 1 blocks up the preparation method of ball, it is characterized in that, in step (2), the Heating temperature of a step is 200 DEG C; Step c in step (2), carries out the operation being heated to 100 DEG C, being forced into 5MPa before cooling.
7. Degradable temporary according to claim 1 blocks up the preparation method of ball, it is characterized in that: the diameter of the degradable ball prepared is 13mm or 15mm or 18mm.
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| CN105089599A (en) * | 2014-05-08 | 2015-11-25 | 中国石油化工股份有限公司 | Device and method for immovable string hydraulic sand blasting and fracturing |
| CN105154044A (en) * | 2015-07-31 | 2015-12-16 | 四川省贝特石油技术有限公司 | Automatic temporary blocking diverting agent and preparation method thereof |
| CN105482799B (en) * | 2015-11-30 | 2018-09-14 | 长江大学 | It is a kind of temporarily to block up diversion agent and preparation method thereof from degradation hydraulic fracturing |
| CN108612508B (en) * | 2018-04-24 | 2020-09-04 | 东方宝麟科技发展(北京)有限公司 | Novel shale gas horizontal well fracturing method utilizing high-strength degradable temporary plugging ball |
| CN108952623B (en) * | 2018-08-12 | 2020-09-11 | 张馨月 | Equal-density plugging ball delivery device and method |
| CN113201855B (en) * | 2021-05-13 | 2022-05-17 | 四川捷贝通能源科技有限公司 | Full-degradable high-strength temporary knot plug |
| CN115977601A (en) * | 2022-11-27 | 2023-04-18 | 西南石油大学 | Temporary plugging fracturing process method combining multi-density temporary plugging balls |
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| CN1962717A (en) * | 2006-11-14 | 2007-05-16 | 广州擎天实业有限公司 | Preparation method of polyester resin for mixing type powdery coating |
| CN102746837A (en) * | 2012-01-13 | 2012-10-24 | 宫立武 | Microsphere temporary plugging agent for leakage oil well |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1962717A (en) * | 2006-11-14 | 2007-05-16 | 广州擎天实业有限公司 | Preparation method of polyester resin for mixing type powdery coating |
| CN102746837A (en) * | 2012-01-13 | 2012-10-24 | 宫立武 | Microsphere temporary plugging agent for leakage oil well |
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