CN113981564A - Sand-carrying fiber and preparation and application thereof - Google Patents
Sand-carrying fiber and preparation and application thereof Download PDFInfo
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- CN113981564A CN113981564A CN202111345473.1A CN202111345473A CN113981564A CN 113981564 A CN113981564 A CN 113981564A CN 202111345473 A CN202111345473 A CN 202111345473A CN 113981564 A CN113981564 A CN 113981564A
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Abstract
The invention discloses a sand-carrying fiber and preparation and application thereof. The sand-carrying fiber is polylactic acid fiber, which comprises the following raw materials in parts by weight: 100 parts of polylactic acid (PLA), 12-16 parts of poly-p-phenylene terephthalamide, 3-5 parts of sodium dodecyl benzene sulfonate, 2-5 parts of citric acid, 15-23 parts of polyvinyl alcohol, 10-22 parts of glyceryl monostearate, 15-25 parts of polyethylene glycol, 10 parts of magnesium phosphate-fibrin glue and 2-3 parts of zinc chloride. The sand-carrying fiber has the characteristics of simple process route, good sand-carrying performance, strong flow conductivity, excellent dispersibility and the like, and can effectively reduce the loss of fracturing fluid. And the magnesium phosphate-fibrin glue and zinc chloride are added into the fiber polymer, so that the prepared sand-carrying fiber has better toughness and solubility.
Description
Technical Field
The invention relates to the field of composite nano materials and oil exploitation technology research, in particular to a sand-carrying fiber with dissolubility in a hydraulic fracturing process, and preparation and application thereof.
Background
With the shortage of conventional oil and gas resources, the exploration and development field of oil and gas industry is gradually extended to the unconventional oil and gas shift, and the attention on the unconventional oil and gas related exploration and research technology is increased. The unconventional oil gas has huge reserves, abundant dense oil gas resources, and safe and efficient exploitation of the unconventional oil gas is in the light of energy transformation and energy safety bureaus. Hydraulic fracturing has been fully focused and vigorously developed to achieve the main goals of yield increase and efficiency increase in the development of compact hydrocarbon reservoirs. The injection of the fracturing fluid is one of the core links of the fracturing technology, is an important technical measure for increasing the injection of reservoir layers of oil and gas wells and water injection wells, and can effectively improve the production rate of oil fields and improve the water injection conditions. Therefore, how to prepare the fracturing fluid with excellent performance is important for the exploitation of oil and gas reservoirs.
One effective method is to add a fibrous material to the fracturing fluid, mix it with the fracturing fluid and proppant, and pump the fracturing fluid and proppant together into the formation using a high pressure pump. As a component of the fracturing fluid, the fiber with good dispersibility can realize automatic dispersion in the fracturing fluid and form a net structure, so that the fracturing fluid with lower viscosity is endowed with more excellent sand carrying performance. Through aggregation with the proppant, the material is an excellent material for improving the suspension property of the proppant, and plays roles in stabilizing proppant clusters and reducing the settling velocity of the proppant. When the closing pressure is higher, the crack formed by the fracturing is easy to close, and the fiber-fracturing fluid system can enable the propping agents such as quartz sand and the like to maintain a suspension state for a longer time in the fracturing process, so that the propping effect when the crack is closed is improved. Therefore, a smooth flow guide channel can be formed in the crack, and the flow guide capacity is higher than that of the fracturing fluid used alone by several grades.
At present, in order to meet the requirements of oil and gas reservoir exploitation, yield increase and efficiency increase, researches on sand-carrying fibers mainly focus on the flow conductivity and the dispersion performance of the sand-carrying fibers, and few researches on the delayed solubility, the easy sand-carrying flowback performance and the like of the sand-carrying fibers are carried out.
Disclosure of Invention
The invention aims to provide a sand-carrying fiber and preparation and application thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a sand-carrying fiber which comprises the following components in parts by weight:
polylactic acid (PLA)100 parts
12-16 parts of poly (p-phenylene terephthalamide);
3-5 parts of sodium dodecyl benzene sulfonate;
2-5 parts of citric acid;
15-23 parts of polyvinyl alcohol, preferably 15-17 parts;
10-22 parts of glyceryl monostearate, preferably 10-15 parts;
15-25 parts of polyethylene glycol, preferably 15-18 parts;
8-10 parts of magnesium phosphate-fibrin glue;
2-3 parts of zinc chloride.
According to the invention, the magnesium phosphate-fibrin glue and zinc chloride are added into the fiber polymer for the first time, so that the prepared sand-carrying fiber has better toughness and solubility.
According to the sand-carrying fiber of the invention, preferably, the relative molecular weight of the polylactic acid is 100000-140000, the relative molecular weight of the polyvinyl alcohol is 25000-35000, and the relative molecular weight of the poly-p-phenylene terephthalamide is 50000-70000.
According to the sand-carrying fiber, the polyvinyl alcohol is preferably 15-17 parts.
According to the sand-carrying fiber, the glyceryl monostearate is preferably 10-15 parts.
According to the sand-carrying fiber, the polyethylene glycol is preferably 15-18 parts.
According to the sand-carrying fiber, the magnesium phosphate-fibrin glue is preferably a uniform mixed product of magnesium phosphate and fibrin glue, and more preferably, the mass ratio of the magnesium phosphate to the fibrin glue is 1: 5.
According to the sand-carrying fiber provided by the invention, the length of the sand-carrying fiber is preferably 5 mm-7 mm.
According to the sand-carrying fiber provided by the invention, the diameter of the sand-carrying fiber is preferably 30-37 μm for achieving a better sand-carrying effect.
According to the sand-carrying fiber provided by the invention, preferably, the surface of the sand-carrying fiber is covered with a film. More preferably, the film has a film material composition comprising: gelatin, a plasticizer (preferably glycerol) and water, more preferably, the mass ratio of the gelatin to the plasticizer to the water is 1:0.5: 1.5. The film is uniformly sprayed on the sand-carrying fiber through a sprayer of a plastic spraying machine, and a layer of soft and elastic film is formed on the surface of the fiber.
The surface of the sand-carrying fiber is uniformly covered with a layer of film, so that the coated sand-carrying fiber can be pumped to a deeper ground seam in the fracturing process, and a better sand-carrying effect is achieved.
The invention also provides a preparation method of the sand-carrying fiber, which comprises the following steps:
melting the mixture of the components, extruding out melt trickle through electrostatic spinning, and immersing the melt after spinning into a coagulating bath for cooling to obtain nascent fiber;
stretching the nascent fiber;
heat setting at 200-220 deg.C, cooling and spraying at normal temperature, steam ironing at 80-100 deg.C, curling, winding, and cutting to obtain the sand-carrying fiber.
According to the preparation method of the invention, preferably, the components are mixed and stirred for 30 min-50 min at 1500r/min to prepare a uniform mixture.
According to the production method of the present invention, preferably, the melting is screw extrusion melting at 200 ℃.
According to the production method of the present invention, preferably, the coagulation bath component is a mixed solution of water and N, N-dimethylacetamide (DMAc).
According to the production method of the present invention, preferably, the temperature of the coagulation bath is 5 ℃ to 10 ℃; the cooling time of the immersion in the coagulation bath is 10 s-15 s.
According to the production method of the present invention, preferably, the stretching includes: guide roller drawing at normal temperature, wet heat drawing in a drawing tank at a temperature of 75 ℃ to 85 ℃, and dry heat drawing in steam at a temperature of 85 ℃ to 100 ℃. The mechanical property and the dimensional stability of the fiber are improved through guide roller drafting, damp heat drafting and dry heat drafting.
According to the preparation method of the invention, the sand-carrying fiber is preferably cut by a fiber cutting machine, so that the length of the obtained sand-carrying fiber is 5 mm-7 mm.
According to the preparation method of the invention, preferably, in order to achieve better sand carrying effect, spray heads with different sizes are used in the electrostatic spinning process, so that the diameter of the obtained sand carrying fiber is 30-37 μm.
According to the preparation method, in order to cover the surface of the sand-carrying fiber with a film, gelatin, a plasticizer (preferably glycerol) and water are mixed according to the mass ratio of 1:0.5:1.5 to prepare a solution, and the solution is uniformly sprayed on the sand-carrying fiber through a spray head of a plastic spraying machine, so that a soft and elastic film can be formed on the surface of the fiber.
The sand-carrying fiber prepared by the method has the delayed dissolving capacity different from that of other sand-carrying fibers. Therefore, the sand-carrying fiber prepared by the method can be pumped to a deeper position of an underground seam along with the fracturing fluid in the stratum, maintains longer sand-carrying capacity, and can effectively prevent the backflow of the propping agent in the later flowback process.
In another aspect, the invention provides an application of the sand-carrying fiber in fracturing reformation of an oil well reservoir.
In the fracturing modification of an oil well reservoir, the preferable usage amount of the sand-carrying fiber is 0.1-1% of the mass of the fracturing fluid.
In order to improve the performance of the fiber, the invention forms the superfine fiber by adding polyester polymer (polylactic acid (PLA)). The density of the monofilament line of the superfine fiber is lower than that of the common fiber, so the superfine fiber is softer and finer than the common sand-carrying fiber. The low viscosity polyester polymer melt is sprayed into staple fibers by a jet of air using an electrospinning process.
In addition, the magnesium phosphate-fibrin glue and zinc chloride are added into the fiber polymer for the first time, so that the prepared sand-carrying fiber has better toughness and solubility.
Compared with the single proppant fracturing fluid, the dissolvable sand-carrying fiber for fracturing still has excellent flow conductivity under higher pressure; in addition, the oil-gas composite material can be dissolved to a great extent at the temperature of 90 ℃, so that the aims of environmental protection and oil-gas yield improvement are fulfilled.
The sand-carrying fiber has the characteristics of simple process route, good sand-carrying performance, strong flow conductivity, excellent dispersibility and the like, and can effectively reduce the loss of fracturing fluid. And the magnesium phosphate-fibrin glue and zinc chloride are added into the fiber polymer, so that the prepared sand-carrying fiber has better toughness and solubility. Because the sand-carrying fiber has dissolubility, excessive fiber residues cannot be generated after the sand-carrying fiber is pumped into the underground along with fracturing fluid, and the risk of crack blockage is low, so that the aims of cleanness, high efficiency and energy consumption reduction can be fulfilled. Along with the great improvement of the flow conductivity, the fracturing fluid can be conveyed faster and farther, so that economic benefits are generated, and the aims of quality improvement, cost reduction and efficiency improvement are fulfilled; the method has wide market prospect for developing unconventional oil and gas reservoirs.
Drawings
Fig. 1A is a SEM test result chart of the sand-carrying fiber prepared in example 1 of the present invention.
FIG. 1B is a SEM test result of a cross section of a sand-carrying fiber prepared in example 1 of the present invention.
Fig. 2 is a flow conductivity test result diagram of the sand-carrying fiber prepared in example 1 of the present invention.
FIG. 3 is a graph of the results of testing the relative sand-suspending performance of proppant on sand-carrying fibers of different mass prepared in example 1 of the present invention.
FIG. 4 is a graph of the test results of the stability of sand-carrying fibers prepared in example 1 to the relative sand-suspending performance of 20g proppant.
FIG. 5 is a graph showing the results of the solubility test of the sand-carrying fiber prepared in example 1 of the present invention at a temperature of 90 ℃.
FIG. 6 is a SEM test result chart of a cross section of a single sand-carrying fiber prepared in example 7 of the present invention.
Detailed Description
In order to more clearly illustrate the invention, the invention is further described below in connection with preferred embodiments. It is to be understood by persons skilled in the art that the following detailed description is illustrative and not restrictive, and is not to be taken as limiting the scope of the invention.
All numerical designations of the invention (e.g., temperature, time, concentration, weight, and the like, including ranges for each) may generally be approximations that vary (+) or (-) in increments of 0.1 or 1.0 as appropriate. All numerical designations should be understood as preceded by the term "about".
Example 1
The embodiment of the invention prepares a sand-carrying fiber, which comprises the following steps:
stirring 100 parts of polylactic acid, 15 parts of poly-p-phenylene terephthalamide, 3 parts of sodium dodecyl benzene sulfonate, 3 parts of citric acid, 16 parts of polyvinyl alcohol, 11 parts of glyceryl monostearate, 16 parts of polyethylene glycol, 8 parts of magnesium phosphate-fibrin glue and 2 parts of zinc chloride for 30min at 1500r/min to prepare a uniformly mixed solution.
Wherein, the relative molecular weight of the polylactic acid is 110000, the relative molecular weight of the polyvinyl alcohol is 27000, and the relative molecular weight of the poly-p-phenylene terephthalamide is 55000.
Extruding and melting the prepared polylactic acid mixture at 200 ℃ by a screw, extruding the molten mixture into melt trickle by electrostatic spinning equipment, extruding the molten mixture into melt trickle by the electrostatic spinning equipment, immersing the melt after spinning into a mixed solution coagulating bath of water and N, N-dimethylacetamide (DMAc) at 10 ℃ for cooling for 15s to obtain nascent fiber; and (3) stretching the nascent fiber, and improving the mechanical property and the dimensional stability of the fiber through guide roller drafting, damp-heat drafting and dry-heat drafting. Heat setting at 200 deg.C, cooling and spraying at normal temperature, steam ironing at 100 deg.C, curling, winding, cutting, and packaging.
According to the preparation method of the embodiment, the length of the sand-carrying fiber is 5 mm-7 mm, and the diameter is 30 μm-32 μm. FIG. 1A shows the SEM test results of sand-carrying fiber prepared in example 1 of the present invention, and the length of the sand-carrying fiber prepared in this example is measured to be 5 mm-7 mm from FIG. 1A. FIG. 1B shows SEM test results of cross-section of sand-carrying fiber prepared in example 1 of the present invention, and the cross-section diameter of the sand-carrying fiber prepared in this example is measured to be 30 μm-32 μm from FIG. 1B.
Example 2
In this embodiment, the sand-carrying fiber prepared in example 1 is tested to simulate the influence of the sand-carrying fiber on the conductivity of the proppant in the fracturing process of the oil well reservoir, so as to understand the relationship between the conductivity of the fracture supported by the sand-carrying fiber in the formation and the change of the closure pressure.
The samples are divided into an experimental group and a control group, and in the experimental group, sand-carrying fibers and 5g of propping agents (ceramic particles) are flatly laid on the surface of the rock covered with the copper wire mesh in a single layer manner, so that the propping agents and the sand-carrying fibers are uniformly and tightly dispersed. The control group only tiled 5g of proppant in a single layer on the surface of the copper mesh coated rock. And opening the flow guide instrument, and applying different pressure loads to obtain flow guide capacity values of the experimental group and the control group under different pressures.
Fig. 2 is a result of a conductivity test of the sand-carrying fiber prepared in example 1 of the present invention, and it can be seen from fig. 2 that the conductivity of the proppant is improved after the sand-carrying fiber is added under a higher pressure. The diversion effect is best when the pressure is 30 MPa.
Example 3
In this example, the sand-carrying fiber prepared in example 1 was tested to examine the effect of the sand-carrying fiber on proppant suspension capacity during fracturing of an oil well reservoir.
Weighing 1500mL of deionized water, placing in a beaker, slowly adding 4.5g of guar gum, stirring at room temperature for 4h for later use, and adjusting the stirring speed to 1500 r/min. The prepared base liquid is divided into ten parts and 100mL of each part in a beaker. 50mg, 100mg, 150mg, 200mg, 225mg, 250mg, 300mg, 350mg, 400mg and 500mg of the soluble sand-carrying fiber prepared in the above example 1 were added, respectively, and one portion was prepared as a blank. Then 1g of propping agent (ceramsite) is added respectively, and the relative sand suspension performance after 1h is observed.
FIG. 3 is a test result of the relative sand-suspending performance of proppant on sand-carrying fibers of different mass prepared in example 1 of the invention, and FIG. 3 shows that the relative sand-suspending performance F/F of proppant in fracturing fluid containing sand-carrying fibers of different mass is within 1h0Comparing, wherein F is the mass of the settling propping agent in the fracturing fluid containing the sand-carrying fiber, and F0The mass of the proppant is not contained in the sand-carrying fiber fracturing fluid. The suspension performance of the proppant is improved more favorably with the increase of the addition of the sand-carrying fibers, and the relative sand suspension performance of the sand-carrying fibers is basically the same after the addition of the fibers reaches 300 mg.
Example 4
In this example, the sand-carrying fiber prepared in example 1 was tested to examine the suspending ability of the sand-carrying fiber to a large amount of proppant during fracturing of an oil well reservoir.
Weighing 500mL of deionized water, placing the deionized water in a beaker, slowly adding 1.5g of guar gum, stirring for 4 hours at room temperature for standby, and adjusting the stirring speed to 1500 rpm. Taking 100mL of prepared base fluid into a beaker respectively, carrying out 5 groups of parallel tests, adding 0.5g of the sand-carrying fiber prepared in the embodiment 1 of the invention into each part, then adding 20g of the propping agent (ceramsite) into each part, and observing the relative sand suspension after 1h, thereby proving that the sand-carrying fiber prepared in the embodiment 1 of the invention still has relatively good relative sand suspension performance stability when a large amount of propping agent is added.
FIG. 4 shows the test results of the stability of the sand-carrying fiber prepared in example 1 of the present invention to the relative sand-suspending performance of 20g proppant; FIG. 4 shows the relative sand-suspending performance F/F of proppant in fracturing fluid without sand-carrying fiber and with sand-carrying fiber in 1h0Comparing, wherein F is the mass of the settling propping agent in the fracturing fluid containing the sand-carrying fiber, and F0The mass of the proppant is not contained in the sand-carrying fiber fracturing fluid. The results show that the sand-carrying fiber is addedAnd then, the suspension property of the propping agent is obviously improved, and the requirement of fracturing field fibers on relative sand suspension performance can be met.
Example 5
In this example, the sand-carrying fiber prepared in example 1 was tested to test the dissolution performance of the sand-carrying fiber for dissolvable fracturing during fracturing in an oil reservoir at 90 ℃.
0.5g of the sand-carrying fiber prepared in example 1 of the present invention was weighed into a centrifuge tube containing 50mL of deionized water, and the tube was placed in a 90 ℃ thermostat water bath for 4 hours using deionized water as a solvent. Then taking out and transferring all the supernatant liquid into a dried centrifugal tube, putting the centrifugal tube into a centrifugal machine, centrifuging for 30min at the rotating speed of 1500r/min, and slowly pouring out the supernatant liquid; pouring the residual fiber into a dry centrifuge tube, centrifuging in a centrifuge for 30min, pouring the supernatant, putting the centrifuge tube into a constant temperature electric heating drying oven, drying at 55 deg.C, and weighing.
The solubility η can be calculated using the following equation (1):
wherein eta is percent solubility, m1The total mass of the centrifuge tube and the fiber after drying is gram (g), m0In total, three replicates were made, in grams (g), for the mass of the centrifuge tube used.
FIG. 5 shows the results of the solubility test of the sand-carrying fiber prepared in example 1 of the present invention at 90 ℃. FIG. 5 shows the values of the dissolution rates of sand-carrying fibers after heating at 90 ℃ for 4 h. The result shows that the sand-carrying fiber prepared in the embodiment 1 of the invention has excellent dissolving performance, can be dissolved in the stratum, reduces sand plugging loss and improves economic benefit.
Example 6
In this embodiment, a coated sand-carrying fiber is prepared on the basis of the sand-carrying fiber prepared in embodiment 1, and includes the following steps:
gelatin, plasticizer (glycerin) and water were mixed in a mass ratio of 1:0.5: 1.5. The prepared solution is uniformly sprayed on the sand-carrying fiber prepared in the example 1 through a spray head of a plastic spraying machine, and a layer of soft and elastic film is formed on the surface of the fiber.
The coated sand-carrying fiber prepared in the embodiment 6 can be pumped into a deeper gap along with the fracturing fluid, and the film on the surface can be dissolved in the fracturing fluid, so that the exploration and development of oil and gas reservoirs are facilitated, and the utilization rate of the fracturing fluid is improved.
Example 7
The embodiment of the invention prepares a sand-carrying fiber, which comprises the following steps:
100 parts of polylactic acid ester, 13 parts of poly-p-phenylene terephthalamide, 5 parts of sodium dodecyl benzene sulfonate, 5 parts of citric acid, 15 parts of polyvinyl alcohol, 13 parts of glyceryl monostearate, 18 parts of polyethylene glycol, 10 parts of magnesium phosphate-fibrin glue and 3 parts of zinc chloride are stirred for 30min at 1500r/min to prepare a uniformly mixed solution.
Wherein, the relative molecular weight of the polylactic acid ester is 120000, the relative molecular weight of the polyvinyl alcohol is 30000, and the relative molecular weight of the poly-p-phenylene terephthamide is 60000.
Extruding and melting the prepared polylactic acid mixture of the polylactic acid ester at 200 ℃ by a screw, extruding the molten mixture into melt trickle by electrostatic spinning equipment, extruding the melt trickle by the electrostatic spinning equipment, immersing the melt after spinning into a mixed solution coagulating bath of water and N, N-dimethylacetamide (DMAc) at 10 ℃ for cooling for 15s to obtain nascent fiber; and (3) stretching the nascent fiber, and improving the mechanical property and the dimensional stability of the fiber through guide roller drafting, damp-heat drafting and dry-heat drafting. Heat setting at 200 deg.C, cooling and spraying at normal temperature, steam ironing at 100 deg.C, curling, winding, cutting, and packaging.
According to the preparation method of the embodiment, the length of the sand-carrying fiber is 5 mm-7 mm, and the diameter is 35 μm-37 μm.
FIG. 6 shows SEM test results of single sand-carrying fibers prepared in example 7 of the present invention, and the diameter of the single sand-carrying fibers prepared in this example is measured to be 35 μm to 37 μm from FIG. 6. It should be understood that the above-mentioned embodiments of the present invention are only examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention, and it will be obvious to those skilled in the art that other variations or modifications may be made on the basis of the above description, and all embodiments may not be exhaustive, and all obvious variations or modifications may be included within the scope of the present invention.
Claims (10)
1. The sand-carrying fiber is characterized by being a polylactic acid fiber, and comprising the following raw materials in parts by weight:
100 portions of polylactic acid
12-16 parts of poly (p-phenylene terephthalamide)
3-5 parts of sodium dodecyl benzene sulfonate
2-5 parts of citric acid
15-23 parts of polyvinyl alcohol
10-22 parts of glycerin monostearate
15-25 parts of polyethylene glycol
8-10 parts of magnesium phosphate-fibrin glue
2-3 parts of zinc chloride.
2. The sand-carrying fiber as claimed in claim 1, wherein the polylactic acid has a relative molecular weight of 100000-140000, the polyvinyl alcohol has a relative molecular weight of 25000-35000, and the poly-p-phenylene terephthalamide has a relative molecular weight of 50000-70000.
3. The sand-carrying fiber according to claim 1, wherein the magnesium phosphate-fibrin glue is a mixed product of magnesium phosphate and fibrin glue; preferably, the mass ratio of the magnesium phosphate to the fibrin glue is 1: 5.
4. The sand-carrying fiber of claim 1, wherein the length of the sand-carrying fiber is 5mm to 7 mm.
5. The sand-carrying fiber of claim 1, wherein the diameter of the sand-carrying fiber is 30-37 μ ι η.
6. The sand-carrying fiber according to any one of claims 1 to 5, wherein the surface of the sand-carrying fiber is covered with a film;
preferably, the film has a film material composition comprising: gelatin, plasticizer and water; more preferably, the mass ratio of gelatin, plasticizer and water is 1:0.5: 1.5.
7. A method for preparing a sand-carrying fiber according to any one of claims 1 to 6, comprising the steps of:
melting the mixture of the components, extruding out melt trickle through electrostatic spinning, and immersing the melt after spinning into a coagulating bath for cooling to obtain nascent fiber;
stretching the nascent fiber;
heat setting at 200-220 deg.C, cooling and spraying at normal temperature, steam ironing at 80-100 deg.C, curling, winding, and cutting to obtain the sand-carrying fiber.
8. The method of claim 7, wherein the melting is screw extrusion melting at 200 ℃.
9. The production method according to claim 7, wherein the coagulation bath is composed of a mixed solution of water and N, N-dimethylacetamide;
preferably, the temperature of the coagulation bath is 5 ℃ to 10 ℃; the time for immersing in the coagulating bath for cooling is 10-15 s; preferably, the stretching comprises: guide roller drawing at normal temperature, wet heat drawing in a drawing tank at a temperature of 75 ℃ to 85 ℃, and dry heat drawing in steam at a temperature of 85 ℃ to 100 ℃.
10. Use of the sand-carrying fiber of any one of claims 1-6 in well reservoir fracturing modification;
preferably, the usage amount of the sand-carrying fiber is 0.1-1% of the mass of the fracturing fluid.
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Inventor after: Niu Yingchun Inventor after: Xu Quan Inventor after: Yang Ziji Inventor before: Xu Quan Inventor before: Niu Yingchun Inventor before: Yang Ziji |