CN112048288A - Oil-based drilling fluid filtration loss reducing plugging agent - Google Patents
Oil-based drilling fluid filtration loss reducing plugging agent Download PDFInfo
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- CN112048288A CN112048288A CN202010903920.XA CN202010903920A CN112048288A CN 112048288 A CN112048288 A CN 112048288A CN 202010903920 A CN202010903920 A CN 202010903920A CN 112048288 A CN112048288 A CN 112048288A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/02—Well-drilling compositions
- C09K8/03—Specific additives for general use in well-drilling compositions
- C09K8/035—Organic additives
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/02—Well-drilling compositions
- C09K8/32—Non-aqueous well-drilling compositions, e.g. oil-based
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10C—WORKING-UP PITCH, ASPHALT, BITUMEN, TAR; PYROLIGNEOUS ACID
- C10C3/00—Working-up pitch, asphalt, bitumen
- C10C3/02—Working-up pitch, asphalt, bitumen by chemical means reaction
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Abstract
The invention discloses a fluid loss plugging agent for oil-based drilling fluid, which comprises the following raw materials: asphalt, liquid SO3Chlorosulfonic acid and fuming sulfuric acid, the preparation equipment of the oil-based drilling fluid filtration-reducing plugging agent comprises: the oil-based drilling fluid filtration loss plugging agent comprises a reaction kettle, a grinding machine, a screen and a sulfonation reactor, wherein the oil-based drilling fluid filtration loss plugging agent comprises the following raw materials: CaO, anhydrous CaCl2The detection equipment for the oil-based drilling fluid filtrate loss plugging agent comprises: a high-speed stirrer, an electronic balance, a constant-temperature drying box, an aging tank, a high-temperature high-pressure filtration loss instrument and a standard sieve. The oil-based drilling fluid filtration loss reducing plugging agent has good fluid loss prevention performance, stabilizes well walls, prevents cracks from opening, and is resistant to plugging by an agentThe pressure performance is better, the performance of the reinforced oil-based drilling fluid is stable, micron-sized cracks are effectively blocked by micron-sized particle sizes, and the leak stoppage effect while drilling is good.
Description
Technical Field
The invention relates to the technical field of a fluid loss plugging agent for an oil-based drilling fluid, in particular to a fluid loss plugging agent for an oil-based drilling fluid.
Background
In a gas field with complex geology, abnormal pressure, high temperature and the like, energy sources need to be obtained through various mechanical equipment in the mining process, wherein geological construction needs to be carried out through a drilling machine, the drilling equipment is inconvenient to safely drill into the inside of a land stone block in the using process, so that the oil-based drilling fluid filtrate loss plugging agent needs to be used for assisting construction in the construction process, and the existing oil-based drilling fluid filtrate loss plugging agent generally adopts asphalt as a main material.
With the continuous use of oil-based drilling fluid loss plugging agents, the following problems are found during the use process:
the existing oil-based drilling fluid loss plugging agent has the defects of large water loss and poor plugging resistance, the plugging compression resistance of the existing oil-based drilling fluid loss plugging agent is limited when the existing oil-based drilling fluid loss plugging agent is used, and the effect after plugging is limited.
Therefore, in order to solve the problems, innovative design on the original oil-based drilling fluid filtrate loss plugging agent is urgently needed.
Disclosure of Invention
The invention aims to provide a fluid loss plugging agent for oil-based drilling fluid, which aims to solve the problems that the existing fluid loss plugging agent for oil-based drilling fluid has large water loss and poor anti-blocking performance when in use, the plugging compression resistance of the existing fluid loss plugging agent for oil-based drilling fluid is limited when in use, and the effect after plugging is limited.
In order to achieve the purpose, the invention provides the following technical scheme: the oil-based drilling fluid loss plugging agent comprises the following preparation raw materials: asphalt, liquid SO3Chlorosulfonic acid and fuming sulfuric acid, the preparation equipment of the oil-based drilling fluid filtration-reducing plugging agent comprises: the oil-based drilling fluid filtration loss plugging agent comprises a reaction kettle, a grinding machine, a screen and a sulfonation reactor, wherein the oil-based drilling fluid filtration loss plugging agent comprises the following raw materials: CaO, anhydrous CaCl2The detection equipment for the oil-based drilling fluid filtrate loss plugging agent comprises: a high-speed stirrer, an electronic balance, a constant-temperature drying box, an aging tank, a high-temperature high-pressure filtration loss instrument and a standard sieve.
Preferably, the preparation method of the fluid loss plugging agent for oil-based drilling fluid comprises the following steps:
step one, asphalt raw material oxidation reaction
Putting an asphalt raw material into a reaction kettle, introducing air into the reaction kettle, adjusting the reaction temperature to 150 ℃, controlling the reaction time to be 30min, oxidizing the asphalt to generate oxidized asphalt, increasing the asphaltene and the rubber content of the asphalt material;
step two, sulfonation reaction of the oxidized asphalt material
Adding the oxidized asphalt material into a sulfonation reactor, and sequentially adding liquid SO into the device3Chlorosulfonic acid, fuming sulfuric acid and other acidic materials, controlling the reaction temperature to be 80 ℃, and controlling the reaction time to be 5 hours to generate a sulfonated asphalt product;
step three, grinding and screening
Putting the processed sulfonated asphalt product into a grinder for processing to ensure that the sulfonated asphalt product is small-particle powder, and processing the ground product by using a screen to control the particle diameter of the sulfonated asphalt powder to be 1-1.5 mm;
step four, catalytic reaction of main raw materials
Adding a sulfonated asphalt material and a phenol material into a reaction kettle, stirring and catalyzing raw materials under the conditions of high temperature and high pressure to carry out mixing reaction, controlling the reaction temperature to be 200 ℃, the stirring speed to be 600r/min, and the reaction time to be 2h, thereby generating the oil-based drilling fluid filtration-loss plugging agent.
Preferably, the method for detecting the fluid loss of the fluid loss plugging agent of the oil-based drilling fluid comprises the following steps:
first, obtaining raw material
Extracting CaO and anhydrous CaCl2White oil base, organic soil, oleic acid ethanolamine, stearate, surfactant betaine acid, barite and oil base drilling fluid loss plugging agent samples;
second step, preparation of reagent samples
Taking 5g of oil-based drilling fluid filtration loss reducing plugging agent by using an electronic balance, placing a sample in a constant-temperature drying box, controlling the drying temperature to be 50-85 ℃, drying the sample for 2h, removing water in the sample, taking out the reagent after drying, and naturally cooling for 20 min;
thirdly, preparing base slurry
Taking 20g of organic soil, screening the organic soil by using a standard screen, placing the screened organic soil in a high-speed stirrer, and then adding 460ml of white oil base (the density is 1.8 g/cm)3) 15g CaO, 22g oleic acid ethanolamine, 27g stearate and 50ml anhydrous CaCl2835g of barite powder and 3.2g of surfactant betaine acid are added into a high-speed stirrer, the rotating speed of the stirrer is controlled to be 11000r/min, the mixture is stirred at high speed for 15min at the room temperature of 18-25 ℃, and the base slurry is taken out and kept stand for 90 min;
step four, aging treatment of the base slurry
Placing the prepared base slurry in an aging tank, controlling the operation temperature to be 150-;
fifth step, fluid loss detection
And respectively putting the prepared base slurry and the reagent into a high-temperature high-pressure filtration apparatus, controlling the detection temperature of the equipment to be 120 ℃, the rotation speed to be 800-.
Preferably, the plugging compression resistance of the oil-based drilling fluid filtrate loss plugging agent is detected as follows:
(I) extraction reagent
Extracting 6 parts of 5g of the oil-based drilling fluid filtrate loss reducing plugging agent, and putting the oil-based drilling fluid filtrate loss reducing plugging agent into different containers for later use;
(II) selecting and testing steel material
Selecting steel materials with crack sizes of 100 microns, 200 microns, 300 microns and 400 microns;
(III) detection of plugging compression resistance
Plugging a reagent on the surface of a crack of a steel material at 120 ℃, and applying different pressures to different detection materials, wherein the detection pressures are respectively 3.5MPa, 5MPa, 10MPa, 15MPa and 20 MPa;
(IV) the results of the detection
The oil-based drilling fluid filtration loss plugging agent can effectively plug and prevent 100-inch crack leakage of 300 mu m, and the pressure-bearing micro crack of 20MPa and 400 mu m needs to adopt a plugging technology.
Compared with the prior art, the invention has the beneficial effects that:
the asphalt raw material in the fluid loss plugging agent for the oil-based drilling fluid is subjected to oxidation and sulfonation reaction treatment, the asphaltene of the material is increased, the rubber content is increased, the effects of fluid loss reduction, lubrication and blockage prevention are achieved, and the agent generated by the main material after catalytic reaction is higher in anti-blocking and fluid loss prevention performance;
after detection, the fluid loss plugging agent for reducing the fluid loss of the oil-based drilling fluid, prepared by the invention, has the advantages of less than 8.0ml of fluid loss, better fluid loss prevention performance, well wall stabilization, crack opening prevention, effective plugging and prevention of the micro-crack leakage of 100-plus-300 mu m, bearing pressure of 20MPa, better plugging compression resistance of the agent, stable performance of the enhanced oil-based drilling fluid, effective plugging of micron-sized cracks with micron-sized particle size and good plugging effect while drilling.
Drawings
FIG. 1 is a schematic diagram of fluid loss detection data according to the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1, the present invention provides a technical solution: the oil-based drilling fluid loss plugging agent comprises the following raw materials: asphalt, liquid SO3Chlorosulfonic acid and fuming sulfuric acid, and the preparation equipment of the oil-based drilling fluid filtration-reducing plugging agent comprises: the oil-based drilling fluid filtration loss plugging agent detection raw materials comprise: CaO, anhydrous CaCl2White oil base, organic soil, oleic acid ethanolamine,Stearate, a surfactant, beet acid and barite powder, and the equipment for detecting the fluid loss plugging agent of the oil-based drilling fluid comprises: a high-speed stirrer, an electronic balance, a constant-temperature drying box, an aging tank, a high-temperature high-pressure filtration loss instrument and a standard sieve.
The preparation method of the oil-based drilling fluid filtrate loss plugging agent comprises the following steps:
the first embodiment is as follows:
step one, asphalt raw material oxidation reaction
Putting an asphalt raw material into a reaction kettle, introducing air into the reaction kettle, adjusting the reaction temperature to 120 ℃, controlling the reaction time to be 20min, oxidizing the asphalt to generate oxidized asphalt, increasing the asphaltene and the rubber content of the asphalt material;
step two, sulfonation reaction of the oxidized asphalt material
Adding the oxidized asphalt material into a sulfonation reactor, and sequentially adding liquid SO into the device3Chlorosulfonic acid, fuming sulfuric acid and other acidic materials, controlling the reaction temperature at 60 ℃ and the reaction time at 5h to generate a sulfonated asphalt product;
step three, grinding and screening
Putting the processed sulfonated asphalt product into a grinder for processing to enable the sulfonated asphalt product to be small-particle powder, and processing the ground product by using a screen to control the particle diameter of the sulfonated asphalt powder to be 1.1 mm;
step four, catalytic reaction of main raw materials
Adding a sulfonated asphalt material and a phenol material into a reaction kettle, stirring and catalyzing raw materials under the conditions of high temperature and high pressure for mixing reaction, controlling the reaction temperature to be 150 ℃, the stirring rotation speed to be 400r/min, and the reaction time to be 2h to generate the oil-based drilling fluid filtration-loss plugging agent.
Example two:
step one, asphalt raw material oxidation reaction
Putting an asphalt raw material into a reaction kettle, introducing air into the reaction kettle, adjusting the reaction temperature to 150 ℃, controlling the reaction time to be 30min, oxidizing the asphalt to generate oxidized asphalt, increasing the asphaltene and the rubber content of the asphalt material;
step two, sulfonation reaction of the oxidized asphalt material
Adding the oxidized asphalt material into a sulfonation reactor, and sequentially adding liquid SO into the device3Chlorosulfonic acid, fuming sulfuric acid and other acidic materials, controlling the reaction temperature to be 80 ℃, and controlling the reaction time to be 5 hours to generate a sulfonated asphalt product;
step three, grinding and screening
Putting the processed sulfonated asphalt product into a grinder for processing to enable the sulfonated asphalt product to be small-particle powder, and processing the ground product by using a screen to control the particle diameter of the sulfonated asphalt powder to be 1.25 mm;
step four, catalytic reaction of main raw materials
Adding a sulfonated asphalt material and a phenol material into a reaction kettle, stirring and catalyzing raw materials under the conditions of high temperature and high pressure to carry out mixing reaction, controlling the reaction temperature to be 200 ℃, the stirring speed to be 600r/min, and the reaction time to be 2h, thereby generating the oil-based drilling fluid filtration-loss plugging agent.
Example three:
step one, asphalt raw material oxidation reaction
Putting an asphalt raw material into a reaction kettle, introducing air into the reaction kettle, adjusting the reaction temperature to 170 ℃, controlling the reaction time to be 40min, oxidizing the asphalt to generate oxidized asphalt, increasing the asphaltene and the rubber content of the asphalt material;
step two, sulfonation reaction of the oxidized asphalt material
Adding the oxidized asphalt material into a sulfonation reactor, and sequentially adding liquid SO into the device3Chlorosulfonic acid, fuming sulfuric acid and other acidic materials, controlling the reaction temperature at 90 ℃ and the reaction time at 4h to generate a sulfonated asphalt product;
step three, grinding and screening
Putting the processed sulfonated asphalt product into a grinder for processing to enable the sulfonated asphalt product to be small-particle powder, and processing the ground product by using a screen to control the particle diameter of the sulfonated asphalt powder to be 1.5 mm;
step four, catalytic reaction of main raw materials
Adding a sulfonated asphalt material and a phenol material into a reaction kettle, stirring and catalyzing raw materials under the conditions of high temperature and high pressure for mixing reaction, controlling the reaction temperature to be 220 ℃, the stirring rotation speed to be 800r/min, and the reaction time to be 2h to generate the oil-based drilling fluid filtration-loss plugging agent.
The method for detecting the filtration loss of the oil-based drilling fluid filtrate loss plugging agent comprises the following steps:
first, obtaining raw material
Extracting CaO and anhydrous CaCl2White oil base, organic soil, oleic acid ethanolamine, stearate, surfactant betaine acid, barite and oil base drilling fluid loss plugging agent samples;
second step, preparation of reagent samples
Taking 5g of oil-based drilling fluid filtration loss reducing plugging agent by using an electronic balance, placing a sample in a constant-temperature drying box, controlling the drying temperature to be 50-85 ℃, drying the sample for 2h, removing water in the sample, taking out the reagent after drying, and naturally cooling for 20 min;
thirdly, preparing base slurry
Taking 20g of organic soil, screening the organic soil by using a standard screen, placing the screened organic soil in a high-speed stirrer, and then adding 460ml of white oil base (the density is 1.8 g/cm)3) 15g CaO, 22g oleic acid ethanolamine, 27g stearate and 50ml anhydrous CaCl2835g of barite powder and 3.2g of surfactant betaine acid are added into a high-speed stirrer, the rotating speed of the stirrer is controlled to be 11000r/min, the mixture is stirred at high speed for 15min at the room temperature of 18-25 ℃, and the base slurry is taken out and kept stand for 90 min;
step four, aging treatment of the base slurry
Placing the prepared base slurry in an aging tank, controlling the operation temperature to be 150-;
fifth step, fluid loss detection
Respectively placing the prepared base slurry and the reagent into a high-temperature high-pressure filtration apparatus, controlling the detection temperature of the equipment to be 120 ℃, the rotation speed to be 800-;
the plugging compression resistance of the oil-based drilling fluid loss plugging agent is detected as follows:
(I) extraction reagent
Extracting 6 parts of 5g of the oil-based drilling fluid filtrate loss reducing plugging agent, and putting the oil-based drilling fluid filtrate loss reducing plugging agent into different containers for later use;
(II) selecting and testing steel material
Selecting steel materials with crack sizes of 100 microns, 200 microns, 300 microns and 400 microns;
(III) detection of plugging compression resistance
Plugging a reagent on the surface of a crack of a steel material at 120 ℃, and applying different pressures to different detection materials, wherein the detection pressures are respectively 3.5MPa, 5MPa, 10MPa, 15MPa and 20 MPa;
(IV) the results of the detection
The oil-based drilling fluid filtration loss plugging agent can effectively plug and prevent 100-inch crack leakage of 300 mu m, and the pressure-bearing micro crack of 20MPa and 400 mu m needs to adopt a plugging technology.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (4)
1. The oil-based drilling fluid loss plugging agent is characterized by comprising the following components in parts by weight: the oil-based drilling fluid filtration loss plugging agent comprises the following raw materials: asphalt, liquid SO3Chlorosulfonic acid and fuming sulfuric acid, the preparation equipment of the oil-based drilling fluid filtration-reducing plugging agent comprises: the oil-based drilling fluid filtration loss plugging agent comprises a reaction kettle, a grinding machine, a screen and a sulfonation reactor, wherein the oil-based drilling fluid filtration loss plugging agent comprises the following raw materials: CaO, anhydrous CaCl2The detection equipment for the oil-based drilling fluid filtrate loss plugging agent comprises: high-speed stirrer, electronic balance, constant-temperature drying oven, aging tank and high-temperature and high-pressure deviceA fluid loss instrument and a standard sieve.
2. The oil-based drilling fluid loss plugging agent of claim 1, wherein the preparation method of the oil-based drilling fluid loss plugging agent comprises the following steps:
step one, asphalt raw material oxidation reaction
Putting an asphalt raw material into a reaction kettle, introducing air into the reaction kettle, adjusting the reaction temperature to 150 ℃, controlling the reaction time to be 30min, oxidizing the asphalt to generate oxidized asphalt, increasing the asphaltene and the rubber content of the asphalt material;
step two, sulfonation reaction of the oxidized asphalt material
Adding the oxidized asphalt material into a sulfonation reactor, and sequentially adding liquid SO into the device3Chlorosulfonic acid, fuming sulfuric acid and other acidic materials, controlling the reaction temperature to be 80 ℃, and controlling the reaction time to be 5 hours to generate a sulfonated asphalt product;
step three, grinding and screening
Putting the processed sulfonated asphalt product into a grinder for processing to ensure that the sulfonated asphalt product is small-particle powder, and processing the ground product by using a screen to control the particle diameter of the sulfonated asphalt powder to be 1-1.5 mm;
step four, catalytic reaction of main raw materials
Adding a sulfonated asphalt material and a phenol material into a reaction kettle, stirring and catalyzing raw materials under the conditions of high temperature and high pressure to carry out mixing reaction, controlling the reaction temperature to be 200 ℃, the stirring speed to be 600r/min, and the reaction time to be 2h, thereby generating the oil-based drilling fluid filtration-loss plugging agent.
3. The oil-based drilling fluid loss plugging agent of claim 2, wherein the method for detecting the fluid loss of the oil-based drilling fluid loss plugging agent comprises the following steps:
first, obtaining raw material
Extracting CaO and anhydrous CaCl2White oil base, organic soil, oleic acid ethanolamine, stearate, surfactant betaine acid, barite and oil base drilling fluid loss plugging agent samples;
second step, preparation of reagent samples
Taking 5g of oil-based drilling fluid filtration loss reducing plugging agent by using an electronic balance, placing a sample in a constant-temperature drying box, controlling the drying temperature to be 50-85 ℃, drying the sample for 2h, removing water in the sample, taking out the reagent after drying, and naturally cooling for 20 min;
thirdly, preparing base slurry
Taking 20g of organic soil, screening the organic soil by using a standard screen, placing the screened organic soil in a high-speed stirrer, and then adding 460ml of white oil base (the density is 1.8 g/cm)3) 15g CaO, 22g oleic acid ethanolamine, 27g stearate and 50ml anhydrous CaCl2835g of barite powder and 3.2g of surfactant betaine acid are added into a high-speed stirrer, the rotating speed of the stirrer is controlled to be 11000r/min, the mixture is stirred at high speed for 15min at the room temperature of 18-25 ℃, and the base slurry is taken out and kept stand for 90 min;
step four, aging treatment of the base slurry
Placing the prepared base slurry in an aging tank, controlling the operation temperature to be 150-;
fifth step, fluid loss detection
And respectively putting the prepared base slurry and the reagent into a high-temperature high-pressure filtration apparatus, controlling the detection temperature of the equipment to be 120 ℃, the rotation speed to be 800-.
4. The oil-based drilling fluid loss plugging agent of claim 2, wherein: the plugging compression resistance of the oil-based drilling fluid loss plugging agent is detected as follows:
(I) extraction reagent
Extracting 6 parts of 5g of the oil-based drilling fluid filtrate loss reducing plugging agent, and putting the oil-based drilling fluid filtrate loss reducing plugging agent into different containers for later use;
(II) selecting and testing steel material
Selecting steel materials with crack sizes of 100 microns, 200 microns, 300 microns and 400 microns;
(III) detection of plugging compression resistance
Plugging a reagent on the surface of a crack of a steel material at 120 ℃, and applying different pressures to different detection materials, wherein the detection pressures are respectively 3.5MPa, 5MPa, 10MPa, 15MPa and 20 MPa;
(IV) the results of the detection
The oil-based drilling fluid filtration loss plugging agent can effectively plug and prevent 100-inch crack leakage of 300 mu m, and the pressure-bearing micro crack of 20MPa and 400 mu m needs to adopt a plugging technology.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102276992A (en) * | 2011-04-21 | 2011-12-14 | 河南金马石油科技有限责任公司 | Modified sulphurized asphalt used for drilling fluid and preparation method thereof, |
| CN108410437A (en) * | 2018-05-09 | 2018-08-17 | 天津市大港渤中石油助剂有限公司 | Drilling fluid sealing agent low Poison sulfonated gilsonite |
| CN109097013A (en) * | 2018-09-06 | 2018-12-28 | 中国海洋石油集团有限公司 | A kind of high temperature resisting type oil base drilling fluid pressure-bearing sealing agent and preparation method thereof |
-
2020
- 2020-09-01 CN CN202010903920.XA patent/CN112048288A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102276992A (en) * | 2011-04-21 | 2011-12-14 | 河南金马石油科技有限责任公司 | Modified sulphurized asphalt used for drilling fluid and preparation method thereof, |
| CN108410437A (en) * | 2018-05-09 | 2018-08-17 | 天津市大港渤中石油助剂有限公司 | Drilling fluid sealing agent low Poison sulfonated gilsonite |
| CN109097013A (en) * | 2018-09-06 | 2018-12-28 | 中国海洋石油集团有限公司 | A kind of high temperature resisting type oil base drilling fluid pressure-bearing sealing agent and preparation method thereof |
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| Title |
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| 来胜利: "《常用精细化工产品研制与生产》", 31 October 2006 * |
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Application publication date: 20201208 |