Crucible lining and manufacturing method and using method thereof
By embedding crucible linings made of purple sand mud and other materials into the nickel-based crucible, the problems of nickel-based crucibles are easily deficient, cost and data deviation in rock pyrolysis experiments, achieving more efficient experimental data accuracy and cost savings.
Patent Information
- Application Number
- CN202311268660.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2023-09-27
- Publication Date
- 2025-03-28
AI Technical Summary
Existing nickel-based crucibles are easily contaminated in rock pyrolysis experiments, have high usage costs, and are difficult to clean residues, resulting in data deviations and samples with high carbonate content are prone to cementing and damage.
It adopts a crucible lining, the main material is purple sand mud, quartz fiber, mullite powder and pore-forming agent, and is made through high-temperature firing, shape and grinding, and is nested in a nickel-based crucible.
It effectively reduces the loss of nickel-based crucible, increases service life, improves the accuracy of pyrolysis data, reduces experimental analysis costs, and saves metal resources.
Smart Images
Figure CN119707509A_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of oil and gas geochemical testing, and in particular to a crucible lining and a manufacturing method and a use method thereof. Background Art
[0002] Rock pyrolysis analysis technology plays an important role in the evaluation of source rocks. The Rock-eval rock pyrolysis instrument can quickly and effectively obtain information on the abundance, maturity and hydrocarbon generation potential of organic matter in source rocks. This technology has been widely used in the field of oil and gas exploration. The Rock-eval rock pyrolysis instrument was first developed and manufactured by the French Petroleum Institute in 1977, and a set of plates and specifications for evaluating source rocks using the analytical data of this instrument was proposed. At present, the Rock-eval series used at home and abroad are mainly 6th and 7th generation products, mainly composed of double heating furnaces, FID detectors, temperature measuring thermocouples, infrared detectors, automatic samplers, gas circuits and software control systems.
[0003] The samples for rock pyrolysis analysis are mainly shale, carbonate rock, clastic rock and coal. The samples need to be crushed before loading. The crucible used for loading is a nickel-based alloy crucible dedicated to Rock-eval rock pyrolysis instrument. The crucible is 15mm high and 8mm in diameter. The middle lower position of the nickel-based alloy crucible and the crucible cover are equipped with a filter screen. The mesh size is smaller than the sample particle size, which plays a role in supporting the sample and circulating the carrier gas. The design specifications of the nickel-based crucible are suitable for the automatic sampler and injection rod of the pyrolysis instrument, and are precision consumables. This special nickel-based crucible has the following problems in actual use: 1. The rock pyrolysis experiment requires the nickel-based crucible containing the sample to be placed in a pyrolysis furnace (300℃~650℃) and an oxidation furnace (300℃~850℃) for burning. The residues after the sample is burned will adhere to the inner wall of the crucible and the filter screen, which is difficult to clean up, causing deviations in the next batch of data; 2. Samples with a high carbonate content will all be cemented in the crucible after burning and cannot be removed, causing damage to the crucible; 3. After a certain period of use, the crucible needs to be cleaned with hydrochloric acid or a mixed solution of chloroform and methanol. During the cleaning process, the filter screen is also easily damaged. After the filter screen is damaged, the entire crucible will be unusable. In addition, this crucible is expensive, with a current market price of about 1,600 yuan per piece. The detection activities for large quantities of samples undoubtedly bring high usage costs to experimental analysis. Moreover, at present, major oilfield enterprises, relevant scientific research institutions and universities at home and abroad conduct countless rock pyrolysis analysis experiments every year, and the loss and high use cost of nickel-based crucibles are also increasing year by year. Summary of the invention
[0004] The present application provides a crucible lining and a manufacturing method and a use method thereof, so as to solve the above-mentioned technical problems that the crucible in water in the prior art is easily contaminated and has high use cost.
[0005] According to one aspect of the present application, an embodiment provides a crucible lining containing the following components in mass percentage: 60-70% purple clay, 10-12% purple clay clinker, 5-6% quartz fiber, 5-6% mullite powder, 5-8% pore-forming agent, and 8-10% deionized water.
[0006] In one embodiment, the purple clay clinker is made by burning purple clay into clinker and then crushing it.
[0007] In one embodiment, the firing temperature of the purple clay clinker is 1280° C.; the mesh size of the purple clay clinker particles is 80 meshes.
[0008] In one embodiment, the pore-forming agent is ammonium bicarbonate.
[0009] According to one aspect of the present application, an embodiment provides a method for manufacturing a crucible lining as described in any one of the above items, comprising the following steps:
[0010] S11. Clinker production: purple sand clay is fired at high temperature to obtain clinker, which is then crushed for later use;
[0011] S12. Clay ratio: prepare the clay according to the components and their dosage;
[0012] S13, shaping: putting the clay into a mold to shape it; after the clay is dried, removing the mold to obtain a green body;
[0013] S14, firing: firing the blank at high temperature to obtain the finished product;
[0014] S15, grinding: grinding the outer wall of the crucible lining to match the inner wall of the crucible;
[0015] S16, Firing: Firing the polished crucible lining and cooling it.
[0016] In one embodiment, in step S1, the firing temperature of the purple clay clinker is 1280° C.; after crushing, the mesh size of the purple clay clinker particles is 80 meshes.
[0017] In one embodiment, in step S3, the clay is placed in a female mold and pressed into the female mold with a male mold, and the model is removed after the clay is naturally dried.
[0018] In one embodiment, in step S6, the polished crucible lining is placed in a muffle furnace and calcined at 850° C. for 20 minutes.
[0019] According to one aspect of the present application, an embodiment provides a method for using a crucible lining as described in any one of the above items,
[0020] S21, weighing the powder of purple sand mud clinker and pouring it into the bottom of the crucible, so that the powder is evenly spread on the filter screen at the bottom of the crucible;
[0021] S22, placing a crucible liner in the crucible;
[0022] S23, weighing the rock powder sample to be tested and placing it into the inner lining of the crucible;
[0023] S24, weighing the powder of purple sand mud clinker and pouring it into the inner lining of the crucible to cover the rock powder sample to be tested;
[0024] S25. Cover the crucible with a lid and perform pyrolysis treatment on the rock powder sample to be tested.
[0025] In one embodiment, the crucible is a nickel-based crucible.
[0026] The crucible lining of the above-mentioned embodiment is mainly made of purple sand clay with good air permeability and high temperature resistance. At the same time, different proportions of quartz fiber, mullite powder and pore-forming agent are added to improve the plasticity, high temperature resistance, corrosion resistance, air permeability and strength of the crucible lining. It is made through the steps of shaping, calcining, polishing, etc. The crucible lining is simple to make and low in cost, and can be applied to the rock pyrolysis analysis test of a large number of samples. In addition, the crucible lining is embedded in the crucible for use, and purple sand clay clinker powder is laid, which can effectively reduce the loss of the crucible in the pyrolysis experiment, increase the number of times the crucible is used, improve the accuracy of the pyrolysis data, and reduce the cost of laboratory analysis. BRIEF DESCRIPTION OF THE DRAWINGS
[0027] Figure 1 is a schematic diagram of a crucible lining in an embodiment of the present application;
[0028] Figure 2 is a schematic diagram of the appearance of a crucible lining in an embodiment of the present application;
[0029] Figure 3 It is a schematic diagram of a crucible liner in cooperation with a crucible for sample placement in one embodiment of the present application;
[0030] Reference numerals:
[0031] 1-crucible cover; 2-nickel-based crucible; 3-rock powder sample to be tested; 4-filter; 5-crucible cover filter; 6-crucible lining; 7-purple clay clinker powder. DETAILED DESCRIPTION
[0032] It should be noted that, in the absence of conflict, the embodiments and features in the embodiments of the present application can be combined with each other. The present application will be described in detail below with reference to the accompanying drawings and in combination with the embodiments.
[0033] In order to enable those skilled in the art to better understand the present application, the technical solutions in the embodiments of the present application will be clearly and completely described below in conjunction with the drawings in the embodiments of the present application. Obviously, the described embodiments are only embodiments of a part of the present application, not all embodiments. Based on the embodiments in the present application, all other embodiments obtained by ordinary technicians in the field without creative work should fall within the scope of protection of the present application.
[0034] It should be noted that the terms "first", "second" etc. in the present application are used to distinguish similar objects, and need not be used to describe a specific order or sequential order. It should be understood that the data used in this way can be interchanged in appropriate circumstances, so that the embodiments of the present application described here. In addition, the terms "including" and "having" and any of their variations are intended to cover non-exclusive inclusions, for example, the process, method, system, product or equipment comprising a series of steps or units need not be limited to those steps or units clearly listed, but may include other steps or units that are not clearly listed or inherent to these processes, methods, products or equipment.
[0035] It should be understood that when an element (such as a layer, film, region, or substrate) is described as being "on" another element, the element may be directly on the other element, or there may be an intermediate element. Moreover, in this application, when an element is described as being "connected" to another element, the element may be "directly connected" to the other element, or "connected" to the other element through a third element.
[0036] Embodiment 1
[0037] In order to reduce the loss of nickel-based crucibles in rock pyrolysis experiments, improve data accuracy, reduce experimental analysis costs, and save metal resources; a crucible lining is invented to solve the problems existing in the use of nickel-based crucibles, which has been described in the background technology.
[0038] For details, please refer to Figure 1 One embodiment of the present application provides a crucible lining, which contains the following components by mass percentage: 60-70% purple sand mud, 10-12% purple sand mud clinker, 5-6% quartz fiber, 5-6% mullite powder, 5-8% pore-forming agent, and 8-10% deionized water. Among them, the role of quartz fiber is to enhance the strength of the crucible lining, and it is not easy to be damaged in later use; the main role of mullite powder is corrosion resistance, and it is easy to demold after the green body is pressed with a model.
[0039] In one embodiment, the pore-forming agent is ammonium bicarbonate, which releases carbon dioxide and ammonia during firing, thereby improving the porosity and mechanical properties of the crucible lining.
[0040] In one embodiment, the purple clay clinker is made by pulverizing purple clay after being fired into clinker. Preferably, the firing temperature of the purple clay clinker is 1280°C; and the mesh number of the purple clay clinker particles is 80 meshes.
[0041] In the above technical scheme, the main material for making the crucible lining is purple sand clay with good air permeability and high temperature resistance. At the same time, quartz fiber, mullite powder and pore-forming agent in different proportions are added to improve the plasticity, high temperature resistance, corrosion resistance, air permeability and strength of the crucible lining. It is made through shaping, calcining and polishing.
[0042] The crucible lining made of the above ratio can reduce the loss of nickel-based crucibles in rock pyrolysis experiments, improve data accuracy, reduce experimental analysis costs, and save metal resources. It is necessary to provide an invention to solve the problems existing in the use of nickel-based crucibles.
[0043] The crucible lining of the invention is simple to manufacture and low in cost, and can be applied to the rock pyrolysis analysis test of a large number of samples. A method for manufacturing the crucible lining is further provided, as shown in the following embodiment 2.
[0044] The crucible lining of the invention is nested in the nickel-based crucible during use, which can reduce the loss of the crucible in the rock pyrolysis experiment, increase the service life of the crucible, reduce the experimental analysis cost, and achieve the effect of energy saving and environmental protection. A method for using the crucible lining is further provided, see the following embodiment three.
[0045] Embodiment 2
[0046] Please refer to Figure 1 , Figure 2 An embodiment of the present application provides a method for manufacturing a crucible lining, comprising the following steps:
[0047] S11. Clinker production: purple sand clay is fired at high temperature to obtain clinker, which is then crushed for later use;
[0048] S12. Clay ratio: prepare the clay according to the components and their dosage;
[0049] S13, shaping: putting the clay into a mold to shape it; after the clay is dried, removing the mold to obtain a green body;
[0050] S14, firing: firing the blank at high temperature to obtain the finished product;
[0051] S15, grinding: grinding the outer wall of the crucible lining to match the inner wall of the crucible;
[0052] S16, Firing: Firing the polished crucible lining and cooling it.
[0053] In one embodiment, in step S1, the firing temperature of the purple clay clinker is 1280°C; after crushing, the mesh size of the purple clay clinker particles is 80 mesh. Preferably, after the purple clay clinker is fired, it needs to be cooled naturally, and then the clinker is ground and sieved with 80 mesh to obtain clinker powder.
[0054] In one embodiment, in step S3, the clay is placed in a female mold, and the male mold is pressed into the female mold. After the clay is naturally dried, the model is removed. Preferably, the model is a gypsum model, and the male mold and the female mold are made of gypsum. Preferably, the height of the crucible lining is 6 mm, the diameter is 6 mm, and the thickness is 0.8 mm. Figure 2 .
[0055] In one embodiment, in step S6, the polished crucible lining is placed in a muffle furnace and fired at 850° C. for 20 minutes. After the firing is completed, the crucible is cooled.
[0056] Through the above steps, a crucible lining suitable for rock pyrolysis can be manufactured, which can be used in conjunction with a crucible. A method for using the crucible lining is further provided, as shown in the following embodiment 3.
[0057] Embodiment 3
[0058] Please refer to Figure 1-Figure 3 An embodiment of the present application provides a method for using a crucible lining, comprising the following steps:
[0059] S21, weighing the powder of purple sand mud clinker (i.e., purple sand mud clinker powder 7) and pouring it into the bottom of the crucible, so that the powder is evenly spread on the filter screen 4 at the bottom of the crucible;
[0060] S22, placing the crucible liner 6 in the crucible;
[0061] S23, weighing an appropriate amount of the rock powder sample 3 to be tested and putting it into the crucible lining 6;
[0062] S24, weigh the powder of purple sand mud clinker and pour it into the crucible lining 6 to cover the rock powder sample 3 to be tested;
[0063] S25, cover the crucible with lid 1;
[0064] Afterwards, the crucible containing the rock powder sample 3 to be tested together with the crucible lining 6 is put on the test machine for testing, and the rock powder sample 3 to be tested is subjected to pyrolysis treatment.
[0065] In one embodiment, the crucible is a nickel-based crucible 2 . The upper and lower layers of purple sand mud clinker powder 7 play a role in protecting the filter screen 4 of the nickel-based crucible 2 .
[0066] In one embodiment, in actual use, the purple sand mud clinker powder 7 at the bottom of the nickel-based crucible 2 is 10-15 mg.
[0067] In one embodiment, in actual use, the amount of purple sand mud clinker powder 7 in the crucible lining 6 is 10-15 mg.
[0068] Embodiment 4
[0069] In view of the problems that nickel-based crucibles in rock pyrolysis experiments are difficult to clean, easy to damage, and have high purchase costs, the present invention provides a crucible lining and a manufacturing method and a use method thereof, which can effectively reduce the loss of nickel-based crucibles in pyrolysis experiments, increase the number of times the crucible is used, improve the accuracy of pyrolysis data, and reduce laboratory analysis costs.
[0070] For details, please refer to Figure 1 , Figure 2 . Taking the nickel-based crucible for rock pyrolysis as a reference / basis, a crucible lining that can be embedded in the nickel-based crucible is made. Preferably, the crucible lining has a height of 6 mm, a diameter of 6 mm, and a thickness of 0.8 mm. The main material for making the crucible lining is purple sand mud. The crucible lining suitable for rock pyrolysis can be made by the following steps.
[0071] 1. Clinker production: burn the purple clay at 1280℃ to make clinker, and crush the fired clinker into 80 mesh for later use.
[0072] 2. Clay ratio: The clay used to make the crucible lining includes the following components in percentage by mass: 60-70% purple sand clay, 10-12% clinker, 5-6% quartz fiber, 5-6% mullite powder, 5-8% pore-forming agent, and 8-10% deionized water.
[0073] 3. Shaping and firing: Put the clay into the female mold of the gypsum model, press the male mold into the middle of the female mold, and after the clay is naturally dried, remove the gypsum model, and the semi-finished product of the crucible lining is ready; after the semi-finished product is dried in the shade for 48 hours, place it in a kiln and fire it for 12 hours at a firing temperature of 1280°C, and take it out after cooling down.
[0074] 4. Grinding: Use sandpaper to grind the outer wall of the fired crucible lining to make it smooth so that the nickel-based crucible can be easily put in and taken out. Then, place the polished crucible lining in a muffle furnace and burn it at 850℃ for 20 minutes, and set it aside after cooling.
[0075] It should be noted that when making the crucible lining, the material mainly used is purple clay, which has stable physical and chemical properties after firing, good air permeability and is not easy to deform. Other components include purple clay clinker, quartz fiber, mullite powder and pore-forming agent.
[0076] Since the crucible lining is very small in size and thickness, it is difficult to make and fire. Therefore, clinker needs to be added during production, which increases the support for characterization and firing. Clinker is made by firing purple sand mud at 1280℃ in a kiln. After natural cooling, the clinker is ground and sieved through 80 mesh. The role of quartz fiber is to enhance the strength of the crucible lining, so that it is not easily damaged during later use; the main role of mullite powder is corrosion resistance, and it is easy to shell after being pressed with a gypsum model; the pore-forming agent is ammonium bicarbonate, which will release carbon dioxide and ammonia during firing, improving the porosity and mechanical properties of the crucible lining.
[0077] In actual production, a preferred solution is that the clay ratio is set to: 65% purple clay, 15% purple clay clinker, 6% quartz fiber, 6% mullite powder, and 12% pore-forming agent.
[0078] Since the nickel-based crucible used in the rock pyrolysis experiment is a consumable material, it is expensive and has a high experimental cost, and the residue in the crucible will cause data errors if it is not cleaned in time. In order to solve the above-mentioned problems existing in the use of nickel-based crucibles in rock pyrolysis experiments, the present invention provides the above-mentioned crucible lining and manufacturing method, and the design size and specifications are suitable for the nickel-based crucible used in the Rock-eval6 rock pyrolysis experiment. The crucible lining is nested in the nickel-based crucible for use, which can reduce the loss of the crucible in the rock pyrolysis experiment, increase the service life of the crucible, reduce the experimental analysis cost, and achieve the effect of energy saving and environmental protection. The crucible lining of the invention is simple to manufacture and low in cost, and can be applied to rock pyrolysis analysis tests of a large number of samples.
[0079] Embodiment 5
[0080] In one embodiment of the present application, the above-mentioned crucible lining is put into practical use.
[0081] Rock pyrolysis experiments can detect multiple parameters of the sample, including adsorbed hydrocarbons S1, cracked hydrocarbons S2, organic carbon dioxide S3, organic carbon monoxide S3CO, organic and mineral carbon monoxide S3'CO, yield index PI, pyrolysis peak temperature Tmax, effective organic carbon PC, residual organic carbon RC, total organic carbon TOC, hydrogen index HI, oxygen index OI, etc.
[0082] In the pyrolysis experiment, whether the placement of the crucible lining will affect the pyrolysis analysis of the actual sample needs to be investigated through a pyrolysis experiment. The crucible lining involved in the present invention is placed in a nickel-based crucible, and then 40 mg of purple clay clinker is loaded, and the machine is tested. From the experimental results, it can be seen that the parameters detected by the crucible lining and the purple clay are basically zero (as shown in Table 1); therefore, the use of the crucible lining of the present invention will not affect the pyrolysis data and can be put into normal use.
[0083]
[0084] Table 1 Crucible lining pyrolysis data statistics
[0085] The above description is only the preferred embodiment of the present application and is not intended to limit the present application. For those skilled in the art, the present application may have various modifications and variations. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application shall be included in the protection scope of the present application.
Claims
1. A crucible lining, characterized in that: The invention contains the following components in percentage by mass: 60-70% of purple sand mud, 10-12% of purple sand mud clinker, 5-6% of quartz fiber, 5-6% of mullite powder, 5-8% of pore-forming agent and 8-10% of deionized water.
2. A crucible lining according to claim 1, characterized in that: The purple sand clay clinker is prepared by burning the purple sand clay into clinker and then crushing it.
3. A crucible lining according to claim 2, characterized in that: The firing temperature of the purple clay clinker is 1280° C.; the mesh size of the purple clay clinker particles is 80 meshes.
4. A crucible lining according to any one of claims 1 to 3, characterized in that: The pore-forming agent is ammonium bicarbonate.
5. A method for manufacturing a crucible lining according to any one of claims 1 to 4, characterized in that: The following steps are involved: S11. Clinker production: purple sand clay is fired at high temperature to obtain clinker, which is then crushed for later use; S12. Clay ratio: prepare the clay according to the components and their dosage; S13, shaping: putting the clay into a mold to shape it; after the clay is dried, removing the mold to obtain a green body; S14, firing: firing the blank at high temperature to obtain the finished product; S15, grinding: grinding the outer wall of the crucible lining to match the inner wall of the crucible; S16, Firing: Firing the polished crucible lining and cooling it.
6. The method for making a crucible lining according to claim 5, characterized in that: In step S1, the firing temperature of the purple clay clinker is 1280° C.; after being crushed, the mesh size of the purple clay clinker particles is 80 meshes.
7. The method for making a crucible lining according to claim 5, characterized in that: In step S3, the clay is placed in the female mold and pressed into the female mold with the male mold. After the clay is naturally dried, the model is removed.
8. The method for making a crucible lining according to claim 5, characterized in that: In step S6, the polished crucible lining is placed in a muffle furnace and fired at 850° C. for 20 minutes.
9. A method for using the crucible lining according to any one of claims 1 to 4, characterized in that: The following steps are involved: S21, weighing the powder of purple sand mud clinker and pouring it into the bottom of the crucible, so that the powder is evenly spread on the filter screen at the bottom of the crucible; S22, placing a crucible liner in the crucible; S23, weighing the rock powder sample to be tested and placing it into the inner lining of the crucible; S24, weighing the powder of purple sand mud clinker and pouring it into the inner lining of the crucible to cover the rock powder sample to be tested; S25. Cover the crucible with a lid and perform pyrolysis treatment on the rock powder sample to be tested.
10. The method for using a crucible lining according to claim 9, characterized in that: The crucible is a nickel-based crucible.