Artificially synthesized pyrophyllite and synthesis process thereof

Abstract

The synthetic pyrophyllite comprises the following components in parts by mass: 20-40 parts of silicon dioxide, 50-60 parts of aluminum oxide, 5-6 parts of a collecting agent and 13-18 parts of a regulator, the regulator comprises 1-4 parts of wollastonite powder, 2-5 parts of hematite and 6-8 parts of water glass, and the collecting agent comprises mixed amine and linoleic acid. The pyrophyllite is formed by directly adopting the silicon dioxide and the aluminum oxide at high temperature and high pressure, pyrophyllite with different requirements can be produced according to requirements while the purity of the pyrophyllite is guaranteed, the collecting agent and the conditioning agent are added into the pyrophyllite, and the collecting agent and the conditioning agent are added into the pyrophyllite. According to the preparation method, pyrophyllite can be effectively promoted to be generated in the reaction process, the yield is increased, the cost is reduced, in the preparation process, a roasting mode of low temperature and then high temperature is adopted, the roasting temperature is effectively controlled, and meanwhile the synthesis stability of the pyrophyllite block is effectively improved.

Description

Technical Field

[0001] The present invention relates to the technical field of diamond synthesis, and more specifically, to an artificially synthesized pyrophyllite and a synthesis process thereof. Background Art

[0002] Pyrophyllite has the characteristics of fine texture, soft and smooth, good mechanical processing performance, white powder, high oil absorption rate, good covering rate, etc. Pyrophyllite can be used to produce refractory materials, ceramics, fillers, coatings, pesticides, and is also used as fillers and carriers for rubber products, cosmetics, pesticides, etc. It has a wide range of uses. The existing pyrophyllite is mainly obtained by processing the existing pyrophyllite ore. Diamond is mainly used to make various diamond tools. Diamond is mainly pressurized by the pressure medium during the synthesis process. Since the synthesis is carried out under high temperature and high pressure, the pressure medium is required to be very high. At present, the synthesis process of diamond mainly uses pyrophyllite as a sealing pressure medium. Since natural pyrophyllite contains a large number of other impurities, it cannot meet the performance requirements of the pressure medium for synthetic diamond synthesis, resulting in the existing natural pyrophyllite that meets the pressure medium for synthetic diamond synthesis is relatively scarce. For this reason, we propose an artificial synthetic pyrophyllite and its synthesis process. Summary of the invention

[0003] The purpose of the present invention is to solve the shortcomings of the prior art and to propose an artificially synthesized pyrophyllite and a synthesis process thereof.

[0004] To achieve the above object, the present invention provides the following technical solution: an artificial synthetic pyrophyllite, comprising the following components in parts by weight:

[0005] 20-40 parts of silicon dioxide, 50-60 parts of aluminum oxide, 5-6 parts of collector, and 13-18 parts of regulator.

[0006] Preferably, the regulator includes 1 to 4 parts of wollastonite powder, 2 to 5 parts of hematite, and 6 to 8 parts of water glass.

[0007] Preferably, the composition comprises the following components in proportion by weight: the collector comprises mixed amine and linoleic acid, and the weight ratio of the mixed amine to the linoleic acid is 3:1.

[0008] Preferably, the composition comprises the following components in parts by mass: 20 parts of silicon dioxide, 50 parts of aluminum oxide, 5 parts of collector, and 13 parts of regulator.

[0009] Preferably, the composition includes the following components in parts by mass: 30 parts of silicon dioxide, 55 parts of aluminum oxide, 5.5 parts of collector, and 16 parts of regulator.

[0010] Preferably, the composition includes the following components in parts by mass: 40 parts of silicon dioxide, 60 parts of aluminum oxide, 6 parts of collector, and 18 parts of regulator.

[0011] A synthetic process for artificially synthesizing pyrophyllite comprises the following steps:

[0012] S1, preparing a conditioning agent; weighing wollastonite powder, hematite and water glass in proportion, crushing the hematite to 1000 mesh to obtain hematite powder, placing the weighed wollastonite powder and hematite powder in a mixer, mixing for 10 minutes, then adding water glass, and continuing to mix until uniform to obtain a conditioning agent;

[0013] S2. Prepare collector: select 10-20% of mixed amine and 10-20% of linoleic acid by mass concentration, and put them into containers for standby use;

[0014] S3, mixed material: weigh 2000 mesh silicon dioxide and 2000 mesh aluminum oxide in proportion, divide them into two parts, put one part of silicon dioxide and aluminum oxide into a mixer, then add one third of the regulator, mix for 20 minutes, take out to obtain material group A, put the remaining silicon dioxide, aluminum oxide and two thirds of the regulator into a mixer, mix for 35 minutes, take out to obtain material group B, add a collector to material group A and material group B, stir evenly, and obtain a mixed material;

[0015] S4, aging: putting the mixed material into a high-pressure aging device, aging for 31 to 37 hours, the aging temperature is 700° C. After the aging is completed, taking it out and pressing it into pyrophyllite embryos according to demand, and drying the pyrophyllite embryos;

[0016] S5, roasting: the dried phyllite embryo is placed in a roasting furnace, the low-temperature roasting temperature is 250°C to 310°C, the roasting time is 3 hours, and then high-temperature roasting is performed, the temperature is raised to 700°C to 900°C, and after heat preservation and curing for 4 hours, the temperature is cooled to room temperature to obtain a phyllite block;

[0017] S6, drying: putting the calcined pyrophyllite block into a microwave drying device, and performing continuous drying treatment using microwaves. When the moisture content of the pyrophyllite is 1.8% to 4.5%, the drying is stopped.

[0018] Preferably, in step S6, during the drying process, a dehumidifier is used to discharge moisture in the microwave drying to speed up the drying process.

[0019] Technical effects and advantages of the present invention:

[0020] 1. The pyrophyllite of the present invention is synthesized directly by using silicon dioxide and aluminum oxide under high temperature and high pressure, which ensures the purity of the pyrophyllite and can produce pyrophyllite of different needs according to demand, reduces impurities, and adds collectors and regulators to effectively promote the formation of pyrophyllite during the reaction process, improve output and reduce costs.

[0021] 2. In the process of synthesizing phyllite, the present invention adopts a low-temperature followed by a high-temperature roasting method, which effectively controls the roasting temperature and effectively improves the synthetic stability of the phyllite block. Long-term high-temperature roasting can effectively improve the pressure transmission of the phyllite block. Dehumidification is performed while drying in the preparation process, which can effectively speed up the drying efficiency. DETAILED DESCRIPTION

[0022] In order to make the purpose, technical scheme and advantages of the present invention clearer, the present invention is further described in detail below in conjunction with specific embodiments. It should be understood that the specific embodiments described herein are only used to explain the present invention and are not intended to limit the present invention. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative work are within the scope of protection of the present invention.

[0023] Example 1

[0024] 20 parts of silicon dioxide, 50 parts of aluminum oxide, 5 parts of collector, and 13 parts of regulator.

[0025] Preparation method:

[0026] S1, prepare a conditioning agent; weigh 1 part of wollastonite powder, 2 parts of hematite and 6 parts of water glass in proportion, crush the hematite to 1000 mesh to obtain hematite powder, put the weighed wollastonite powder and hematite powder into a mixer, mix for 10 minutes, then add water glass, continue mixing until uniform, and obtain a conditioning agent;

[0027] S2. Prepare a collector: select a mixed amine with a mass concentration of 10-20% and a linoleic acid with a mass concentration of 10-20%, and put them into containers for standby use, wherein the weight ratio of the mixed amine to the linoleic acid is 3:1;

[0028] S3, mixed material: weigh silicon dioxide and aluminum oxide in proportion, select 2000 mesh for both silicon dioxide and aluminum oxide, divide them into two parts, put one part of silicon dioxide and aluminum oxide into a mixer, then add one-third of the regulator, mix for 20 minutes, take out to obtain material group A, put the remaining silicon dioxide, aluminum oxide and two-thirds of the regulator into a mixer, mix for 35 minutes, take out to obtain material group B, add a collector to material group A and material group B, stir evenly, and obtain a mixed material;

[0029] S4, aging: putting the mixed material into a high-pressure aging device for aging for 31 to 37 hours at a aging temperature of 1000 to 1400° C. and an air pressure of 400 to 500 MPa. After aging, taking out the mixed material and pressing it into pyrophyllite embryos according to demand, and drying the pyrophyllite embryos;

[0030] S5, roasting: the dried phyllite embryo is placed in a roasting furnace, the low-temperature roasting temperature is 250°C to 310°C, the roasting time is 3 hours, and then high-temperature roasting is performed, the temperature is raised to 700°C to 900°C, and after heat preservation and curing for 4 hours, the temperature is cooled to room temperature to obtain a phyllite block;

[0031] S6, drying: the calcined pyrophyllite blocks are placed in a microwave drying device, and continuously dried using microwaves. A dehumidifier is used to discharge moisture in the microwave drying process to speed up the drying process. When the moisture content of the pyrophyllite is 1.8% to 4.5%, the drying process is stopped.

[0032] Example 2

[0033] 30 parts of silicon dioxide, 55 parts of aluminum oxide, 5.5 parts of collector, and 16 parts of regulator.

[0034] Preparation method:

[0035] S1, prepare a conditioning agent; weigh 2 parts of wollastonite powder, 3 parts of hematite and 6 parts of water glass in proportion, crush the hematite to 1000 mesh to obtain hematite powder, put the weighed wollastonite powder and hematite powder into a mixer, mix for 10 minutes, then add water glass, continue mixing until uniform, and obtain a conditioning agent;

[0036] S2. Prepare a collector: select a mixed amine with a mass concentration of 10-20% and a linoleic acid with a mass concentration of 10-20%, and put them into containers for standby use, wherein the weight ratio of the mixed amine to the linoleic acid is 3:1;

[0037] S3, mixed material: weigh silicon dioxide and aluminum oxide in proportion, select 2000 mesh for both silicon dioxide and aluminum oxide, divide them into two parts, put one part of silicon dioxide and aluminum oxide into a mixer, then add one-third of the regulator, mix for 20 minutes, take out to obtain material group A, put the remaining silicon dioxide, aluminum oxide and two-thirds of the regulator into a mixer, mix for 35 minutes, take out to obtain material group B, add a collector to material group A and material group B, stir evenly, and obtain a mixed material;

[0038] S4, aging: putting the mixed material into a high-pressure aging device for aging for 31 to 37 hours at a aging temperature of 1000 to 1400° C. and an air pressure of 400 to 500 MPa. After aging, taking out the mixed material and pressing it into pyrophyllite embryos according to demand, and drying the pyrophyllite embryos;

[0039] S5, roasting: the dried phyllite embryo is placed in a roasting furnace, the low-temperature roasting temperature is 250°C to 310°C, the roasting time is 3 hours, and then high-temperature roasting is performed, the temperature is raised to 700°C to 900°C, and after heat preservation and curing for 4 hours, the temperature is cooled to room temperature to obtain a phyllite block;

[0040] S6, drying: the calcined pyrophyllite blocks are placed in a microwave drying device, and continuously dried using microwaves. A dehumidifier is used to discharge moisture in the microwave drying process to speed up the drying process. When the moisture content of the pyrophyllite is 1.8% to 4.5%, the drying process is stopped.

[0041] Example 3

[0042] 40 parts of silicon dioxide, 60 parts of aluminum oxide, 6 parts of collector, and 18 parts of regulator. Preparation method:

[0043] S1, prepare a conditioning agent; weigh 3 parts of wollastonite powder, 4 parts of hematite and 7 parts of water glass in proportion, crush the hematite to 1000 mesh to obtain hematite powder, put the weighed wollastonite powder and hematite powder into a mixer, mix for 10 minutes, then add water glass, continue mixing until uniform, and obtain a conditioning agent;

[0044] S2. Prepare a collector: select a mixed amine with a mass concentration of 10-20% and a linoleic acid with a mass concentration of 10-20%, and put them into containers for standby use, wherein the weight ratio of the mixed amine to the linoleic acid is 3:1;

[0045] S3, mixed material: weigh silicon dioxide and aluminum oxide in proportion, select 2000 mesh for both silicon dioxide and aluminum oxide, divide them into two parts, put one part of silicon dioxide and aluminum oxide into a mixer, then add one-third of the regulator, mix for 20 minutes, take out to obtain material group A, put the remaining silicon dioxide, aluminum oxide and two-thirds of the regulator into a mixer, mix for 35 minutes, take out to obtain material group B, add a collector to material group A and material group B, stir evenly, and obtain a mixed material;

[0046] S4, aging: putting the mixed material into a high-pressure aging device for aging for 31 to 37 hours at a aging temperature of 1000 to 1400° C. and an air pressure of 400 to 500 MPa. After aging, taking out the mixed material and pressing it into pyrophyllite embryos according to demand, and drying the pyrophyllite embryos;

[0047] S5, roasting: the dried phyllite embryo is placed in a roasting furnace, the low-temperature roasting temperature is 250°C to 310°C, the roasting time is 3 hours, and then high-temperature roasting is performed, the temperature is raised to 700°C to 900°C, and after heat preservation and curing for 4 hours, the temperature is cooled to room temperature to obtain a phyllite block;

[0048] S6, drying: the calcined pyrophyllite blocks are placed in a microwave drying device, and continuously dried using microwaves. A dehumidifier is used to discharge moisture in the microwave drying process to speed up the drying process. When the moisture content of the pyrophyllite is 1.8% to 4.5%, the drying process is stopped.

[0049] Example 4

[0050] 35 parts of silicon dioxide, 55 parts of aluminum oxide, 5 parts of collector, and 13 parts of regulator.

[0051] Preparation method:

[0052] S1, prepare a conditioning agent; weigh 4 parts of wollastonite powder, 5 parts of hematite and 8 parts of water glass in proportion, crush the hematite to 1000 mesh to obtain hematite powder, put the weighed wollastonite powder and hematite powder into a mixer, mix for 10 minutes, then add water glass, continue mixing until uniform, and obtain a conditioning agent;

[0053] S2. Prepare a collector: select 10-20% of a mixed amine and 10-20% of linoleic acid by mass concentration, and put them into containers for standby use, wherein the weight ratio of the mixed amine to the linoleic acid is 3:1;

[0054] S3, mixed material: weigh silicon dioxide and aluminum oxide in proportion, select 2000 mesh for both silicon dioxide and aluminum oxide, divide them into two parts, put one part of silicon dioxide and aluminum oxide into a mixer, then add one-third of the regulator, mix for 20 minutes, take out to obtain material group A, put the remaining silicon dioxide, aluminum oxide and two-thirds of the regulator into a mixer, mix for 35 minutes, take out to obtain material group B, add a collector to material group A and material group B, stir evenly, and obtain a mixed material;

[0055] S4, aging: putting the mixed material into a high-pressure aging device for aging for 31 to 37 hours at a aging temperature of 1000 to 1400° C. and an air pressure of 400 to 500 MPa. After aging, taking out the mixed material and pressing it into pyrophyllite embryos according to demand, and drying the pyrophyllite embryos;

[0056] S5, roasting: the dried phyllite embryo is placed in a roasting furnace, the low-temperature roasting temperature is 250°C to 310°C, the roasting time is 3 hours, and then high-temperature roasting is performed, the temperature is raised to 700°C to 900°C, and after heat preservation and curing for 4 hours, the temperature is cooled to room temperature to obtain a phyllite block;

[0057] S6, drying: the calcined pyrophyllite blocks are placed in a microwave drying device, and continuously dried using microwaves. A dehumidifier is used to discharge moisture in the microwave drying process to speed up the drying process. When the moisture content of the pyrophyllite is 1.8% to 4.5%, the drying process is stopped.

[0058] Control group 1

[0059] S1. Synthetic phyllite block: 4 parts of barite powder and 3 parts of calcite powder are selected and mixed evenly to obtain an auxiliary additive, 40 parts of phyllite powder are selected in proportion and placed in a mixer, and then 15% of the auxiliary additive is added, and then water glass is added and mixed until uniform to obtain a mixture; the remaining 40 parts of phyllite powder are added to the mixture twice, and each time mixing is for 15 to 20 minutes to obtain a phyllite block mixture; the weighed mixture is placed in a phyllite block mold, and the phyllite blocks are pressed by a four-column hydraulic press, and finally the phyllite blocks are placed in a roasting device, the roasting temperature is 200°C to 380°C, and the roasting time is 3 to 4 hours. After the roasting is completed, the temperature is naturally lowered to obtain the final product.

[0060] The products obtained in Examples 1, 2, 3, 4 and Control Group 1 were subjected to pressure transmission coefficient performance test and compressive strength test, and diamonds were prepared from the products obtained in Examples 1, 2, 3, 4 and Control Group 1 and the diamond synthesis gauge pressure (MPa) was tested to obtain the following table:

[0061]

[0062]

[0063] It can be seen from the above table that the pyrophyllite prepared by the present invention has good compressive strength and pressure transmission coefficient, which fully meets the performance requirements of the pressure transmission medium for synthetic diamond. At the same time, when the pyrophyllite prepared by the present invention is used to process artificial diamond, it has a good synthetic surface pressure.

[0064] The products obtained in Examples 1, 2, 3, 4 and Control Group 1 were tested for ingredients, and the following table was obtained:

[0065] Example 1 Example 2 Example 3 Example 4 Control group 1 <![CDATA[Al2O3]]> 28.21 27.91 26.86 27.83 35.95 <![CDATA[SiO2]]> 66.43 65.78 67.98 66.35 54.28 <![CDATA[Fe2O3]]> 0.41 0.32 0.24 0.33 0.84 <![CDATA[H2O]]> 4.21 4.01 3.95 3.78 3.32

[0066] Finally, it should be noted that the above is only a preferred embodiment of the present invention and is not intended to limit the present invention. Although the present invention has been described in detail with reference to the aforementioned embodiments, it is still possible for those skilled in the art to modify the technical solutions described in the aforementioned embodiments or to make equivalent substitutions for some of the technical features therein. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the protection scope of the present invention.

Claims

1. An artificially synthesized pyrophyllite, Features: The composition includes the following components in parts by weight: 20-40 parts of silicon dioxide, 50-60 parts of aluminum oxide, 5-6 parts of collector, and 13-18 parts of regulator.

2. The synthetic pyrophyllite according to claim 1, Features: The regulator includes 1-4 parts of wollastonite powder, 2-5 parts of hematite, and 6-8 parts of water glass.

3. The artificial synthetic pyrophyllite according to claim 1, Features: It includes the following components in weight ratio: the collector includes mixed amine and linoleic acid, and the weight ratio of the mixed amine to the linoleic acid is 3:

1.

4. The artificial synthetic pyrophyllite according to claim 1, Features: The invention comprises the following components in parts by mass: the invention comprises the following components in parts by mass: 20 parts of silicon dioxide, 50 parts of aluminum oxide, 5 parts of collector and 13 parts of regulator.

5. The artificial synthetic pyrophyllite according to claim 1, Features: The composition comprises the following components in parts by weight: 30 parts of silicon dioxide, 55 parts of aluminum oxide, 5.5 parts of collector, and 16 parts of regulator.

6. The artificial synthetic pyrophyllite according to claim 1, Features: The composition comprises the following components in parts by weight: 40 parts of silicon dioxide, 60 parts of aluminum oxide, 6 parts of collector, and 18 parts of regulator.

7. A process for synthesizing artificial pyrophyllite according to any one of claims 1 to 6, It is characterized in that The steps include: S1, preparing a conditioning agent; weighing wollastonite powder, hematite and water glass in proportion, crushing the hematite to 1000 mesh to obtain hematite powder, placing the weighed wollastonite powder and hematite powder in a mixer, mixing for 10 minutes, then adding water glass, and continuing to mix until uniform to obtain a conditioning agent; S2. Prepare collector: select 10-20% of mixed amine and 10-20% of linoleic acid by mass concentration, and put them into containers for standby use; S3, mixed material: weigh 2000 mesh silicon dioxide and 2000 mesh aluminum oxide in proportion, divide them into two parts, put one part of silicon dioxide and aluminum oxide into a mixer, then add one third of the regulator, mix for 20 minutes, take out to obtain material group A, put the remaining silicon dioxide, aluminum oxide and two thirds of the regulator into a mixer, mix for 35 minutes, take out to obtain material group B, add a collector to material group A and material group B, stir evenly, and obtain a mixed material; S4, aging: putting the mixed material into a high-pressure aging device, aging for 31 to 37 hours at a aging temperature of 700° C., taking it out after aging, pressing it into pyrophyllite embryos according to demand, and drying the pyrophyllite embryos; S5, roasting: the dried phyllite embryo is placed in a roasting furnace, the low-temperature roasting temperature is 250°C to 310°C, the roasting time is 3 hours, and then high-temperature roasting is performed, the temperature is raised to 700°C to 900°C, and after heat preservation and curing for 4 hours, the temperature is cooled to room temperature to obtain a phyllite block; S6, drying: putting the calcined pyrophyllite block into a microwave drying device, and performing continuous drying treatment using microwaves. When the moisture content of the pyrophyllite is 1.8% to 4.5%, the drying is stopped.

8. A synthetic process for artificially synthesizing pyrophyllite according to claim 7, Features: In step S6, during the drying process, a dehumidifier is used to discharge moisture in the microwave drying.

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