AU2021342988B2 - Illite, preparation method therefor and use thereof - Google Patents
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- 229910052900 illite Inorganic materials 0.000 title claims abstract description 228
- VGIBGUSAECPPNB-UHFFFAOYSA-L nonaaluminum;magnesium;tripotassium;1,3-dioxido-2,4,5-trioxa-1,3-disilabicyclo[1.1.1]pentane;iron(2+);oxygen(2-);fluoride;hydroxide Chemical compound [OH-].[O-2].[O-2].[O-2].[O-2].[O-2].[F-].[Mg+2].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[K+].[K+].[K+].[Fe+2].O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2 VGIBGUSAECPPNB-UHFFFAOYSA-L 0.000 title claims abstract description 228
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 239000000725 suspension Substances 0.000 claims abstract description 80
- 238000004062 sedimentation Methods 0.000 claims abstract description 62
- 239000000843 powder Substances 0.000 claims abstract description 53
- 238000000926 separation method Methods 0.000 claims abstract description 53
- 238000000034 method Methods 0.000 claims abstract description 45
- 238000000265 homogenisation Methods 0.000 claims abstract description 34
- 238000000498 ball milling Methods 0.000 claims abstract description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 239000007788 liquid Substances 0.000 claims description 84
- 238000013519 translation Methods 0.000 claims description 26
- 238000000227 grinding Methods 0.000 claims description 19
- 239000002245 particle Substances 0.000 abstract description 59
- 238000009826 distribution Methods 0.000 abstract description 20
- 238000001179 sorption measurement Methods 0.000 abstract description 13
- 239000012141 concentrate Substances 0.000 abstract 1
- 239000000047 product Substances 0.000 description 29
- 239000000463 material Substances 0.000 description 22
- 239000012535 impurity Substances 0.000 description 17
- 238000000746 purification Methods 0.000 description 12
- 230000008569 process Effects 0.000 description 11
- 238000005265 energy consumption Methods 0.000 description 7
- 238000001704 evaporation Methods 0.000 description 6
- 230000008020 evaporation Effects 0.000 description 6
- 239000006228 supernatant Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 238000001694 spray drying Methods 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 230000003247 decreasing effect Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 230000005484 gravity Effects 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 239000013049 sediment Substances 0.000 description 4
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 3
- 238000004364 calculation method Methods 0.000 description 3
- 239000002734 clay mineral Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 239000011591 potassium Substances 0.000 description 3
- 229910052700 potassium Inorganic materials 0.000 description 3
- 239000002893 slag Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 239000005995 Aluminium silicate Substances 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 235000012211 aluminium silicate Nutrition 0.000 description 2
- 239000002537 cosmetic Substances 0.000 description 2
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000004576 sand Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000009827 uniform distribution Methods 0.000 description 2
- 238000005299 abrasion Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 229910000323 aluminium silicate Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004061 bleaching Methods 0.000 description 1
- 239000000872 buffer Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000005188 flotation Methods 0.000 description 1
- 230000003116 impacting effect Effects 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 238000007885 magnetic separation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 239000010445 mica Substances 0.000 description 1
- 229910052618 mica group Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/36—Silicates having base-exchange properties but not having molecular sieve properties
- C01B33/38—Layered base-exchange silicates, e.g. clays, micas or alkali metal silicates of kenyaite or magadiite type
- C01B33/40—Clays
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
- A61K8/26—Aluminium; Compounds thereof
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/10—General cosmetic use
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Birds (AREA)
- Dispersion Chemistry (AREA)
- Epidemiology (AREA)
- Dermatology (AREA)
- Disintegrating Or Milling (AREA)
- Nitrogen And Oxygen Or Sulfur-Condensed Heterocyclic Ring Systems (AREA)
Abstract
Illite, a preparation method therefor and use thereof. The preparation method comprises: mixing illite raw ore powder with water, performing ball milling, and performing cyclone separation, so as to obtain a primary suspension; then performing primary sedimentation on the primary suspension, and performing separation, so as to obtain a secondary suspension; and crushing the secondary suspension by using a high-pressure homogenization method, then performing secondary sedimentation, and performing separation, so as to obtain illite. The preparation method can increase the purity of illite, enable the particle size to be small and concentrate the particle size distribution; and when the prepared illite is applied to preparation of a skin care product, the skin feeling and adsorption performance of the skin care product can be improved.
Description
English Translation of PCT/CN2021/082384
[0001] The present application relates to the technical field of preparation of raw materials for cosmetics and skin care products, in particular to a method for preparing illite and an application of the illite.
[0002] Illite is a potassium-containing aluminosilicate mica clay mineral, which is first discovered on the island of Erie in the United States. Illite is also called "hydromuscovite". The chemical composition of illite is mainly K20, A12 0 3 and SiO2 . Illite has low hardness and is unable to expand; besides, illite has the characteristics of having rich potassium and high aluminum content, being smooth, soft, heat-resistant, having high oil absorption rate, low ultraviolet ray transmittance, good rheological property, high whiteness, good abrasion resistance and acid and alkali resistance, and is widely used in the fields of potassium fertilizer preparation, pigments for papermaking, sanitary ceramics, water-retaining functional materials, cosmetics and rubber and plastic fillers. With the continuous in-depth research on the application of illite, illite has increasingly become an important functional material with multiple uses. The purity and particle size of illite directly affect the quality and function of the illite, thereby affecting its application field. Therefore, the purification and processing of illite is an important process for developing and utilizing illite.
[0003] At present, there is no mature process for the purification of illite at home and abroad, the illite raw ore is simply purified by referring to the purification methods of other clay minerals, for example, high gradient magnetic separation, acid leaching method, roasting method, dry gravity chromatography separation, thermal flotation beneficiation and chemical bleaching method are used to purify the illite raw ore. However, when illite is purified by these commonly used purification methods of clay minerals, there are often problems such as complicated purification process, low purity of illite products and secondary pollution, and the
English Translation of PCT/CN2021/082384
control of particle size of the illite is rarely involved.
[0004] Therefore, a method of preparing illite with high purity and concentrated particle size distribution is to be provided.
[0005] Based on this, a method for preparing high-quality illite is provided according to the present application, which can improve the purity of illite, make the particle size small and the particle size distribution concentrated.
[0006] The following technical solutions are provided according to the present application.
[0007] According to an aspect of the present application, a method for preparing illite is provided, comprising the following steps:
mixing illite raw ore powder with water, performing ball milling, and performing cyclone separation, to obtain a primary suspension liquid;
performing primary sedimentation to the primary suspension liquid, and performing separation, to obtain a secondary suspension liquid; and
crushing the secondary suspension liquid by using a high pressure homogenization method, then performing secondary sedimentation, and performing separation, to obtain the illite.
[0008] In some embodiments, a pressure is 100 Bar to 300 Bar when the secondary suspension liquid is crushed by using the high pressure homogenization method.
[0009] In some embodiments, a pressure is 200 Bar to 300 Bar when the secondary suspension liquid is crushed by using the high pressure homogenization method.
[0010] In some embodiments, a time of the primary sedimentation is 0.5d to 3d; and/or a time of the secondary sedimentation is l d to 7d.
[0011] In some embodiments, a feed-in flow rate of the cyclone separation step is 10 m3 /h to 20 m3 /h.
[0012] In some embodiments, based on a total mass of the illite raw ore powder and the water,
English Translation of PCT/CN2021/082384
a mass percentage of the illite raw ore powder is 50% to 90%.
[0013] In some embodiments, a time of the primary sedimentation is Id to 3d.
[0014] According to another aspect of the present application, illite prepared by any of the above preparation methods is provided.
[0015] An application of the above illite in preparing a skin care product is further provided according to the present application.
[0016] A mud mask including the above illite is further provided according to present application.
Beneficial effect
[0017] In the above method of preparing high-quality illite, the illite raw ore powder is first mixed with water and then ball milling is performed. In the process of ball milling, the illite raw ore powder is crushed to obtain illite with a smaller particle size. Then, impurities such as gravel and slag carried in the illite raw ore powder are separated by cyclone separation, so as to obtain a primary suspension liquid. And then, the primary suspension liquid is subjected to primary sedimentation, the impurities in the primary suspension liquid gradually sediment, while the illite hydromica, that is, pure illite, is still suspended in the upper-layer liquid, thus the impurities can be separated, and the secondary suspension liquid containing illite with relatively higher purity can be obtained. Further, the secondary suspension liquid is crushed by the high pressure homogenization method to obtain illite with a finer particle size and more concentrated distribution of particle size, and further secondary sedimentation is performed, so that the illite can be further purified to obtain high-purity illite.
[0018] The illite prepared by the above high-quality illite preparation method has high purity, small particle size and uniform distribution of particle size, which improves the appearance, skin feel, adsorption performance and other properties of illite. Further, when the prepared illite is applied in the preparation of the skin care product, the skin feel and adsorption performance of the skin care product can be improved.
[0019] A mud mask is further provided according to the present application, which includes the above illite. The illite obtained by the above preparation method has high purity, small
English Translation of PCT/CN2021/082384
particle size and uniform distribution of particle size, so that the prepared mud mask has good skin feel and adsorption performance.
[0020] Figure 1 is a graph showing ore grinding efficiencies under different solid content of material according to a first embodiment;
[0021] Figure 2 is a graph showing the purity of illite prepared under different time of primary sedimentation according to a third embodiment;
[0022] Figure 3 is a graph showing particle size distribution of illite obtained when a pressure of high pressure homogenization treatment is 200 Bar according to a forth embodiment; and
[0023] Figure 4 is a graph showing the purity of illite prepared under different time of secondary sedimentation according to a fifth embodiment.
[0024] In order to facilitate understanding of the present application, the present application will be described more fully below, and preferred embodiments of the present application will be given. However, the present application may be embodied in many different forms and is not limited to the embodiments described herein. Instead, these embodiments are provided so that the present disclosure can be more thoroughly and completely understood.
[0025] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by those skill in the art to which this application belongs. The terms used herein in the description of the present application are only for the purpose of describing specific embodiments, which are not intended to limit the present application. The term "and/or" used herein includes any and all combinations of one or more of the associated listed items.
[0026] The purity of illite has always been an important factor in considering the quality of illite, because the purity of illite not only affects its quality and appearance, but also affects its
English Translation of PCT/CN2021/082384
application field and usage range. In the conventional technology, the purity of illite obtained by the illite purification process which have been reported is mostly between 70% and 80%, and there are few methods for obtaining high-purity illite, especially the purification method for obtaining illite with the purity greater than 90%.
[0027] Moreover, the focus of the illite purification process in the conventional technology is to improve the purity, extraction rate and utilization rate of illite, and there are few reports on the research of the particle size of illite. It is precisely because the quality of illite obtained in the conventional technology is not high enough, the application field of illite is greatly limited. For example, in the field of skin care products, especially in mud masks, kaolin is mostly used as a substitute for mud, while illite is only used as an auxiliary conceptual additive. This is mainly because the purity and quality of illite itself is not high, which does not have obvious advantages compared with kaolin.
[0028] Based on this, in this application, in consideration of the structural characteristics of illite, the technical staff make the illite hydromica in the illite raw ore more fully dissolved in the water by using the multi-stage crushing process, and then separate the illite hydromica from the impurity ore by using the suspension characteristics of the illite hydromica and the effect of gravity sedimentation, so as to obtain illite with high purity and good quality.
[0029] In addition, it is found by further research on the properties of illite that the particle size of illite can not only change the skin feel and appearance of skin care products, but also affect their adsorption performances. After a large amount of experimental research, the technical staff of the present application creatively adopted the high pressure homogenization process to crush the illite to make the particle size finer and more uniformly distributed, and further performed purification to illite, so as to obtain illite with high purity, small particle size and uniform particle size distribution, which improves the skin feel, appearance and adsorption performance of the skin care products when being applied to the preparation of skin care products.
[0030] A method of preparing illite is provided according to an embodiment of the present application, which includes the following steps S10 to S30.
English Translation of PCT/CN2021/082384
[0031] Step S10, mixing illite raw ore powder with water, performing ball milling, and performing cyclone separation, to obtain a primary suspension liquid.
[0032] The illite raw ore powder is mixed with the water and then ball milling is performed. During the ball milling process, the illite raw ore powder is crushed to obtain illite with a smaller particle size. Then, the impurities such as gravel and slag are separated by the cyclone separation, so as to obtain the primary suspension liquid.
[0033] In some embodiments, in step S10, a mass percentage of the illite raw ore powder is 50% to 90% based on a total mass of the illite raw ore powder and the water.
[0034] In some the embodiments, instep S10, the time of the ball milling step is 4h to 12h.
[0035] The mass percentage of the illite raw ore powder affects the grinding concentration of the material in the ball milling step, and the mass percentage of the illite raw ore powder refers to the mass percentage of the solid material contained in the material during the ball milling step. It not only affects the production capacity and energy consumption of the mill, but also affects the quality of the products obtained by ball milling, thereby affecting the purification effect of illite.
[0036] The grinding efficiency of the ball mill refers to a ratio between productivity of the mill and energy consumption of the mill. The specific calculation is shown in formulas (1), (2) and (3):
q=m/Vt (1); W=Pt=UIt (2); q=q/W (3)
[0037] In formula (1), q represents the productivity of the mill, m represents an output of ore, unit: ton; V represents an effective volume of a barrel of the mill, unit: m3 ; t represents working time of the mill, unit: h.
[0038] In formula (2), W represents the energy consumption of the mill, P represents a power of the ball mill, the unit is kW; U represents the voltage, unit: V; I represents the current, unit: A.
[0039] In formula (3), q represents the grinding efficiency, q represents the productivity of the mill, and W represents the energy consumption of the mill, unit: kW.
English Translation of PCT/CN2021/082384
[0040] Based on the total mass of the illite raw ore powder and the water, the mass percentage of the illite raw ore powder is 50% to 90%. The productivity of the ball milling is high, the grinding efficiency is high, and the illite products obtained by ball milling are of good quality.
[0041] In some embodiments, the ball milling step in step S10 is performed by using a wet ball mill.
[0042] Preferably, based on the total mass of the illite raw ore powder and the water, the mass percentage of the illite raw ore powder is 50% to 80%. Further preferably, the mass percentage of the illite raw ore powder is 70% to 80%.
[0043] In some embodiments, the feed-in flow rate in the cyclone separation step in step S10 is 10m3 /h to 20m/h.
[0044] Impurities such as gravel or slag mixed in the illite raw ore powder can be separated by the cyclone separation, so as to obtain relatively pure illite. It is found by the technical staff of the present application in further experiments that the feed-in flow rate in the cyclone separation step has a great influence on the separation and purification efficiency of the illite raw ore powder.
[0045] When other process conditions remain unchanged, with the increase of the feed-in flow rate, the separation efficiency of the cyclone separation step shows a trend offirstly increasing significantly and then increasing slowly. Specifically, when the inlet flow rate increased from 10m 3/h to 15m 3/h, the separation efficiency increased from 36.61% to about 76.53%; and when the inlet flow rate continued to increase from 15m 3/h to 20m 3/h, the separation efficiency slowly increased to around 82.4%. Preferably, the feed-in flow rate in the cyclone separation step in step S10 is 15m 3/h to 20m 3/h.
[0046] In some embodiments, the cyclone separation step in step S10 is performed by a cyclone separator. Further, the technical staff in the present application have found that, with the increase of the feed-in flow rate, the energy consumption increases accordingly, and a pressure difference in the cyclone separator is also increased, which will increase the cost and the equipment loss. Further preferably, the feed-in flow rate in the cyclone separation step in
English Translation of PCT/CN2021/082384
step S10 is 15m/h.
[0047] In step S20, the primary suspension liquid obtained in step S10 is subjected to primary sedimentation to obtain a secondary suspension liquid.
[0048] The primary suspension liquid is subjected to primary sedimentation, the impurities in the primary suspension liquid gradually sediment, and the illite hydromica in illite is still suspended in the upper-layer liquid, so that illite can be further purified.
[0049] In some embodiments, the time of the primary sedimentation instep S20 is Id to 3d.
[0050] The purity of illite refers to the content of illite hydromica in illite, and the illite hydromica has a suspension characteristic. In the primary sedimentation, the illite hydromica with the suspension characteristic is still suspended in the water, while the impurity ore slowly sediments due to the action of gravity.
[0051] When the other process conditions were kept unchanged, and the time of the primary sedimentation was changed for experimental exploration, the results showed that, in the case that the time of the primary sedimentation was l d to 3d, the impurity ore gradually sedimented due to the action of gravity, thereby increasing the content of the illite hydromica in illite, that is, the purity of illite is improved. Further, in the case that the time of the primary sedimentation is more than 3d, some illite hydromica with relatively larger particle size in the primary suspension liquid also sedimented, which will reduce the content of the illite hydromica and the productivity of illite. Preferably, the time of the primary sedimentation is Id to 3d.
[0052] In some embodiments, in step S20, negative-pressure suction is employed in the separation step to suck up the upper-layer liquid, to obtain a secondary suspension liquid.
[0053] In step S30, the secondary suspension liquid obtained in step S20 is crushed by using a high pressure homogenization method, and then secondary sedimentation is performed, to obtain illite by separation.
[0054] The secondary suspension liquid is crushed by the homogenization method to obtain illite with finer particle size and more concentrated distribution of particle size. It is found by the technical staff of the present application that, when the secondary suspension liquid is crushed by using the high pressure homogenization method, the pressure has a great influence
English Translation of PCT/CN2021/082384
on the particle size of illite, especially the distribution of particle size.
[0055] In some embodiments, the pressure is 100 Bar to 300 Bar when the secondary suspension liquid is crushed by using the high pressure homogenization method.
[0056] When the other process conditions were kept unchanged, as the pressure of the high pressure homogenization treatment increased from 100 Bar to 300 Bar, the average particle size of the prepared illite decreased from 401.35 nm to 332.64 nm, showing a decreasing trend with the increase of pressure. But when the pressure is 200 Bar, the average particle size of illite is 342.52 nm, indicating that when the pressure exceeds 200 Bar, the increase of pressure has relatively small effect on the decrease of the particle size. When the high pressure homogenization method is used to crush the secondary suspension liquid under a pressure of 100 Bar to 300 Bar, illite with relatively smaller particle size can be obtained.
[0057] In some embodiments, in step S30, the pressure is 200 Bar to 300 Bar when the secondary suspension liquid is crushed by using the high pressure homogenization method.
[0058] When the pressure is 200 Bar to 300 Bar as the high pressure homogenization method is used to crush the secondary suspension liquid, illite with relatively smaller particle size and more concentrated distribution of particle size can be obtained. Specifically, when the pressure is 200Bar as the high pressure homogenization method is used to crush the secondary suspension liquid, the particle size distribution range of the obtained illite is 198.55 nr to 434.81 nm, and the particle sizes are concentrated between 266.4 nm to 357.43 nm, and the distribution range is relatively concentrated.
[0059] In some embodiments, in step S30, when the high pressure homogenization method is used to crush the secondary suspension liquid, the number of times of homogenization is 1 to 3 times; specifically, the number of times of homogenization is 3 times.
[0060] Further, after the secondary suspension liquid is crushed by the high pressure homogenization method, the average particle size of the particles in the suspension is smaller. During the secondary sedimentation process, with the increase of the sedimentation time, the purity of illite shows a trend of gradual increase, the solid impurity particles can effectively sediment, and be effectively separated from the illite hydromica, which further improves the
English Translation of PCT/CN2021/082384
purity of illite.
[0061] In some embodiments, in step S30, the time of the secondary sedimentation is Id to 7d.
[0062] When the other process conditions were kept unchanged, the time of the secondary sedimentation was changed for experimental exploration. The results showed that, when the time of the secondary sedimentation was between Id and 3d, the purity of illite increased significantly, and as the sedimentation time continued to increase to 7d, the purity of illite basically no longer changed; and if the sedimentation time is too long, the suspended illite hydromica also sedimented, which led to decrease in the productivity of illite.
[0063] In some embodiments, in step S30, the time of the secondary sedimentation is I d to 6d. Preferably, the time of the secondary sedimentation is 2d to 5d.
[0064] In some embodiments, the above preparation method further includes step Si1 of crushing the illite raw ore to obtain the above illite raw ore powder. Specifically, in step SlI, the illite raw ore is subjected to primary crushing to obtain the illite raw ore powder. Specifically, primary crushing of the illite raw ore is performed by a jaw crusher to obtain the illite raw ore powder.
[0065] When the jaw crusher is used for primary crushing of the illite raw ore, a processing capacity of the jaw crusher is 1 t/h to 800 t/h, which may be selected according to the actual material amount.
[0066] Further, the ore with better appearance and quality is preferably selected from the illite raw ore, and impurities that are visible and obvious to the naked eye are removed.
[0067] In some embodiments, in step S30, after the secondary sedimentation step, a step of obtaining the illite by separation is further provided. Specifically, after the secondary sedimentation, a supernatant liquid in the suspension liquid is sucked out for evaporation treatment to evaporate excess water, so that the moisture content of the product is kept between 30% and 40%, and then the product is sterilized and then hermetically stored, to obtain high-purity illite.
[0068] Illite prepared by any of the above preparation methods is provided according to an
English Translation of PCT/CN2021/082384
embodiment of the present application.
[0069] According to the above method for preparing high-quality illite, the illite raw ore powder is successively crushed by ball milling and high pressure homogenization method, which can make the crushing of the illite raw ore more thorough, moreover, the illite hydromica in the ore can be more fully separated through two times of sedimentation, which improves the purity of illite while improving the utilization rate of illite hydromica. In addition, with the high pressure homogenization technology, not only the illite can be crushed more thoroughly, but also can the particle size of illite can be controlled, so that the particle size of the prepared finished product is smaller and the particle size distribution is more concentrated, thereby improving properties of the illite such as the appearance, skin feel and adsorption performance, so that the obtained illite has high purity, small particle size and uniform particle size distribution, which improves performances of the illite such as the appearance, skin feel and adsorption performance. Therefore, when the obtained illite with high purity, small and concentratedly distributed particle size is used in the preparation of skin care products, the skin feel and adsorption performance of the skin care products can be improved.
[0070] An application of the above illite in the preparation of skin care products is further provided according to an embodiment of the present application.
[0071] The illite prepared by the above preparation method has high purity, small and uniformly distributed particle size, so that the appearance, skin feel, adsorption performance and other properties of illite can be improved. Therefore, when the obtained illite with high purity, small and concentratedly distributed particle size is used in the preparation of skin care products, the skin feel and adsorption performance of the skin care products can be improved.
[0072] A mud mask including the above illite is further provided according to the present application.
[0073] The lower the impurity content, the higher the purity, the smaller the particle size and the narrower the particle size distribution of illite, the finer the skin feel of the illite, and the specific surface area and adsorption performance also increase, which can improve the skin feel and adsorption performance of the mud mask.
English Translation of PCT/CN2021/082384
[0074] Here, illite, the method of preparing the illite and the application of the illite are exemplified according to the present application, but the present application is not limited to the following examples.
[0075] 1) The ore with better appearance and quality was preferably selected from the illite raw ore, and impurities that are visible and obvious to the naked eye were removed. Then primary crushing was performed to the illite raw ore by a jaw crusher, to obtain illite raw ore powder.
[0076] 2) The illite raw ore powder obtained in step 1) was mixed with water to obtain a mixed material, which was subjected to ball milling by a wet ball mill for 8 hours. After the ball milling was completed, cyclone separation was performed to the mixed material by a cyclone separator, where the feed-in flow rate of the cyclone separation was 15 m 3/h, and a primary suspension liquid is obtained.
[0077] 3) The primary suspension liquid obtained in step 2) was subjected to primary sedimentation for 24 hours. The suspension liquid was layered, and the upper-layer liquid in the suspension liquid was sucked out by negative-pressure suction, that is, a secondary suspension liquid was obtained by separation.
[0078] 4) The secondary suspension liquid obtained in step 3) was placed in a high pressure homogenizer with a pressure of 200 Bar for high pressure homogenization cycle treatment for three times, then secondary sedimentation was performed for 72h, then the supernatant liquid in the suspension liquid was sucked out to be subjected to evaporation treatment, to evaporate excess water, so that the moisture content of the product was kept between 30% and 40%, and then the product was sterilized and hermetically stored, thus the high-purity illite is obtained.
[0079] 5) Three batches of illite were randomly sampled while being hermetically stored, and dry illite powder was obtained after spray-drying, and the purity of the dry illite powder of the sample was tested.
[0080] In the first embodiment, the influence of the solid content of the material on the
English Translation of PCT/CN2021/082384
efficiency of the ball milling in step 2) was explored. With the total mass of illite raw ore powder and water and other experimental conditions being kept unchanged and the mass of illite raw ore powder in step 2) being changed, the above steps were repeated, and the grinding efficiency of the ball mill was calculated according to the following formulas, the specific calculation is shown in formulas (1), (2) and (3):
q=m/Vt (1); W=Pt=UIt (2); q=q/W (3).
[0081] In formula (1), q represents the productivity of the mill, m represents the output of ore, unit: ton; V represents the effective volume in the barrel of the mill, unit: m3 ; t represents the working time of the mill, unit: h.
[0082] In formula (2), W represents the energy consumption of the mill, P represents the power of the ball mill, the unit is kW; U represents the voltage, unit: V; I represents the current, unit: A.
[0083] In formula (3), q represents the grinding efficiency, q represents the productivity of the mill, and W represents the energy consumption of the mill, unit: kW.
[0084] The specific results were shown in Figure 1, in which the ordinate represents the grinding efficiency, and the abscissa represents the grinding efficiency, that is, the mass percentage of the illite raw ore powder based on the total mass of the illite raw ore powder and the water. It can be seen from Figure 1 that as the grinding concentration increased from 0.5 to 0.8, the grinding efficiency increased from 61.5% to 65%, showing a rising trend with the increase of concentration; and when the concentration exceeded 0.8, the grinding efficiency declined instead. This may be because when the grinding concentration inside the mill is low, the ore pulp flows too fast in the barrel, which leads to low grinding efficiency. The increase of concentration of the ore pulp increases the chance of the steel balls impacting the ore material, which leads to increase of the grinding efficiency. When the concentration of the ore pulp exceeds 0.8, surfaces of the steel balls will absorb a large amount of ore powder, which buffers the impact force between the steel balls and the ore material, thereby reducing the grinding efficiency.
[0085] Further, the concentrations of illite obtained under different grinding concentrations
English Translation of PCT/CN2021/082384
were tested. The details are shown in Table 1.
Table 1
Grinding Concentration Purity ofIllite
50% 85%
60% 89%
70% 92.5%
80% 94%
90% 91.50%
Second Embodiment
[0086] 1) The ore with relatively better appearance and quality was preferably selected from the illite raw ore, and impurities that are visible and obvious to the naked eye were removed. Then the illite raw ore was subjected to primary crushing by a jaw crusher, to obtain illite raw ore powder.
[0087] 2) 800g of illite raw ore powder obtained in step 1) was mixed with 200g of water to obtain a mixed material, and ball milling was performed by a wet ball mill to the mixed material for 8 hours; after the ball milling was completed, the mixed material was subjected to cyclone separation by a cyclone separator, to obtain a primary suspension liquid.
[0088] 3) Primary sedimentation was performed to the primary suspension liquid obtained in step 2) for 24 hours, the suspension liquid was layered, and the upper-layer liquid in the suspension liquid was sucked out by negative-pressure suction, that is, the secondary suspension liquid was obtained by separation.
[0089] 4) The secondary suspension liquid obtained in step 3) was placed in a high pressure homogenizer with a pressure of 200 Bar to be subjected to high pressure homogenization cycle treatment for three times, then secondary sedimentation was performed for 72h; and then the supernatant liquid in the suspension liquid was sucked out for evaporation treatment, to
English Translation of PCT/CN2021/082384
evaporate excess water, so that the moisture content of the product was kept between 30% and 40%, and then the product was sterilized and hermetically stored, to obtain high-purity illite.
[0090] 5) Three batches of illite were randomly sampled while being hermetically stored, dry illite powder was obtained after spray-drying, and the purity of the dry illite powder of the sample was tested.
[0091] In the second embodiment, the influence of the feed-in flow rate of cyclone separation in step 2) on the separation effect was explored, with other conditions being kept unchanged and the feed-in flow rate of cyclone separation being changed, the above steps were repeated, three experiments were carried out each time, and the average value was calculated. The results were shown in Table 2. The calculation formula of separation efficiency is as follows:
separation efficiency =o/oi
[0092] In the formula, q represents the separation efficiency; o, represents the sand content at a bottom opening of the cyclone separator; oi represents the sand content at an inlet of the cyclone separator.
Table 2 Feed-in flow rate Separation Separation efficiency of Separation efficiency of Average separation 3 (m /h) efficiency of the the second time the third time efficiency first time (%) (%) (%) (0%)
10 37.52 36.83 35.49 36.61 12.5 45.39 47.85 43.62 45.62 15 75.84 75.91 77.85 76.53 17.5 78.97 76.35 79.66 78.33 20 81.22 83.46 82.53 82.4
Third Embodiment
[0093] 1) The ore with better appearance and quality was preferably selected from the illite raw ore, and impurities that are visible and obvious to the naked eye were removed. Then the illite raw ore was subjected to primary crushing by a jaw crusher, to obtain illite raw ore powder.
English Translation of PCT/CN2021/082384
[0094] 2) 800g of illite raw ore powder obtained in step 1) was mixed with 200g of water to obtain a mixed material, and ball milling was performed by a wet ball mill to the mixed material for 8 hours; after the ball milling was completed, the mixed material was subjected to cyclone separation by a cyclone separator, and the feed-in flow rate of the cyclone separation was 15 m3/h, to obtain a primary suspension liquid.
[0095] 3) Primary sedimentation was performed to the primary suspension liquid obtained in step 2), the suspension liquid was layered, and the upper-layer liquid in the suspension liquid was sucked out by negative-pressure suction, that is, the secondary suspension liquid was obtained by separation.
[0096] 4) The secondary suspension liquid obtained in step 3) was placed in a high pressure homogenizer with a pressure of 200 Bar to be subjected to high pressure homogenization cycle treatment for three times, then secondary sedimentation was performed for 72h; and then the supernatant liquid in the suspension was sucked out for evaporation treatment, to evaporate excess water, so that the moisture content of the product was kept between 30% and 40%, and then the product was sterilized and hermetically stored, to obtain high-purity illite.
[0097] 5) Three batches of illite were randomly sampled while being hermetically stored, dry illite powder was obtained after spray-drying, and the purity of the dry illite powder of the sample was tested.
[0098] In the third embodiment, the influence of the time of the primary sedimentation in step 3) on the purification effect was explored, with other conditions being kept unchanged and the time of primary sedimentation being changed, the above steps were repeated. The results were shown in Figure 2, in which the ordinate represents the purity of illite (%), and the abscissa represents the time of the primary sedimentation (d). It can be seen from Figure 2 that with the increase of sedimentation time, the purity of illite showed a trend of increasing significantly at first and then increasing slowly. In the case that the sedimentation time was 0 days, the purity of the obtained illite was 41%; after sedimentation for 1 day, the purity of illite reached 84.1%, and the purity was 88.5% and 90.3% under sedimentation for 2 days and 3 days, respectively.
Fourth Embodiment
English Translation of PCT/CN2021/082384
[0099] 1) The ore with relatively better appearance and quality was preferably selected from the illite raw ore, and impurities that are visible and obvious to the naked eye were removed. Then the illite raw ore was subjected to primary crushing by a jaw crusher, to obtain illite raw ore powder.
[00100] 2) 800g of illite raw ore powder obtained in step 1) was mixed with 200g of water to obtain a mixed material, and ball milling was performed by a wet ball mill to the mixed material for 8 hours; after the ball milling was completed, the mixed material was subjected to cyclone separation by a cyclone separator, and the feed-in flow rate of the cyclone separation was 15 m3/h, to obtain a primary suspension liquid.
[00101] 3) Primary sedimentation was performed to the primary suspension liquid obtained in step 2) for ld, the suspension was layered, and the upper-layer liquid in the suspension liquid was sucked out by negative-pressure suction, that is, the secondary suspension liquid was obtained by separation.
[00102] 4) The secondary suspension liquid obtained in step 3) was placed in a high pressure homogenizer with different pressures to be subjected to high pressure homogenization cycle treatment for three times, then secondary sedimentation was performed for 72h; and then the supernatant liquid in the suspension liquid was sucked out for evaporation treatment, to evaporate excess water, so that the moisture content of the product was kept between 30% and 40%, and then the product was sterilized and then hermetically stored, to obtain high-purity illite.
[00103] 5) Three batches of illite were randomly sampled while being hermetically stored, dry illite powder was obtained after spray-drying, and the purity of the dry illite powder of the sample was tested.
[00104] In the fourth embodiment, the influence of the pressure of the high pressure homogenization treatment in step 4) on the particle size of illite was explored, with other conditions being kept unchanged, and the pressure of the high pressure homogenization treatment being changed, the above steps were repeated. The experiments were repeated three times each time, and the average particle size was calculated. The results were shown in Table 3,
English Translation of PCT/CN2021/082384
as the pressure of homogenization increased from 100 Bar to 300 Bar, the average particle size of illite decreased from 401.35 nm to 332.64 nm, showing a decreasing trend with increasing pressure. But when the pressure was 200 Bar, the average particle size of illite was 342.52 nm.
Table 3
Pressure 100 Bar 200 Bar 300 Bar
First Test Particle Size 400.05 nm 340.59 nm 329.75 nm
Second Test Particle Size 398.69 nm 344.19 nm 336.32 nm
Third Test Particle Size 405.32 nm 342.78 nm 331.84 nm
Average Particle Size 401.35 nm 342.52 nm 332.64 nm
[00105] Further, the particle size distribution of the illite obtained when the pressure of the high pressure homogenization treatment was 200 Bar was tested, and the results were shown in Figure 3, in which the ordinate represents the particle size (nm), and the abscissa represents the relative strength. It can be seen from the figure that the particle size distribution of illite ranged from 198.55 nm to 434.81 nm, and is concentrated between 266.4 nm and 357.43 nm, and the distribution range is relatively concentrated.
Fifth Embodiment
[00106] 1) The ore with relatively better appearances and quality was preferably selected from the illite raw ore, and impurities that are visible and obvious to the naked eye were removed. Then the illite raw ore was subjected to primary crushing by a jaw crusher, to obtain illite raw ore powder.
[00107] 2) 800g of illite raw ore powder obtained in step 1) was mixed with 200g of water to obtain a mixed material, and ball milling was performed by a wet ball mill to the mixed material for 8 hours; after the ball milling was completed, the mixed material was subjected to cyclone separation by a cyclone separator, and the feed-in flow rate of the cyclone separation was 20 m3/h, to obtain a primary suspension liquid.
English Translation of PCT/CN2021/082384
[00108] 3) Primary sedimentation was performed to the primary suspension liquid obtained in step 2) for ld, the suspension liquid was layered, and the upper-layer liquid in the suspension liquid was sucked out by negative-pressure suction, that is, the secondary suspension liquid was obtained by separation.
[00109] 4) The secondary suspension liquid obtained in step 3) was placed in a high pressure homogenizer with a pressure of 200 Bar to be subjected to high pressure homogenization cycle treatment for three times, then secondary sedimentation was performed; and then the supernatant liquid in the suspension liquid was sucked out for evaporation treatment, to evaporate excess water, so that the moisture content of the product was kept between 30% and 40%, and then the product was sterilized and then hermetically stored, to obtain high-purity illite.
[00110] 5) Three batches of illite were randomly sampled while being hermetically stored, dry illite powder was obtained after spray-drying, and the purity of the dry illite powder of the sample was tested.
[00111] In the fifth embodiment, the influence of the time of secondary sedimentation instep 4) on the purity of illite was explored, with other conditions being kept unchanged and the time of secondary sedimentation being changed, the above steps were repeated. The results were shown in Figure 4, in which the ordinate represents the purity of the prepared illite, and the abscissa represents the sedimentation time (d) of the secondary sedimentation.
First Comparative Embodiment
[00112] The first comparative embodiment is basically the same as the example when the time of the secondary sedimentation is 3d in the fifth example, and the difference is that in step 4) of the first comparative example, the secondary suspension liquid is crushed by ball milling.
[00113] The results showed that the purity of the obtained illite is 90.5%; the distribution range was 800 nm to 1700 nm, and the distribution was mainly between 1050 nm to 1580 nm, and hence the particle size distribution was not concentrated.
[00114] The above embodiments only express several solutions of the present application, the descriptions thereof are specific and detailed, but should not be construed as a limitation on the
English Translation of PCT/CN2021/082384
scope of the present application. It should be pointed out that for those skilled in the art, several modifications and improvements can be made without departing from the concept of the present application, which all belong to the protection scope of the present application. Therefore, the protection scope of the present application is defined by the appended claims.
Claims (1)
- English Translation of PCT/CN2021/0823841. A preparation method for preparing illite, comprising:mixing illite raw ore powder with water, performing ball milling, and performing cyclone separation, to obtain a primary suspension liquid;performing primary sedimentation to the primary suspension liquid, and performing separation, to obtain a secondary suspension liquid; andcrushing the secondary suspension liquid by using a high pressure homogenization method, then performing secondary sedimentation, and performing separation, to obtain the illite.2. The preparation method according to claim 1, wherein a pressure is 100 Bar to 300 Bar when the secondary suspension liquid is crushed by using the high pressure homogenization method.3. The preparation method according to claim 1, wherein a pressure is 200 Bar to 30Bar when the secondary suspension liquid is crushed by using the high pressure homogenization method.4. The preparation method according to claim 1, wherein a time of the primary sedimentation is 0.5d to 3d; and/ora time of the secondary sedimentation is l d to 7d.5. The preparation method according to any one of claims 1 to 4, wherein a feed-in flow rate of the cyclone separation step is 10 m3 /h to 20 m3 /h.6. The preparation method according to any one of claims 1 to 4, wherein, based on a totalEnglish Translation of PCT/CN2021/082384mass of the illite raw ore powder and the water, a mass percentage of the illite raw ore powder is 50% to 90%.7. The preparation method according to any one of claims 1 to 4, wherein a time of the primary sedimentation is I d to 3d.8. Illite, prepared by the preparation method according to any one of claims I to 7.9. An application of the illite according to claim 8 in preparing a skin care product.10. A mud mask, wherein the mud mask comprises the illite according to claim 8.English Translation English Translation of of PCT/CN2021/082384 PCT/CN2021/08238466 6563.5 64 62.5 63 61.5 62 61 6059 58 57 0.5 0.6 0.7 0.8 0.9Grinding concentrationFigure 11 Figure100 88.5 89.6 90.3 84.1 86.465.841.7100 0 0.5 1 1.5 2 2.5 3 Sedimentation time/dFigure 22 Figure1/2 1/2English Translation English Translation of of PCT/CN2021/082384 PCT/CN2021/082384500 434.81 450 394.33 400 357.43 324.07 350 293.82 266.4 300 241.53 218.99 250 198.55 200 150 10050 0 0 20 40 60 80 100 120 relative strengthFigure 33 Figure96 95.1 95.2 94.9 94.5 94 94 92.4 93 92 91 89.889 88 87 1 2 3 4 5 6 7Sedimentation time/dFigure 44 Figure2/2 2/2
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