TW202211905A - Illite and preparation method and application thereof and mud mask - Google Patents
Illite and preparation method and application thereof and mud mask Download PDFInfo
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- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/36—Silicates having base-exchange properties but not having molecular sieve properties
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- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
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Abstract
Description
本發明涉及化妝護膚品原料製備技術領域，特別是涉及一種伊利石(Illite)的製備方法與應用。The invention relates to the technical field of preparation of raw materials for cosmetic skin care products, in particular to a preparation method and application of illite.
伊利石是一種含鉀鋁矽酸鹽雲母族黏土礦物，最早發現於美國伊利島。伊利石又稱“水白雲母”，伊利石的礦石化學成分以K 2O、Al 2O 3和SiO 2為主。伊利石的硬度低，具有不膨脹性；同時，伊利石具有富鉀、高鋁、光滑、鬆軟、耐熱、高吸油率、紫外線透過率低、流變性好、白度高、耐磨性好和抗酸鹼性等特性，被廣泛應用於鉀肥制取、造紙顏料、衛生陶瓷、保水功能材料、化妝品和橡塑填料等領域。隨著對伊利石的應用不斷的深入研究，伊利石日益成為一種重要的具有多用途的功能材料。而伊利石的純度及粒徑直接影響到伊利石的品質及功能，從而影響其應用領域；因此，伊利石的提純加工是開發利用伊利石的用途的重要工序。 Illite is a potassium-containing aluminosilicate mica clay mineral, first discovered on the island of Erie in the United States. Illite is also called "water muscovite". The chemical composition of illite is mainly K 2 O, Al 2 O 3 and SiO 2 . Illite has low hardness and non-expansion; at the same time, illite has potassium-rich, high-aluminum, smooth, soft, heat-resistant, high oil absorption, low UV transmittance, good rheology, high whiteness, good wear resistance and It is widely used in potash fertilizer preparation, papermaking pigments, sanitary ceramics, water-retaining functional materials, cosmetics, rubber and plastic fillers and other fields. 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 illite, thereby affecting its application field; therefore, the purification and processing of illite is an important process for developing and utilizing illite.
目前，國內外對伊利石的提純還沒有成熟的工藝，只是參照其他粘土礦物的提純方法對伊利石原礦進行簡單提純處理，如採用高梯度磁選法、酸浸法、焙燒法、幹法重力層析分離法、熱浮選礦和化學漂白法等對伊利石原礦進行提純處理。然而，採用這些常用的粘土礦物的提純方法對伊利石進行提純處理時，往往存在提純工藝複雜、伊利石產品純度不高和二次污染等問題，且罕有涉及對伊利石的粒徑調控的問題。At present, there is no mature process for the purification of illite at home and abroad, but the illite ore is simply purified by referring to the purification methods of other clay minerals, such as high gradient magnetic separation method, acid leaching method, roasting method, dry gravity layer The illite ore is purified by analytical separation, thermal flotation and chemical bleaching. 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 rarely involving the control of particle size of illite. .
因此，急需研發出一種能製備高純度、且粒徑分佈集中的伊利石的方法。Therefore, there is an urgent need to develop a method for preparing illite with high purity and concentrated particle size distribution.
本發明提供了一種伊利石的製備方法，該製備方法能夠提高伊利石的純度、使粒徑小且粒徑分佈集中。The invention provides a preparation method of illite, which can improve the purity of illite, make the particle size small and the particle size distribution concentrated.
本發明還提供一種伊利石，其純度高、粒徑小且分佈集中。The present invention also provides an illite with high purity, small particle size and concentrated distribution.
本發明還提供一種伊利石在製備護膚品中的應用及一種泥漿面膜，可提高其膚感和吸附性能。The invention also provides an application of illite in the preparation of skin care products and a mud mask, which can improve the skin feel and adsorption performance.
本發明的伊利石的製備方法，包括以下步驟：將伊利石原礦粉與水混合，球磨，旋流分離，得到初級懸浮液。將所述懸浮液進行初級沉降，得到二級懸浮液。採用高壓均質法破碎所述二級懸浮液，再進行二級沉降，分離得到伊利石。The preparation method of illite of the present invention comprises the following steps: mixing illite raw ore powder with water, ball milling, and cyclone separation to obtain a primary suspension. The suspension is subjected to primary settling to obtain a secondary suspension. The secondary suspension is crushed by the high pressure homogenization method, and then the secondary sedimentation is carried out to separate and obtain illite.
本發明的一實施例中，所述採用高壓均質法破碎所述二級懸浮液時的壓力為100Bar~300Bar。In an embodiment of the present invention, the pressure when the secondary suspension is crushed by the high-pressure homogenization method is 100 Bar to 300 Bar.
本發明的一實施例中，所述採用高壓均質法破碎所述二級懸浮液時的壓力為200Bar~300Bar。In an embodiment of the present invention, the pressure when the secondary suspension is crushed by the high-pressure homogenization method is 200 Bar to 300 Bar.
本發明的一實施例中，所述初級沉降的時間為0.5天~3天；和/或所述二級沉降的時間為1天~7天。In an embodiment of the present invention, the time for the primary settling is 0.5 days to 3 days; and/or the time for the secondary settling is 1 day to 7 days.
本發明的一實施例中，所述旋流分離步驟的進料流量為10m 3/h~20m 3/h時。 In an embodiment of the present invention, the feed flow rate of the cyclone separation step is 10 m 3 /h to 20 m 3 /h.
本發明的一實施例中，以所述伊利石原礦粉與所述水的總品質為基準，所述伊利石原礦粉的品質百分數為50%~90%。In an embodiment of the present invention, based on the total quality of the illite ore powder and the water, the quality percentage of the illite ore powder is 50% to 90%.
本發明的一實施例中，所述初級沉降的時間為1天~3天。In an embodiment of the present invention, the time for the primary settling is 1 day to 3 days.
本發明的伊利石由上述任一種製備方法製得。The illite of the present invention is prepared by any of the above-mentioned preparation methods.
本發明提供一種伊利石在製備護膚品中的應用。The invention provides an application of illite in the preparation of skin care products.
本發明進一步提供一種泥漿面膜，該泥漿面膜包括上述伊利石。The present invention further provides a mud mask comprising the above-mentioned illite.
基於上述，由本發明伊利石的製備方法所製得的伊利石，其純度高、粒徑小且粒徑分佈均勻，從而能提高伊利石的外觀、膚感及吸附性能等性能。進一步地，將製得的伊利石應用在製備護膚品或泥漿面膜時，能提高護膚品或泥漿面膜的膚感和吸附性能。Based on the above, the illite prepared by the illite preparation method of the present invention has high purity, small particle size and uniform particle size distribution, so that the appearance, skin feel and adsorption performance of illite can be improved. Further, when the prepared illite is applied in the preparation of skin care products or mud facial masks, the skin feel and adsorption performance of the skin care products or mud facial masks can be improved.
為了便於理解本發明，下面將對本發明進行更全面的描述，並給出了本發明的較佳實施例。但是，本發明可以以許多不同的形式來實現，並不限於本文所描述的實施例。相反地，提供這些實施例的目的是使對本發明的公開內容的理解更加透徹全面。In order to facilitate understanding of the present invention, the present invention will be described more fully below, and preferred embodiments of the present invention will be given. However, the present invention may be embodied in many different forms and is not limited to the embodiments described herein. Rather, these embodiments are provided so that a thorough and complete understanding of the present disclosure is provided.
除非另有定義，本文所使用的所有的技術和科學術語與屬於本發明的技術領域的技術人員通常理解的含義相同。本文中在本發明的說明書中所使用的術語只是為了描述具體的實施例的目的，不是旨在於限制本發明。本文所使用的術語“和／或”包括一個或多個相關的所列專案的任意的和所有的組合。Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terms used herein in the description of the present invention are for the purpose of describing specific embodiments only, and are not intended to limit the present invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
伊利石的純度一直是考察伊利石品質的重要因素，因為伊利石的純度不僅影響其品質和外觀等，還會影響其應用領域和使用範圍。現有技術中，目前已報導的伊利石的提純工藝得到的伊利石的純度多在70%~80%之間，鮮有能製得高純度的伊利石，尤其是得到純度大於90%的伊利石的提純的方法。The purity of illite has always been an important factor in examining the quality of illite, because the purity of illite not only affects its quality and appearance, but also affects its application field and scope of use. In the prior art, the purity of the illite obtained by the reported purification process of illite is mostly between 70% and 80%, and it is rare to obtain high-purity illite, especially to obtain illite with a purity greater than 90%. method of purification.
且，現有技術的伊利石提純工藝的關注點多在於提高伊利石純度、提取率和利用率等方面，而關於伊利石粒徑方面的研究鮮有報導。正是因為現有技術中得到的伊利石的品質還不夠高，因此伊利石的應用領域大大受限。例如，在護膚品領域，特別是泥漿面膜中，多是以高嶺土作為泥漿替代原料使用，而伊利石僅僅作為輔助的概念性添加劑。這主要是因為伊利石本身的純度及品質不高，相比於高嶺土不具有明顯優勢。Moreover, the focus of the illite purification process in the prior art is to improve the purity, extraction rate and utilization rate of illite, and there are few reports on the research on the particle size of illite. It is precisely because the quality of illite obtained in the prior art 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 mud substitute raw material, while illite is only used as an auxiliary conceptual additive. This is mainly because the purity and quality of illite itself is not high, and it does not have obvious advantages compared with kaolin.
基於此，本發明的技術人員結合伊利石的結構特性，通過多級破碎工藝，使伊利石原礦中的伊利水雲母更充分的分散於水中，再利用伊利水雲母的懸浮特性以及重力沉降作用，將伊利水雲母與雜質礦石實現分離，從而獲得具有高純度、高品質的伊利石。Based on this, the technical personnel of the present invention combined the structural characteristics of illite, and through the multi-stage crushing process, made the illite ore in the illite ore more fully dispersed in the water, and then used the suspension characteristics of illite and the effect of gravity sedimentation, The illite is separated from the impurity ore to obtain high-purity and high-quality illite.
且進一步通過對伊利石性質的研究發現：伊利石的粒徑不僅能夠改變護膚產品的膚感和外觀等性狀，而且還影響其吸附性能。經過大量實驗研究，本發明的技術人員創造性的採用高壓均質工藝，對伊利石進行破碎，使其具有更細小、分佈更均勻的粒徑，並進一步提純，從而得到純度高、粒徑小且粒徑分佈均勻的伊利石，應用於製備護膚品時，提高了護膚產品的膚感、外觀和吸附性性能。And further research on the properties of illite found that the particle size of illite can not only change the skin feel and appearance of skin care products, but also affect its adsorption performance. After a large amount of experimental research, the technical personnel of the present invention creatively adopted the high-pressure homogenization process to crush the illite to have a finer and more uniform particle size, and further purify it to obtain high purity, small particle size and granular When the illite with uniform diameter distribution is used in the preparation of skin care products, the skin feel, appearance and adsorption properties of the skin care products are improved.
本發明一實施方式提供了一種伊利石的製備方法，包括以下步驟S10~S30。An embodiment of the present invention provides a method for preparing illite, including the following steps S10-S30.
步驟S10、將伊利石原礦粉與水混合，球磨，旋流分離，得到初級懸浮液。Step S10, mixing illite ore powder with water, ball milling, and cyclone separation to obtain a primary suspension.
將伊利石原礦粉末和水混合後球磨，球磨過程中對伊利石原礦粉進行了破碎得到粒徑更小的伊利石，再通過旋流分離，將碎石碎渣等雜質分離出來，從而得到初級懸浮液。The illite ore powder is mixed with water and then ball-milled. During the ball milling process, the illite ore powder is crushed to obtain illite with a smaller particle size. Then, the impurities such as crushed stone and slag are separated by cyclone separation, so as to obtain primary illite. suspension.
在其中一些實施例中，步驟S10中，以伊利石原礦粉與水的總品質為基準，伊利石原礦粉的品質百分數為50%~90%。In some of the embodiments, in step S10, based on the total quality of the illite ore powder and water, the quality percentage of the illite ore powder is 50% to 90%.
在其中一些實施例中，步驟S10中，球磨步驟的時間為4小時~12小時。In some of these embodiments, in step S10, the time of the ball milling step is 4 hours to 12 hours.
伊利石原礦粉的品質百分數影響到球磨步驟時物料的磨礦濃度，伊利石原礦粉的品質百分數即指球磨步驟時，物料中所含固體物料品質的百分數。它不僅影響磨機生產能力、能耗，還會影響球磨後得到的產品品質，從而影響伊利石的提純效果。The quality percentage of illite raw ore powder affects the grinding concentration of the material in the ball milling step. The quality percentage of illite raw ore powder refers to the quality 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 after ball milling, thereby affecting the purification effect of illite.
球磨的磨礦效率是指磨機的產率與磨機能耗之間的比值，具體計算見式(1)、(2)和(3)：The grinding efficiency of ball mill refers to the ratio between the yield of the mill and the energy consumption of the mill. The specific calculation is shown in formulas (1), (2) and (3):
q=m/Vt 式(1)；q=m/Vt Formula (1);
W=Pt=UIt 式(2)；W=Pt=UIt Formula (2);
η=q/W 式(3)。η=q/W Formula (3).
其中，式(1)中，q表示磨機的產率，m為礦石產量，單位：噸(t)；V是磨機筒體內的有效體積，單位：立方公尺(m 3)；t為磨機工作時間，單位：小時(h)。 Among them, in formula (1), q represents the yield of the mill, m is the output of ore, unit: ton (t); V is the effective volume in the barrel of the mill, unit: cubic meter (m 3 ); t is Mill working time, unit: hour (h).
式(2)中，W表示磨機的能耗，P為球磨機功率，單位：千瓦(kW)；U為電壓，單位：伏特(V)；I為電流，單位：安培(A)。In formula (2), W represents the energy consumption of the mill, P is the power of the ball mill, unit: kilowatt (kW); U is the voltage, unit: volt (V); I is the current, unit: ampere (A).
式(3)中，η表示磨礦效率，q表示磨機的產率，W表示磨機的能耗，單位：千瓦(kW)。In formula (3), η represents the grinding efficiency, q represents the productivity of the mill, and W represents the energy consumption of the mill, in kilowatts (kW).
以伊利石原礦粉與水的總品質為基準，當伊利石原礦粉的品質百分數為50%~90%。球磨的產率高，磨礦效率高，且球磨獲得的伊利石產品品質好。Based on the total quality of illite ore powder and water, the quality percentage of illite ore powder is 50%~90%. The yield of ball milling is high, the grinding efficiency is high, and the illite products obtained by ball milling are of good quality.
在其中一些實施例中，步驟S10中的球磨步驟採用濕式球磨機進行。In some of these embodiments, the ball milling step in step S10 is performed using a wet ball mill.
優選地，以伊利石原礦粉與水的總品質為基準，伊利石原礦粉的品質百分數為50%~80%。進一步優選地，伊利石原礦粉的品質百分數為70%~80%。Preferably, based on the total quality of the illite ore powder and water, the quality percentage of the illite ore powder is 50% to 80%. Further preferably, the quality percentage of illite ore powder is 70% to 80%.
在其中一些實施例中，步驟S10中的旋流分離步驟的進料流量為10m 3/h~20m 3/h。 In some of these embodiments, the feed flow rate of the cyclone separation step in step S10 is 10 m 3 /h˜20 m 3 /h.
通過旋流分離能將伊利石原礦粉中夾雜的碎石或碎渣等雜質分離出來，從而獲得較純的伊利石。本發明的技術人員在進一步的實驗過程中發現：進行旋流分離步驟時的進料流量對伊利石原礦粉的分離提純效率有較大影響。Impurities such as crushed stone or slag mixed in the illite raw ore powder can be separated by cyclone separation, so as to obtain purer illite. The technical personnel of the present invention found in the further experiment process that the feed flow rate during the cyclone separation step has a great influence on the separation and purification efficiency of the illite raw ore powder.
當其他工藝條件保持不變，隨著進料流量的增長，旋流分離步驟的分離效率呈現出先顯著增長再緩慢上升的趨勢。具體的，當進口流量從10m 3/h增加到15m 3/h時，分離效率從36.61%上升至76.53%左右；而當進口流量從15m 3/h繼續增加到20m 3/h時，分離效率則緩慢增長至82.4%左右。優選地，步驟S10中的旋流分離步驟的進料流量為15m 3/h~20m 3/h。 When other process conditions remain unchanged, with the increase of the feed flow rate, the separation efficiency of the cyclone separation step shows a trend of firstly increasing significantly and then slowly increasing. Specifically, when the inlet flow 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 continued to increase from 15m 3 /h to 20m 3 /h, the separation efficiency Then it slowly increased to about 82.4%. Preferably, the feed flow rate of the cyclone separation step in step S10 is 15m 3 /h~20m 3 /h.
在其中一些實施例中，步驟S10中的旋流分離步驟採用旋流分離器進行。進一步地，本發明的技術人員發現：隨著進料流量的增長，能耗會相應增加，並且會導致旋流分離器內的壓力差增大，而這都將會造成成本的增長和儀器損耗的加重。進一步優選地，步驟S10中的旋流分離步驟的進料流量為15m 3/h。 In some of these embodiments, the cyclone separation step in step S10 is performed using a cyclone separator. Further, those skilled in the present invention found that with the increase of the feed flow, the energy consumption will increase accordingly, and the pressure difference in the cyclone separator will increase, which will lead to the increase of cost and the loss of equipment. aggravation. Further preferably, the feed flow rate of the cyclone separation step in step S10 is 15 m 3 /h.
步驟S20、將步驟S10獲得的初級懸浮液進行初級沉降，得到二級懸浮液。In step S20, the primary suspension obtained in step S10 is subjected to primary sedimentation to obtain a secondary suspension.
將初級懸浮液進行初級沉降，初級懸浮液的雜質逐漸沉澱下來，而伊利石中的伊利水雲母仍懸浮在上層液體中，從而可以進一步提純伊利石。The primary suspension is subjected to primary sedimentation, the impurities of the primary suspension are gradually precipitated, and the illite mica in the illite is still suspended in the upper liquid, so that the illite can be further purified.
在其中一些實施例中，步驟S20中初級沉降的時間為1天~3天。In some of these embodiments, the time for the primary sedimentation in step S20 is 1 day to 3 days.
伊利石純度指的是伊利石中伊利水雲母的含量，而伊利水雲母具有懸浮特性，在初級沉降中，具有懸浮特性的伊利水雲母仍然懸停在水中，而雜質礦石則由於重力作用緩慢沉降下來。The purity of illite refers to the content of illite in illite, and illite has a suspension characteristic. In the primary settlement, the illite with suspension characteristics is still suspended in the water, while the impurity ore settles slowly due to gravity down.
當控制其他工藝條件保持不變，改變初級沉降的時間進行實驗探究，結果表明：當初級沉降的時間為1天~3天時，雜質礦石則由於重力作用逐漸沉降下來，從而提高了伊利石中的伊利水雲母的含量，即提高了伊利石的純度。進一步地，當初級沉降的時間為超過3天時，初級懸浮液中部分粒徑較大的伊利水雲母也會隨之沉降下來，反而造成伊利水雲母的含量降低，伊利石的產率下降。優選地，初級沉降時間為1天~3天。When the other process conditions were kept unchanged, and the time of primary settling was changed, the results showed that: when the time of primary settling was 1 day to 3 days, the impurity ore gradually settled down due to the action of gravity, thus increasing the concentration of illite. The content of illite mica increases the purity of illite. Further, when the primary sedimentation time is more than 3 days, some illite with larger particle size in the primary suspension will also settle down, which will reduce the content of illite and the yield of illite. Preferably, the primary settling time is 1 day to 3 days.
在其中一些實施例中，步驟S20中，分離步驟採用負壓抽吸的方式吸取上層液體，得到二級懸浮液。In some of the embodiments, in step S20, the separation step adopts negative pressure suction to suck up the upper layer liquid to obtain a secondary suspension.
步驟S30、採用高壓均質法破碎步驟S20獲得的二級懸浮液，再進行二級沉降，分離得到伊利石。In step S30, the secondary suspension obtained in step S20 is crushed by a high pressure homogenization method, and then secondary sedimentation is performed to separate and obtain illite.
均質法破碎二級懸浮液，從而獲得粒徑更細、粒徑分佈更集中的伊利石。本發明技術人員發現：採用高壓均質法破碎二級懸浮液，壓力對伊利石的粒徑大小、尤其是粒徑分佈有很大影響。The homogenization method crushes the secondary suspension to obtain illite with finer particle size and more concentrated particle size distribution. Those skilled in the present invention have found that: using the high pressure homogenization method to crush the secondary suspension, the pressure has a great influence on the particle size of illite, especially the particle size distribution.
在其中一些實施例中，上述採用高壓均質法破碎二級懸浮液時的壓力為100Bar~300Bar。In some of the embodiments, the pressure when the secondary suspension is crushed by the high-pressure homogenization method is 100 Bar to 300 Bar.
當控制其他工藝條件保持不變，隨著高壓均質處理的壓力從100Bar增加到300Bar，製得的伊利石的平均粒徑從401.35nm減小至332.64nm，呈現出隨壓力增大而減小的趨勢。但是當壓力為200Bar時，伊利石的平均粒徑即為342.52nm，說明當壓力超過200Bar之後，壓力的增加對粒徑減少的影響較小。當採用高壓均質法破碎二級懸浮液時的壓力為100Bar~300Bar時，能得到粒徑較小的伊利石。When other process conditions were controlled to remain unchanged, as the pressure of the high-pressure homogenization treatment increased from 100Bar to 300Bar, the average particle size of the prepared illite decreased from 401.35nm to 332.64nm, showing a decrease with the increase of the pressure. trend. But when the pressure is 200Bar, the average particle size of illite is 342.52nm, indicating that when the pressure exceeds 200Bar, the increase of pressure has little effect on the decrease of particle size. When the pressure of the secondary suspension is 100Bar~300Bar by the high-pressure homogenization method, illite with smaller particle size can be obtained.
在其中一些實施例中，步驟S30中，採用高壓均質法破碎二級懸浮液時的壓力為200Bar~300Bar。In some embodiments, in step S30, the pressure when the secondary suspension is crushed by the high-pressure homogenization method is 200Bar˜300Bar.
當採用高壓均質法破碎二級懸浮液時的壓力為200Bar~300Bar時，能得到粒徑較小且粒徑更加集中的伊利石。具體的，當採用高壓均質法破碎二級懸浮液時的壓力為200Bar時，得到伊利石的粒徑分佈範圍為198.55nm~434.81nm，且集中分佈在266.4nm~357.43nm之間，分佈範圍相對比較集中。When the high-pressure homogenization method is used to crush the secondary suspension with a pressure of 200Bar~300Bar, illite with smaller particle size and more concentrated particle size can be obtained. Specifically, when the pressure when the secondary suspension is crushed by the high-pressure homogenization method is 200Bar, the particle size distribution range of the obtained illite is 198.55nm~434.81nm, and the distribution is concentrated between 266.4nm~357.43nm, and the distribution range is relatively relatively concentrated.
在其中一些實施例中，步驟S30中，採用高壓均質法破碎二級懸浮液時，均質次數為1次~3次；具體地，均質次數為3次。In some of the embodiments, in step S30, when the secondary suspension is crushed by the high-pressure homogenization method, the number of times of homogenization is 1 to 3 times; specifically, the number of times of homogenization is 3 times.
進一步地，採用高壓均質法破碎二級懸浮液後，使得懸浮液中料體的顆粒均粒徑更細小，在二級沉降過程中，隨著沉降時間的增加，伊利石的純度呈現出逐漸增大的趨勢，固體雜質顆粒能夠有效的沉降下來，從而與伊利水雲母有效分離，進一步提高伊利石的純度。Further, after the secondary suspension is crushed by the high-pressure homogenization method, the average particle size of the material in the suspension is made smaller. The large trend is that the solid impurity particles can effectively settle down, so as to be effectively separated from the illite hydromica, and further improve the purity of illite.
在其中一些實施例中，步驟S30中，二級沉降的時間為1天~7天。In some of these embodiments, in step S30, the time for the secondary settling is 1 day to 7 days.
當控制其他工藝條件保持不變，改變二級沉降的時間進行實驗探究，結果表明：當二級沉降時間在1天~3天之間時，伊利石純度增長比較明顯，隨著沉降時間持續增加至7天，伊利石純度基本不再發生變化；而沉降時間過長，懸浮的伊利水雲母也會產生沉降，反而導致伊利石的產率反而下降。When controlling other process conditions to remain unchanged, changing the time of secondary settling for experimental exploration, the results show that when the time of secondary settling is between 1 day and 3 days, the purity of illite increases significantly, and with the continuous increase of settling time After 7 days, the purity of illite basically does not change; and if the sedimentation time is too long, the suspended illite will also settle, which will lead to a decrease in the yield of illite.
在其中一些實施例中，步驟S30中，二級沉降的時間為1天~6天。優選地，二級沉降的時間為2天~5天。In some of the embodiments, in step S30, the time for the secondary settling is 1 day to 6 days. Preferably, the time for the secondary settling is 2 days to 5 days.
在其中一些實施例中，上述製備方法還包括將伊利石原礦破碎製得伊利石原礦粉的步驟S11。具體如下：In some of the embodiments, the above preparation method further includes step S11 of crushing illite ore to obtain illite ore powder. details as follows:
步驟S11、將伊利石原礦進行初級破碎，獲得伊利石原礦粉。具體地，採用顎式破碎機將伊利石原礦進行初級破碎，獲得伊利石原礦粉。In step S11, primary crushing of illite ore is performed to obtain illite ore powder. Specifically, primary crushing of illite ore is performed with a jaw crusher to obtain illite ore powder.
採用顎式破碎機將伊利石原礦進行初級破碎時，採用顎式破碎機的處理量為1t/h~800t/h，可根據實際物料量選擇。When primary illite ore is crushed by jaw crusher, the processing capacity of jaw crusher is 1t/h~800t/h, which can be selected according to the actual material volume.
進一步地，伊利石原礦中優選形態和品質較優的礦石，去除肉眼可見、明顯的雜質。Further, ore with better shape and quality is preferred in illite raw ore to remove impurities that are visible and obvious to the naked eye.
在其中一些實施例中，步驟S30中，在二次沉澱步驟之後，還包括分離得到伊利石的步驟，具體如下：In some of these embodiments, in step S30, after the secondary precipitation step, the step of separating and obtaining illite is further included, as follows:
二次沉澱後，將懸浮液中上層清液抽吸出來進行蒸發處理，以蒸發多餘水分，使得產品的水分含量保持在30%~40%之間，再對產品進行滅菌處理後密封保存，得到高純度的伊利石。After the secondary precipitation, the supernatant liquid in the suspension 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 the product is sterilized and then sealed and stored to obtain. High-purity illite.
上述高品質伊利石的製備方法中，先將伊利石原礦粉與水混合後球磨，球磨過程中對伊利石原礦粉進行了破碎，得到粒徑更小的伊利石，再通過旋流分離將伊利石原礦粉中夾帶的碎石碎渣等雜質分離出來，從而分離得到初級懸浮液；然後將初級懸浮液進行初級沉降，初級懸浮液的雜質逐漸沉澱下來，而伊利水雲母，即純伊利石仍懸浮在上層液體中，從而能分離出雜質，得到含較高純度的伊利石的二級懸浮液；進一步地，採用高壓均質法破碎二級懸浮液，從而獲得粒徑更細、粒徑分佈更集中的伊利石，並進一步進行二級沉降，從而能進一步提純伊利石，得到高純度的伊利石。In the above-mentioned preparation method of high-quality illite, the illite ore powder is first mixed with water and then ball-milled. The impurities such as gravel and slag entrained in the stone ore powder are separated out to obtain a primary suspension; then the primary suspension is subjected to primary sedimentation, and the impurities in the primary suspension are gradually precipitated, while the illite, that is, pure illite still remains. It is suspended in the upper layer liquid, so that impurities can be separated, and a secondary suspension containing higher purity illite can be obtained; further, the secondary suspension is broken by a high-pressure homogenization method, so as to obtain a finer particle size and a better particle size distribution. The concentrated illite is further subjected to secondary sedimentation, so that the illite can be further purified to obtain high-purity illite.
本發明的一實施方式提供上述任一種製備方法製得的伊利石。An embodiment of the present invention provides illite prepared by any of the above preparation methods.
上述高品質伊利石的製備方法先後通過球磨和高壓均質法對伊利石原礦粉進行破碎，能夠使伊利石礦石的破碎更為徹底，同時通過兩次沉澱使得礦石中伊利水雲母能夠更充分地分離，在提高伊利水雲母的利用率的同時提高伊利石的純度。此外，採用了高壓均質技術不僅使得伊利石破碎更為徹底，而且能夠控制伊利石粒徑，使得製備的成品粒徑更細小、粒徑分佈更集中，從而提高伊利石的外觀、膚感及吸附性能等屬性，使製得的伊利石的純度高、粒徑小且粒徑分佈均勻，從而能提高伊利石的外觀、膚感及吸附性能等性能。因此，將製得的高純度、粒徑小且分佈集中的伊利石應用在製備護膚品時，能提高護膚品的膚感和吸附性能。The above-mentioned high-quality illite preparation method successively crushes the illite ore powder by ball milling and high-pressure homogenization, which can make the crushing of the illite ore more thorough, and at the same time, through two precipitations, the illite in the ore can be more fully separated. , while improving the utilization rate of illite hydromica and improving the purity of illite. In addition, the use of high-pressure homogenization technology not only makes the illite broken more thoroughly, but also can control the particle size of illite, so that the particle size of the prepared product is smaller and the particle size distribution is more concentrated, thereby improving the appearance, skin feel and adsorption of illite. Properties and other properties, the obtained illite has high purity, small particle size and uniform particle size distribution, so that the appearance, skin feel and adsorption performance of illite can be improved. Therefore, when the obtained illite with high purity, small particle size and concentrated distribution is used in the preparation of skin care products, the skin feel and adsorption performance of the skin care products can be improved.
本發明一實施方式還提供了上述伊利石在製備護膚品中的應用。An embodiment of the present invention also provides the application of the above illite in the preparation of skin care products.
上述製備方法製得的伊利石的純度高、粒徑小且粒徑分佈均勻，從而能提高伊利石的外觀、膚感及吸附性能等性能。因此，將製得的高純度、粒徑小且分佈集中的伊利石應用在製備護膚品時，能提高護膚品的膚感和吸附性能。The illite prepared by the above preparation method has high purity, small particle size and uniform particle size distribution, 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 particle size and concentrated distribution is used in the preparation of skin care products, the skin feel and adsorption performance of the skin care products can be improved.
本發明進一步提供了一種泥漿面膜，該泥漿面膜包括上述伊利石。The present invention further provides a mud mask comprising the above-mentioned illite.
伊利石的雜質含量越少、純度越高、粒徑越小及其粒徑分佈範圍越窄，則伊利石的膚感越細膩，比表面積和吸附性能也會隨之上升，從而能提升泥漿面膜的膚感和吸附性能。The lower the impurity content of illite, the higher the purity, the smaller the particle size and the narrower the particle size distribution, the finer the skin feel of illite, and the specific surface area and adsorption performance will also increase, which can improve the mud mask. skin feel and adsorption properties.
這裏按照本發明的伊利石及其製備方法與應用舉例，但本發明並不局限於下述實施例。Here, according to the illite of the present invention and its preparation method and application examples, the present invention is not limited to the following examples.
實施例1Example 1
1)從伊利石原礦中優選形態和品質較優的礦石，去除肉眼可見、明顯的雜質。然後採用顎式破碎機將伊利石原礦進行初級破碎，獲得伊利石原礦粉。1) Select the ore with better shape and quality from the illite ore, and remove the visible and obvious impurities. Then primary crushing of illite ore is carried out by jaw crusher to obtain illite ore powder.
2)將步驟1)獲得的伊利石原礦粉和水混合得到混合物料，採用濕式球磨機進行球磨8小時，球磨完畢後將混合物料通過旋流分離器進行旋流分離，旋流分離的進料流量為15m 3/h，得到初級懸浮液。 2) The illite ore powder obtained in step 1) is mixed with water to obtain a mixed material, and a wet ball mill is used to perform ball milling for 8 hours. After the ball milling is completed, the mixed material is subjected to cyclone separation by a cyclone separator, and the feed of the cyclone separation is carried out. The flow rate was 15 m 3 /h and a primary suspension was obtained.
3)將步驟2)獲得的初級懸浮液進行初級沉澱24小時，懸浮液分層，通過負壓抽吸將懸浮液中的上層液體抽吸出來，即分離得到二級懸浮液。3) The primary suspension obtained in step 2) is subjected to primary precipitation for 24 hours, the suspension is layered, and the upper layer liquid in the suspension is sucked out by negative pressure suction, that is, the secondary suspension is obtained by separation.
4)將步驟3)獲得的得到二級懸浮液置於壓力為200Bar的高壓均質機內進行高壓均質迴圈處理三次，然後進行二次沉澱72小時；然後將懸浮液中上層清液抽吸出來進行蒸發處理，以蒸發多餘水分，使得產品的水分含量保持在30%~40%之間，再對產品進行滅菌處理後密封保存，得到高純度的伊利石。4) The obtained secondary suspension obtained in step 3) is placed in a high-pressure homogenizer with a pressure of 200Bar to carry out high-pressure homogenization loop treatment three times, and then secondary precipitation is carried out for 72 hours; then the supernatant in the suspension is sucked out Evaporation treatment is carried out 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 sealed and stored to obtain high-purity illite.
5)在密封保存的同時隨機取樣三批次伊利石，噴乾後獲得伊利石乾粉，檢測樣品的伊利石乾粉純度。5) Three batches of illite are randomly sampled while being sealed and preserved, and dry illite powder is obtained after spray-drying, and the purity of the dry illite powder of the sample is tested.
本實施例1對步驟2)中物料的固含量對球磨效率的影響進行探索，保持伊利石原礦粉與水的總品質及其他實驗條件不變，改變步驟2)中伊利石原礦粉的品質，重複進行上述步驟，按下述公式計算球磨的磨礦效率：In the
具體計算見式(1)、(2)和(3)：The specific calculations are shown in formulas (1), (2) and (3):
q=m/Vt 式(1)；q=m/Vt Formula (1);
W=Pt=UIt 式(2)；W=Pt=UIt Formula (2);
η=q/W 式(3)。η=q/W Formula (3).
其中，式(1)中，q表示磨機的產率，m為礦石產量，單位：噸(t)；V是磨機筒體內的有效體積，單位：立方公尺(m 3)；t為磨機工作時間，單位：小時(h)。 Among them, in formula (1), q represents the yield of the mill, m is the output of ore, unit: ton (t); V is the effective volume in the barrel of the mill, unit: cubic meter (m 3 ); t is Mill working time, unit: hour (h).
式(2)中，W表示磨機的能耗，P為球磨機功率，單位：千瓦(kW)；U為電壓，單位：伏特(V)；I為電流，單位：安培(A)。In formula (2), W represents the energy consumption of the mill, P is the power of the ball mill, unit: kilowatt (kW); U is the voltage, unit: volt (V); I is the current, unit: ampere (A).
式(3)中，η表示磨礦效率，q表示磨機的產率，W表示磨機的能耗，單位：千瓦(kW)。In formula (3), η represents the grinding efficiency, q represents the productivity of the mill, and W represents the energy consumption of the mill, in kilowatts (kW).
具體結果如圖1所示，圖1中縱坐標表示磨礦效率，橫坐標表示磨礦濃度，即以伊利石原礦粉與水的總品質為基準，伊利石原礦粉的所占的品質分數。從圖1中可知：當礦磨濃度從0.5上升到0.8的過程中，磨礦效率從61.5%增加至65%，呈現出隨濃度增長而上升的趨勢；而當濃度超過0.8之後，磨礦效率反而出現下降。這可能是因為當磨機內部的磨礦濃度較低時，礦漿在筒體內流動速度過快，導致研磨的效率較低，而礦漿濃度的上升會增加鋼球衝擊礦料的機會，使磨礦效率增加。而當礦漿濃度超過0.8之後，鋼球的表面會吸附大量的礦粉，從而緩衝鋼球與礦料的衝擊力，降低了磨礦效率。The specific results are shown in Figure 1. In Figure 1, the ordinate represents the grinding efficiency, and the abscissa represents the grinding concentration, that is, the quality fraction of the illite ore powder based on the total quality of the illite ore powder and water. It can be seen from Figure 1 that when the concentration of ore grinding increases from 0.5 to 0.8, the grinding efficiency increases from 61.5% to 65%, showing a rising trend with the increase of concentration; and when the concentration exceeds 0.8, the grinding efficiency Instead, it declined. This may be because when the grinding concentration inside the mill is low, the slurry flows too fast in the cylinder, resulting in low grinding efficiency. Efficiency increases. When the slurry concentration exceeds 0.8, the surface of the steel ball will absorb a large amount of mineral powder, thereby buffering the impact force of the steel ball and the mineral material, reducing the grinding efficiency.
進一步地，測試了在不同磨礦濃度下，得到的伊利石的濃度。具體如下表1所示：
表1
實施例2Example 2
1)從伊利石原礦中優選形態和品質較優的礦石，去除肉眼可見、明顯的雜質。然後採用顎式破碎機將伊利石原礦進行初級破碎，獲得伊利石原礦粉。1) Select the ore with better shape and quality from the illite ore, and remove the visible and obvious impurities. Then primary crushing of illite ore is carried out by jaw crusher to obtain illite ore powder.
2)將步驟1)獲得的800g伊利石原礦粉和200g水混合得到混合物料，採用濕式球磨機進行球磨8小時，球磨完畢後將混合物料通過旋流分離器進行旋流分離，得到初級懸浮液。2) 800g of illite ore powder obtained in step 1) and 200g of water were mixed to obtain a mixture, and a wet ball mill was used to perform ball milling for 8 hours. After the ball milling, the mixture was cyclone separated by a cyclone to obtain a primary suspension. .
3)將步驟2)獲得的初級懸浮液進行初級沉澱24小時，懸浮液分層，通過負壓抽吸將懸浮液中的上層液體抽吸出來，即分離得到二級懸浮液。3) The primary suspension obtained in step 2) is subjected to primary precipitation for 24 hours, the suspension is layered, and the upper layer liquid in the suspension is sucked out by negative pressure suction, that is, the secondary suspension is obtained by separation.
4)將步驟3)獲得的得到二級懸浮液置於壓力為200Bar的高壓均質機內進行高壓均質迴圈處理三次，然後進行二次沉澱72小時；然後將懸浮液中上層清液抽吸出來進行蒸發處理，以蒸發多餘水分，使得產品的水分含量保持在30%~40%之間，再對產品進行滅菌處理後密封保存，得到高純度的伊利石。4) The obtained secondary suspension obtained in step 3) is placed in a high-pressure homogenizer with a pressure of 200Bar to carry out high-pressure homogenization loop treatment three times, and then secondary precipitation is carried out for 72 hours; then the supernatant in the suspension is sucked out Evaporation treatment is carried out 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 sealed and stored to obtain high-purity illite.
5)在密封保存的同時隨機取樣三批次伊利石，噴乾後獲得伊利石乾粉，檢測樣品伊利石乾粉純度。5) Three batches of illite were randomly sampled while being sealed and preserved, and the illite dry powder was obtained after spray-drying, and the purity of the sample illite dry powder was tested.
本實施例2對步驟2)中，旋流分離時的進料流量對分離效果的影響進行探究，保持其他條件不變，改變旋流分離的進料流量，重複進行上述步驟，每次進行三次實驗，計算平均值。結果如表2所示。其中，分離效率的計算公式如下：In this Example 2, in step 2), the influence of the feed flow rate during cyclone separation on the separation effect was explored, and other conditions were kept unchanged, the feed flow rate of cyclone separation was changed, and the above steps were repeated for three times each time. Experiment and calculate the average. The results are shown in Table 2. Among them, the calculation formula of separation efficiency is as follows:
分離效率η=ω o/ω i Separation efficiency η=ω o /ω i
式中，η表示分離效率；ω
o表示旋流分離器的底流口處的沙粒含量；ω
i表示旋流分離器入口處的沙粒含量。
表2
實施例3Example 3
1)從伊利石原礦中優選形態和品質較優的礦石，去除肉眼可見、明顯的雜質。然後採用顎式破碎機將伊利石原礦進行初級破碎，獲得伊利石原礦粉。1) Select the ore with better shape and quality from the illite ore, and remove the visible and obvious impurities. Then primary crushing of illite ore is carried out by jaw crusher to obtain illite ore powder.
2)將步驟1)獲得的800g伊利石原礦粉和200g水混合得到混合物料，採用濕式球磨機進行球磨8小時，球磨完畢後將混合物料通過旋流分離器進行旋流分離，進料流量為15m 3/h，得到初級懸浮液。 2) 800g of illite ore powder obtained in step 1) was mixed with 200g of water to obtain a mixture, and a wet ball mill was used to perform ball milling for 8 hours. After the ball milling, the mixture was cyclone separated by a cyclone, and the feed flow was 15 m 3 /h to obtain a primary suspension.
3)將步驟2)獲得的初級懸浮液進行初級沉澱，懸浮液分層，通過負壓抽吸將懸浮液中的上層液體抽吸出來，即分離得到二級懸浮液。3) The primary suspension obtained in step 2) is subjected to primary precipitation, the suspension is layered, and the upper layer liquid in the suspension is sucked out by negative pressure suction, that is, the secondary suspension is obtained by separation.
4)將步驟3)獲得的得到二級懸浮液置於壓力為200Bar的高壓均質機內進行高壓均質迴圈處理三次，然後進行二次沉澱72小時；然後將懸浮液中上層清液抽吸出來進行蒸發處理，以蒸發多餘水分，使得產品的水分含量保持在30%~40%之間，再對產品進行滅菌處理後密封保存，得到高純度的伊利石。4) The obtained secondary suspension obtained in step 3) is placed in a high-pressure homogenizer with a pressure of 200Bar to carry out high-pressure homogenization loop treatment three times, and then secondary precipitation is carried out for 72 hours; then the supernatant in the suspension is sucked out Evaporation treatment is carried out 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 sealed and stored to obtain high-purity illite.
5)在密封保存的同時隨機取樣三批次伊利石，噴乾後獲得伊利石乾粉，檢測樣品的伊利石乾粉純度。5) Three batches of illite are randomly sampled while being sealed and preserved, and dry illite powder is obtained after spray-drying, and the purity of the dry illite powder of the sample is tested.
本實施例3對步驟3)中，初級沉澱的時間對提純效果的影響進行探究，保持其他條件不變，改變初級沉澱的時間，重複進行上述步驟。結果如圖2所示，圖2中縱坐標為伊利石純度（%），橫坐標為初級沉澱時間（天(d)）。從圖2可看出隨著沉降時間的增加，伊利石的純度呈現出先顯著增大後緩慢增長的趨勢。當沉降時間為0天的伊利石，得到的伊利石的純度為41%，沉降1天之後，伊利石純度達到84.1%，沉降2天和3天的純度分別為88.5%和90.3%。In this Example 3, in step 3), the influence of the time of primary precipitation on the purification effect was explored, other conditions were kept unchanged, the time of primary precipitation was changed, and the above steps were repeated. The results are shown in Figure 2, where the ordinate in Figure 2 is the illite purity (%), and the abscissa is the primary precipitation time (day (d)). It can be seen from Figure 2 that with the increase of sedimentation time, the purity of illite shows a trend of increasing significantly at first and then slowly increasing. When the sedimentation time is 0 days, the purity of the obtained illite is 41%. After sedimentation for 1 day, the purity of illite reaches 84.1%, and the purity of sedimentation for 2 days and 3 days is 88.5% and 90.3%, respectively.
實施例4Example 4
1)從伊利石原礦中優選形態和品質較優的礦石，去除肉眼可見、明顯的雜質。然後採用顎式破碎機將伊利石原礦進行初級破碎，獲得伊利石原礦粉。1) Select the ore with better shape and quality from the illite ore, and remove the visible and obvious impurities. Then primary crushing of illite ore is carried out by jaw crusher to obtain illite ore powder.
2)將步驟1)獲得的800g伊利石原礦粉和200g水混合得到混合物料，採用濕式球磨機進行球磨8小時，球磨完畢後將混合物料通過旋流分離器進行旋流分離，進料流量為15m 3/h，得到初級懸浮液。 2) 800g of illite ore powder obtained in step 1) was mixed with 200g of water to obtain a mixture, and a wet ball mill was used to perform ball milling for 8 hours. After the ball milling, the mixture was cyclone separated by a cyclone, and the feed flow was 15 m 3 /h to obtain a primary suspension.
3)將步驟2)獲得的初級懸浮液進行初級沉澱1天，懸浮液分層，通過負壓抽吸將懸浮液中的上層液體抽吸出來，即分離得到二級懸浮液。3) The primary suspension obtained in step 2) is subjected to primary precipitation for 1 day, the suspension is layered, and the upper layer liquid in the suspension is sucked out by negative pressure suction, that is, the secondary suspension is obtained by separation.
4)將步驟3)獲得的得到二級懸浮液置於不同壓力的高壓均質機內進行高壓均質迴圈處理三次，然後進行二次沉澱72小時；然後將懸浮液中上層清液抽吸出來進行蒸發處理，以蒸發多餘水分，使得產品的水分含量保持在30%~40%之間，再對產品進行滅菌處理後密封保存，得到高純度的伊利石。4) the obtained secondary suspension obtained in step 3) is placed in the high-pressure homogenizer of different pressures to carry out high-pressure homogenization loop treatment three times, and then secondary precipitation is carried out for 72 hours; Evaporation treatment is used 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 sealed and stored to obtain high-purity illite.
5)在密封保存的同時隨機取樣三批次伊利石，噴乾後獲得伊利石乾粉，檢測樣品的伊利石乾粉純度。5) Three batches of illite are randomly sampled while being sealed and preserved, and dry illite powder is obtained after spray-drying, and the purity of the dry illite powder of the sample is tested.
本實施例4對步驟4)中，高壓均質處理的壓力對伊利石粒徑的影響進行探究，保持其他條件不變，改變高壓均質處理的壓力，重複進行上述步驟。每次重複進行三次實驗，計算得到平均粒徑。結果如表3所示，隨著均質壓力從100Bar增加到300Bar，伊利石的平均粒徑從401.35nm減小至332.64nm，呈現出隨壓力增大而減小的趨勢。但是當壓力為200Bar時，伊利石的平均粒徑即為342.52nm。
表3
進一步地，測試高壓均質處理的壓力為200Bar時製得的伊利石的粒徑分佈進行檢測，結果如圖3所示，圖中，縱坐標為粒徑大小(nm），橫坐標表示為相對強度。從圖中可以得知，伊利石的粒徑分佈範圍為198.55nm~434.81nm，且集中分佈在266.4nm~357.43nm之間，分佈範圍相對比較集中。Further, the particle size distribution of the illite obtained when the pressure of the test high-pressure homogenization treatment was 200Bar was detected, and the results were as shown in Figure 3. In the figure, the ordinate is the particle size (nm), and the abscissa is expressed as the relative intensity. . It can be seen from the figure that the particle size distribution range of illite is 198.55nm~434.81nm, and the distribution is concentrated between 266.4nm~357.43nm, and the distribution range is relatively concentrated.
實施例5Example 5
1)從伊利石原礦中優選形態和品質較優的礦石，去除肉眼可見、明顯的雜質。然後採用顎式破碎機將伊利石原礦進行初級破碎，獲得伊利石原礦粉。1) Select the ore with better shape and quality from the illite ore, and remove the visible and obvious impurities. Then primary crushing of illite ore is carried out by jaw crusher to obtain illite ore powder.
2)將步驟1)獲得的800g伊利石原礦粉和200g水混合得到混合物料，採用濕式球磨機進行球磨8小時，球磨完畢後將混合物料通過旋流分離器進行旋流分離，進料流量為20m 3/h，得到初級懸浮液。 2) 800g of illite ore powder obtained in step 1) was mixed with 200g of water to obtain a mixture, and a wet ball mill was used to perform ball milling for 8 hours. After the ball milling, the mixture was cyclone separated by a cyclone, and the feed flow was 20 m 3 /h to obtain a primary suspension.
3)將步驟2)獲得的初級懸浮液進行初級沉澱1天，懸浮液分層，通過負壓抽吸將懸浮液中的上層液體抽吸出來，即分離得到二級懸浮液。3) The primary suspension obtained in step 2) is subjected to primary precipitation for 1 day, the suspension is layered, and the upper layer liquid in the suspension is sucked out by negative pressure suction, that is, the secondary suspension is obtained by separation.
4)將步驟3)獲得的得到二級懸浮液置於壓力為200Bar的高壓均質機內進行高壓均質迴圈處理三次，然後進行二次沉澱；然後將懸浮液中上層清液抽吸出來進行蒸發處理，以蒸發多餘水分，使得產品的水分含量保持在30%~40%之間，再對產品進行滅菌處理後密封保存，得到高純度的伊利石。4) The obtained secondary suspension obtained in step 3) is placed in a high-pressure homogenizer with a pressure of 200Bar to carry out high-pressure homogenization loop treatment three times, and then secondary precipitation; then the supernatant in the suspension is sucked out and evaporated Treatment is 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 sealed and stored to obtain high-purity illite.
5)在密封保存的同時隨機取樣三批次伊利石，噴乾後獲得伊利石乾粉，檢測樣品的伊利石乾粉純度。5) Three batches of illite are randomly sampled while being sealed and preserved, and dry illite powder is obtained after spray-drying, and the purity of the dry illite powder of the sample is tested.
本實施例5對步驟4)中，二次沉澱的時間對伊利石純度的影響進行探究，保持其他條件不變，改變二次沉澱的時間，重複進行上述步驟。結果如圖4所示，圖中縱坐標表示製得的伊利石的純度，橫坐標表示二次沉澱的沉澱時間（天(d)）。In this Example 5, in step 4), the influence of the time of secondary precipitation on the purity of illite was explored, other conditions were kept unchanged, the time of secondary precipitation was changed, and the above steps were repeated. The results are shown in Figure 4, where the ordinate represents the purity of the prepared illite, and the abscissa represents the precipitation time (day (d)) of the secondary precipitation.
對比例1Comparative Example 1
對比例1與實施例5中二次沉澱的時間為3天時的實施例基本相同，不同之處在於：對比例1中步驟4）中採用球磨法對到二級懸浮液進行破碎。Comparative Example 1 is basically the same as Example 5 when the secondary precipitation time is 3 days, the difference is that in step 4) in Comparative Example 1, the secondary suspension is crushed by ball milling.
結果表明，獲得的伊利石的純度為90.5%；分佈範圍為800nm~1700nm，且集中分佈在1050nm~1580nm之間，粒徑分佈不集中。The results show that the purity of the obtained illite is 90.5%; the distribution range is 800nm~1700nm, and the distribution is concentrated between 1050nm~1580nm, and the particle size distribution is not concentrated.
以上所述實施例的各技術特徵可以進行任意的組合，為使描述簡潔，未對上述實施例中的各個技術特徵所有可能的組合都進行描述，然而，只要這些技術特徵的組合不存在矛盾，都應當認為是本說明書記載的範圍。The technical features of the above-described embodiments can be combined arbitrarily. For the sake of brevity, all possible combinations of the technical features in the above-described embodiments are not described. However, as long as there is no contradiction between the combinations of these technical features, All should be regarded as the scope described in this specification.
以上所述實施例僅表達了本申請的幾種實施方式，其描述較為具體和詳細，但並不能因此而理解為對申請專利範圍的限制。應當指出的是，對於本領域的普通技術人員來說，在不脫離本申請構思的前提下，還可以做出若干變形和改進，這些都屬於本申請的保護範圍。因此，本申請專利的保護範圍應以所附權利要求為准。The above-mentioned embodiments only represent several embodiments of the present application, and the descriptions thereof are relatively specific and detailed, but should not be construed as a limitation on the scope of the patent application. It should be pointed out that for those skilled in the art, without departing from the concept of the present application, several modifications and improvements can be made, which all belong to the protection scope of the present application. Therefore, the scope of protection of the patent of the present application shall be subject to the appended claims.
圖1為實施例1中不同物料固含量下的磨礦效率圖；
圖2為實施例3中的不同初級沉澱時間下製得的伊利石的純度圖；
圖3為實施例4中高壓均質處理的壓力為200Bar時制得的伊利石的粒徑分佈圖；
圖4為實施例5中的不同二級沉澱時間下製得的伊利石的純度圖。
Fig. 1 is the grinding efficiency figure under different material solid content among the
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| CN2132562Y (en) * | 1992-07-08 | 1993-05-12 | 中国矿业大学 | Super-fine homogenizer |
| CN101016157A (en) * | 2006-02-09 | 2007-08-15 | 浙江海力生制药有限公司 | Method of purifying montmorillonite, purified montmorillonite and composition thereof |
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| KR101426891B1 (en) * | 2012-12-20 | 2014-08-05 | (주)세영씨앤티 | Manufacturing method of illite nanoparticles |
| KR101332268B1 (en) * | 2013-01-23 | 2013-11-22 | 주식회사 다솔 | Cosmetic composition containing illite and manufacturing method |
| KR101629299B1 (en) * | 2013-05-31 | 2016-06-13 | 주식회사 케미랜드 | Powder coated with vegetable butter or fat-soluble vitamin C derivatives and cosmetic composition containing the same |
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| CN105878062A (en) * | 2014-12-27 | 2016-08-24 | 延吉兆意博士创业科技有限公司 | Illite beauty facial mask and manufacturing method thereof |
| CN106269215B (en) * | 2016-07-26 | 2018-11-13 | 长春工业大学 | A method of illite powder is produced by illite clay mine |
| CN106580756B (en) * | 2016-12-21 | 2019-06-07 | 湖南御家化妆品制造有限公司 | Mineral hot spring water and preparation method and application thereof |
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| CN111204774B (en) * | 2020-01-19 | 2022-10-18 | 延边大学 | Method for preparing submicron illite dry powder particles by improving illite dispersion degree |
| CN112125314B (en) * | 2020-09-21 | 2021-07-30 | 湖南御家化妆品制造有限公司 | Illite and preparation method and application thereof |
-
2020
- 2020-09-21 CN CN202010995075.3A patent/CN112125314B/en active Active
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2021
- 2021-03-23 WO PCT/CN2021/082384 patent/WO2022057227A1/en active Application Filing
- 2021-03-23 AU AU2021342988A patent/AU2021342988B2/en active Active
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| AU2021342988A1 (en) | 2022-12-01 |
| CN112125314A (en) | 2020-12-25 |
| CN112125314B (en) | 2021-07-30 |
| WO2022057227A1 (en) | 2022-03-24 |
| CA3180986A1 (en) | 2022-03-24 |
| AU2021342988B2 (en) | 2023-11-09 |
| TWI784528B (en) | 2022-11-21 |
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