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公开(公告)号：US20160002061A1
公开(公告)日：2016-01-07
申请号：US14648425
申请日：2013-11-28
Inventor： Xiaojun Bao , Yuanyuan Yue , Tiesen Li , Haiyan Liu , Shengbao He , Jianning Yu
IPC: C01B39/40
CPC classification number: C01B39/40 , B01J20/18 , B01J29/40 , B01J35/002 , C01B39/38
Abstract: The present invention pertains to the field of molecular sieve synthesis, and relates to a synthesis method of ZSM-5 type molecular sieves. In this method, natural minerals, i.e., natural kaolin and natural diatomite, are used as the total silicon source and aluminum source required for the molecular sieve synthesis, and these two natural minerals are calcinated and subjected to acidic (alkaline) treatment before they are mixed at a certain ratio, and then crystallized under hydrothermal conditions to obtain the product, a ZSM-5 type molecular sieve. The ZSM-5 type molecular sieve obtained by the method according to the present invention is a hierarchical porous material having a crystallinity of 70% to 120% as compared to conventional ZSM-5 type molecular sieves synthesized by using pure chemical reagents, and the silica-to-alumina ratio in the molecular sieve product may be adjusted by varying the ratio of the two minerals in the raw materials for the synthesis. According to the present invention, the range of raw materials for the preparation of molecular sieve materials is broadened, and therefore not only the cost for the molecular sieve production is greatly reduced but also the greenness in the production process of the molecular sieve material is significantly improved.
Abstract translation: 本发明涉及分子筛合成领域，涉及ZSM-5型分子筛的合成方法。 在这种方法中，使用天然矿物，即天然高岭土和天然硅藻土作为分子筛合成所需的总硅源和铝源，并将这两种天然矿物煅烧并进行酸性（碱性）处理，然后再处理 以一定比例混合，然后在水热条件下结晶，得到ZSM-5型分子筛。 与通过使用纯化学试剂合成的常规ZSM-5型分子筛相比，通过本发明的方法获得的ZSM-5型分子筛是结晶度为70％〜120％的分级多孔材料，二氧化硅 可以通过改变合成原料中两种矿物的比例来调节分子筛产物中的氧化铝比。 根据本发明，用于制备分子筛材料的原料的范围变宽，因此不仅分子筛生产的成本大大降低，而且分子筛材料的生产过程中的绿色显着 改进。
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公开(公告)号：US11426702B2
公开(公告)日：2022-08-30
申请号：US17006723
申请日：2020-08-28
Applicant: CHINA UNIVERSITY OF PETROLEUM-BEIJING
Inventor： Chunmao Chen , Zhichang Liu , Zhongjin Yi , Rui Zhang , Jiahao Liang , Xianghai Meng , Haiyan Liu , Chunming Xu , Qinghong Wang
IPC: C02F9/00 , C02F11/122 , C04B5/00 , C02F11/16 , B01J19/20 , C02F11/13 , C10G53/04 , C02F11/12 , C02F1/52 , C02F1/56 , C02F1/66 , C02F11/127 , C02F1/00 , C02F103/36 , C02F11/121
Abstract: A method and a system for treatment of a spent chloroaluminate ionic liquid catalyst and an alkaline wastewater, where the method includes: 1) mixing the catalyst with a concentrated brine for hydrolysis reaction until residual activity of the catalyst is completely eliminated, to obtain an acidic hydrolysate and an acid-soluble oil; 2) mixing the acidic hydrolysate with an alkaline solution containing the alkaline wastewater for neutralization reaction until this reaction system becomes weak alkaline, to obtain a neutralization solution; 3) fully mixing the neutralization solution with a flocculant, carrying out sedimentation and separation, collecting the concentrated brine at an upper layer for reuse in the hydrolysis reaction, and collecting concentrated flocs at a lower layer; 4) dehydrating the concentrated flocs to obtain concentrated brine for reuse into the hydrolysis reaction, and collecting a wet solid slag; and 5) drying the wet solid slag to obtain a dry solid slag.
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公开(公告)号：US10822242B2
公开(公告)日：2020-11-03
申请号：US16525503
申请日：2019-07-29
Applicant: CHINA UNIVERSITY OF PETROLEUM—BEIJING
Inventor： Haiyan Liu , Tao Zheng , Zhichang Liu , Xianghai Meng , Rui Zhang , Chunming Xu
Abstract: The present application provides a ZSM-35 molecular sieve and a preparation method thereof. The ZSM-35 molecular sieve is an aggregated ZSM-35 molecular sieve having a hierarchical macro-meso-microporous pore structure. Raw materials for the preparation method do not include an organic template agent and a crystal seed, and the preparation method includes the following steps: preparing a reactant gel where a molar ratio of SiO2, Al2O3, Na2O, K2O, oxygen-containing acid radical and H2O is (20-40):1.0:(1.5-2.0):(4.0-6.5):(1.0-4.0):(600-1200); sequentially performing an aging treatment and a crystallization treatment on the reactant gel, washing and drying a resulting synthetic product. The ZSM-35 molecular sieve provided by the present application may be obtained by synthesizing without using an organic template agent and crystal seed, and because it has a hierarchical pore structure, it is favorable for material diffusion and mass transfer.
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4.发明授权公开(公告)号：US10758894B2
公开(公告)日：2020-09-01
申请号：US16237857
申请日：2019-01-02
Applicant: China University of Petroleum-Beijing
Inventor： Haiyan Liu , Lina Zhang , Xiaojun Bao
IPC: B01J29/00 , B01J29/85 , B01J29/40 , B01J21/04 , B01J21/12 , B01J21/08 , B01J37/00 , B01J37/30 , B01J35/08 , B01J35/02 , B01J37/02 , B01J37/06 , B01J37/04 , B01J37/08 , B01J37/03 , C07C1/24 , B01J21/16
Abstract: The present invention relates to a composite catalytic material of SAPO-34/ZSM-5@kaolin microspheres and its preparation and use, the method comprises the steps of: 1) processing kaolin into kaolin microspheres, and baking them to obtain activated kaolin microspheres; 2) mixing the activated kaolin microspheres obtained in step 1), water, a phosphorus source, and a template agent to prepare a gel; 3) mixing the gel obtained in step 2) and a ZSM-5 molecular sieve, and carrying out aging, crystallization, and separation to obtain a composite material of SAPO-34/ZSM-5@kaolin; 4) subjecting the composite material obtained in step 3) to ammonium exchange treatment and baking, to obtain the composite catalytic material of SAPO-34/ZSM-5@kaolin microspheres. The present invention not only greatly shortens the preparation route for the catalyst and reduces the cost of catalyst preparation, but also allows adjustment of the fractions of SAPO-34 and ZSM-5 molecular sieves in the composite material by adjustment of the synthesis conditions.
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Patent Agency Ranking
5.发明授权公开(公告)号：US11634334B2
公开(公告)日：2023-04-25
申请号：US17037409
申请日：2020-09-29
Applicant: CHINA UNIVERSITY OF PETROLEUM-BEIJING
Inventor： Tao Zheng , Haiyan Liu , Zhichang Liu , Xianghai Meng , Rui Zhang , Chunming Xu
IPC: C01B39/44
Abstract: The present disclosure provides a method of synthesizing an aluminosilicate molecular sieve by a crystal seed-assisted method, a natural aluminosilicate clay mineral treated and activated by an alkali is used as a crystal seed for synthesis of the aluminosilicate molecular sieve, and the target molecular sieve product is synthesized by hydrothermal crystallization, wherein the synthesis process does not require addition of conventional crystal seeds of a molecular sieve or use of any organic template agent, thus the synthesized product does not require a calcination process to remove the template agent. The method of synthesizing an aluminosilicate molecular sieve by a crystal seed-assisted method can meet the requirements of both crystallinity and nucleation time, and greatly reduce costs of synthesizing the aluminosilicate molecular sieve, and reduce the environmental pollution caused by removal of the template agent by calcinating.
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6.发明申请公开(公告)号：US20190224652A1
公开(公告)日：2019-07-25
申请号：US16237857
申请日：2019-01-02
Applicant: China University of Petroleum-Beijing
Inventor： Haiyan Liu , Lina Zhang , Xiaojun Bao
IPC: B01J29/00 , B01J21/16 , B01J29/85 , B01J29/40 , B01J21/04 , B01J21/12 , B01J21/08 , B01J37/00 , B01J37/30 , B01J35/08 , B01J35/02 , B01J37/02 , B01J37/06 , B01J37/04 , B01J37/08 , B01J37/03 , C07C1/24
Abstract: The present invention relates to a composite catalytic material of SAPO-34/ZSM-5@kaolin microspheres and its preparation and use, the method comprises the steps of: 1) processing kaolin into kaolin microspheres, and baking them to obtain activated kaolin microspheres; 2) mixing the activated kaolin microspheres obtained in step 1), water, a phosphorus source, and a template agent to prepare a gel; 3) mixing the gel obtained in step 2) and a ZSM-5 molecular sieve, and carrying out aging, crystallization, and separation to obtain a composite material of SAPO-34/ZSM-5@kaolin; 4) subjecting the composite material obtained in step 3) to ammonium exchange treatment and baking, to obtain the composite catalytic material of SAPO-34/ZSM-5@kaolin microspheres. The present invention not only greatly shortens the preparation route for the catalyst and reduces the cost of catalyst preparation, but also allows adjustment of the fractions of SAPO-34 and ZSM-5 molecular sieves in the composite material by adjustment of the synthesis conditions.
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公开(公告)号：US10287172B2
公开(公告)日：2019-05-14
申请号：US15527969
申请日：2014-11-19
Inventor： Xiaojun Bao , Yuanyuan Yue , Jinbiao Yang , Haiyan Liu , Pei Yuan
Abstract: The present invention provides a preparation method of Beta molecular sieve, comprising: activating a mineral having low silica-to-alumina ratio and a mineral having high silica-to-alumina ratio, respectively, wherein the mineral having low silica-to-alumina ratio is activated via a sub-molten salt medium, and the mineral having high silica-to-alumina ratio is activated via means of high-temperature calcination; mixing the activated minerals with sodium chloride, potassium chloride, water and template agent for hydrothermal crystallization, wherein the charged amounts of the raw materials satisfies a molar ratio of: 0.03-0.18 Na2O: 0.01-0.03 K2O: 0.1-0.4 (TEA)2O: 1 SiO2: 0.01-0.5 Al2O3: 12-40 H2O; cooling the crystallized product and removing the mother liquor by filtration, washing the resulting filter cake with water to neutral and drying it to obtain the Beta molecular sieve.
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公开(公告)号：US09963350B2
公开(公告)日：2018-05-08
申请号：US14648425
申请日：2013-11-28
Inventor： Xiaojun Bao , Yuanyuan Yue , Tiesen Li , Haiyan Liu , Shengbao He , Jianning Yu
CPC classification number: C01B39/40 , B01J20/18 , B01J29/40 , B01J35/002 , C01B39/38
Abstract: The present invention pertains to the field of molecular sieve synthesis, and relates to a synthesis method of ZSM-5 type molecular sieves. In this method, natural minerals, i.e., natural kaolin and natural diatomite, are used as the total silicon source and aluminum source required for the molecular sieve synthesis, and these two natural minerals are calcinated and subjected to acidic (alkaline) treatment before they are mixed at a certain ratio, and then crystallized under hydrothermal conditions to obtain the product, a ZSM-5 type molecular sieve. The ZSM-5 type molecular sieve obtained by the method according to the present invention is a hierarchical porous material having a crystallinity of 70% to 120% as compared to conventional ZSM-5 type molecular sieves synthesized by using pure chemical reagents, and the silica-to-alumina ratio in the molecular sieve product may be adjusted by varying the ratio of the two minerals in the raw materials for the synthesis. According to the present invention, the range of raw materials for the preparation of molecular sieve materials is broadened, and therefore not only the cost for the molecular sieve production is greatly reduced but also the greenness in the production process of the molecular sieve material is significantly improved.
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公开(公告)号：US09845249B2
公开(公告)日：2017-12-19
申请号：US14902423
申请日：2013-12-02
Applicant: China University of Petroleum-Beijing
Inventor： Haiyan Liu , Xinyan Sun , Xiaojun Bao , Gang Shi
IPC: C01B39/26
CPC classification number: C01B39/265 , C01B39/26
Abstract: The present invention provides a method for preparing a mordenite, which is a method for preparing the mordenite through a hydrothermal crystallization by using natural aluminosilicate minerals as total silicon sources and total aluminum sources, comprising the steps of: subjecting the natural aluminosilicate minerals to activation treatment which is an activation by sub-molten salt and an activation by thermal treatment; selecting and mixing the activated natural aluminosilicate minerals according to the silicon-to-aluminum ratio of the targeted mordenite, adding thereto deionized water, sodium hydroxide, crystal seed, a templating agent to obtain a reaction mixture; adjusting the reaction mixture by using an inorganic acid to have a pH of 10-13, and then aging it at 40-80° C. for 6-24 hours; and subjecting the aged reaction mixture to hydrothermal crystallization, and then filtering, washing, drying and calcinating the crystallized product to obtain the mordenite. The method for preparing a mordenite provided in the present invention enlarges the sources of raw materials for a molecular sieve, has a low cost and a simple process route, and can largely reduce the cost for synthesizing a molecular sieve.
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