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化学进展 2020, Vol. 32 Issue (8): 1017-1048 DOI: 10.7536/PC200428 前一篇   后一篇

• 综述 •

凝聚态化学的研究对象与主要科学问题

徐如人1,**(), 于吉红1, 闫文付1   

  1. 1. 吉林大学无机合成与制备化学国家重点实验室 化学学院 长春 130012
  • 收稿日期:2020-04-01 修回日期:2020-04-22 出版日期:2020-08-24 发布日期:2020-04-23
  • 通讯作者: 徐如人
  • 基金资助:
    国家自然科学基金项目(U1967215); 国家自然科学基金项目(21835002); 国家自然科学基金项目(21621001)
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Goals and Major Scientific Issues in Condensed Matter Chemistry

Ruren Xu1,**(), Jihong Yu1, Wenfu Yan1   

  1. 1. State Key Laboratory of Inorganic Synthesis and Preparative Chemistry, College of Chemistry, Jilin University, Changchun 130012, China
  • Received:2020-04-01 Revised:2020-04-22 Online:2020-08-24 Published:2020-04-23
  • Contact: Ruren Xu
  • About author:
    ** e-mail:
  • Supported by:
    the National Natural Science Foundation of China(U1967215); the National Natural Science Foundation of China(21835002); the National Natural Science Foundation of China(21621001)

本文提出了“凝聚态化学(Condensed Matter Chemistry)”的概念,提出其研究对象是由传统化学上被视为反应主体的原子、离子以及分子等“基本粒子”,藉“稳定的粘连关系”凝聚形成的具有特定组成、多层次结构与性质、功能的物质凝聚态。本文以固态为例,讨论了(1)凝聚态的多层次结构;(2)凝聚态的化学性质与化学反应;(3)凝聚态构筑化学中的前沿科学问题;(4)凝聚态化学中的高新表征方法与技术的发展与开拓。并对四个领域中的主要科学问题进行了比较深入的探讨,为进一步再认识传统化学,特别是对其中心问题,即化学反应的再认识提供了方向与基础,为开展“凝聚态的多层次结构-化学性质与化学反应-凝聚态物质的构筑定向合成与精准制备”三个方面的关系研究,总结规律与“分态”建立“凝聚态结构理论”与“凝聚态化学反应理论”,建设“凝聚态化学”提供了科学体系与内容,并为进一步开展“凝聚态工程学”研究提供了前提与基础。

关键词： 凝聚态, 固态, 多层次结构, 化学反应, 催化, 构筑, 表征

The concept of condensed matter chemistry is proposed as a new scientific discipline. It studies the composition, the multi-level structure, properties and chemical reactions of matters in condensed states formed via stable adhesions. This compares to the classical chemistry, which studies more localized issues, namely the properties of basic particles like atoms, ions and molecules and their electron-moving reactions. In this article, we use examples from solid state matters to illustrate cutting-edge research issues related to(1) the multi-level structures,(2) chemical properties and reactions,(3) constructive chemistry, and(4) novel characterization techniques of condensed matters. In-depth discussions regarding key scientific questions of the new discipline are presented, to set a stage enabling us to reexamine the core scientific issues in the classical chemistry, namely chemical reactions, in the new and larger context and to study the relationships among multi-level structures of condensed matters, chemical properties and reactions, and construction rational synthesis and precision preparation for materials in condensed matter states. The goals are to develop theories of “condensed matter organization” and “chemical reactions”, leading to the full development of the science of condensed matter chemistry as well as condensed matter engineering.

Contents

1 Goals of condensed matter chemistry

2 Major scientific issues in condensed matter chemistry

2.1 Multi-level structures of condensed matter

2.2 Chemical properties and chemical reactions of condensed matter

2.2.1 Chemical reactions in multilevel structured atomic(ionic) crystalline matter

2.2.2 Chemical reactions in molecular crystalline coordination compounds

2.2.3 Chemical reactions in isomeric atomic crystal solid matter

2.2.4 Properties and chemical reactions in allotropes of(molecular and atomic crystals) solid matter

2.2.5 “State” - “state” reactions in atomic(ionic) and molecular crystals in solid matter

2.2.6 Chemical reactions between organic solid matter

2.2.7 Chemical reactions of crystalline polymorphs and amorphous forms in solid matter

2.2.8 Influence of multi-level structure on catalysis in solid matter

2.2.9 Influence of crystal intergrowth on catalysis in crystalline solid matter

2.2.10 Influence of polymorphs on catalysis in crystalline solid matter

2.3 Emerging scientific issues in the constructive chemistry of condensed matter

2.4 State-of-the-art characterization techniques for condensed matter

3 Conclusion and outlook

Key words: condensed state, solid state, multi-level structure, chemical reaction, catalysis, construction, characterization
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图1 铁-氧相图的一部分(垂直虚线相应于化学计量组成FeO)[5]
Fig.1 Part of phase diagram of Fe-O(Dashed line indicates the stoichiometric composition of FeO)[5]
表1 Pr n O2 n -2组成和稳定范围[8]
Table 1 Composition of Pr n O2 n -2 at varied temperatures[8]
Oxide n x in PrOx n at T/K T/K
Pr4O6(Pr2O3) 4 1.500 1.500~1.503 1273
Pr7O12(l) 7 1.714 1.713~1.719 973
Pr9O16(ζ) 9 1.778 1.776~1.778 773
Pr5O9(ε) 10 1.800 1.779~1.801 723
Pr11O20(δ) 11 1.818 1.817~1.820 703
Pr6O11(β) 12 1.833 1.831~1.836 673
表2 纳米金催化剂原粉中金颗粒的担载量和表面积[33]
Table 2 Loading and surface area of As-synthesized catalysts[33]
TiO2 support type Synthesis loading ICP loading(%) XANES loading(%) Surface area (m2/g) Au areal density in units of(111) monolayers a
anatase 13 13 10.0 b 225 0.12
anatase 6 5.2 n/a 225 0.051
anatase 3 2.8 n/a 225 0.027
brookite 13 3.3 2.7 b 106 0.069
rutile 13 14 11.9 b 77 0.39
rutile 6 2.9 n/a 77 0.083
P25 13 5.7 4.1 b 47 0.27
P25 13 7.2 8 47 0.34
P25 6.5 4.5 5 47 0.21
图2 包含空位对的链状M7O12 结构(6配位金属立方体可表示为MO6(Vo)2)[8]
Fig.2 Chain-like structure of M7O12 containing vacancy pair(octahedrally coordinated metal atom is presented as MO6(Vo)2)[8]
图3 在体心立方的c型氧化物中金属链沿所有(111)轴的交织堆积[8]
Fig.3 Alternative stacking of metal chain along all(111) axes in c-type cubic-centered oxides[8]
图4 KBrO3在等离子体和热作用下的分解反应(1)和(2)的反应温度与反应ΔG的关系[9]
Fig.4 The dependence of the ΔG on the temperature of the reactions (1) and (2)[9]
图5 晶体固态MBrO3的机械化学分解:1-NaBrO3, 2-KBrO3, 3-CsBrO3, 4-RbBrO3 [9]
Fig.5 Mechanochemical decomposition of MBrO3, 1-NaBrO3, 2-KBrO3, 3-CBrO3, 4-RbBrO3 [9]
图6 稀土二元硫族化合物的晶胞常数[10]
Fig.6 Lattice constant for the mono-chalcogenides of the rare earth elements[10]
图7 沿b轴的一维链状配位聚合物[Fe(μ-atrz)(atrz)2(H2O)2]·4H2O(BF4)2(平衡阴离子和水分子已略去)脱水形成三维[Fe(μ-atrz)3(BF4)2]框架结构[14, 15]
Fig.7 The formation of 3D framework of [Fe(μ-atrz)3(BF4)2] by the linear 1D chain coordination polymer of [Fe(μ-atrz)(atrz)2(H2O)2]·4H2O(BF4)2 along the b-axis(counter anions, water molecules in the lattice and hydrogen atoms are omitted) via dehydration[14, 15]
图8 (a) 催化剂原粉活性:P25>锐钛矿>金红石>板钛矿;(b) 在8%O2-He气氛下300 ℃处理30 min后催化剂活性[33]
Fig.8 CO oxidation activity over Au-TiO2 catalysts with different supports:(a) from the as-synthesized sample;(b) following treatment in 8% O2-He pretreated at 573 K for 30 min[33]
图9 SiO2相变和稳定度[37]
Fig.9 Phase transition of SiO2 at ambient pressure[37]
图10 BaO和SiO2的反应相图[38]
Fig.10 Phase diagram of BaO and SiO2 [38]
图11 黑磷的结构:(a)正交黑磷,(b)斜方黑磷,(c)立方黑磷[39]
Fig.11 Structure of black phosphorus:(a) orthorhombic,(b) rhombohedral, and(c) cubic black phosphorus[39]
图12 TiO2摩尔含量>60%的BaO-TiO2相图[40, 41]
Fig.12 Phase relations in the BaO-TiO2 system for compositions with > 60 % mole fraction TiO2. Abbreviations and symbols used include: BT(BaTiO3); B6T17(Ba6Ti17O40); B4T13(Ba4Ti13O30); BT4(BaTi4O9); B2T9(Ba2Ti9O20); L(liquid);(·) solid phases, quenched;(o) melted, quenched[40, 41]
图13 三元交互体系Ag,Pb‖Cl,Br[42]
Fig.13 Diagonal cross section of triternary mutual system Ag,Pb‖Cl,Br-liquidus[42]
图14 三元交互体系K,Na‖Cl,SO4-liquids[43]
Fig.14 Diagonal cross section of triternary mutual system K,Na‖Cl,SO4-liquids[43]
表3 三元交互体系K,Na‖Cl,SO4对角线上的组成、温度与固相[43]
Table 3 Diagonal cross section of triternary mutual system K,Na‖Cl,SO4 liquidus[43]
%
(KCl)2 		t° Твердые
Фазы		 %
(KCl)2 		t° Твердые
Фазы		 %
(KCl)2 		t° Твердые
Фазы
0 884 Na2SO4 25 624 ФазаX* 40 532 ФазаX*
5 824 ″ 27 608 ″ 45 540 KCl
10 772 ″ 30 594 ″ 50 564 ″
15 718 ″ 33 578 ″ 55 588 ″
18 690 ″ 36 560 ″ 65 635 ″
21 662 ″ 38 548 ″ 70 682 ″
表4 三元交互体系K,Na‖Cl,SO4复分解反应的二元低共融点[43]
Table 4 Nonvarint point and solid phase in(KCl)2-Na2SO4 [43]
t° %(KCl)2 Tвepдыe Фaзы
624 24.6 Na2SO4,Фaзa X
525 41.5 KCl,Фaзa X
表5 三元交互体系K,Na‖Cl,SO4的三元低共融点[43]
Table 5 Eutectic temperature and composition, solid phase in(KCl)2-Na2SO4 [43]
Обозна-
чення нарнс.270		 t° %W Твердые Фазы
(KCl)2 (NaCl)2 Na2SO4 K2SO4
P1 534 25.5 13.5 61 - Na2SO4,Фаза X,NaCl
E 514 39 2.5 58.5 - NaCl,
Фаза X,KCl
P2 538 41.5 - 53 5.5 KCl,Фаза X,K2SO4
表6 第一列过渡金属在高氧压条件下不常见氧化态的稳定性[47]
Table 6 Stabilization of unusual oxidation states of transition metals of the first raw under high oxygen pressures[47]
Element Oxidation state Electronic configuration Oxide
Cr Cr(Ⅴ) t 2 g 2 e g 0 La2LiV1- x Cr x O6
Fe Fe(Ⅳ) t 2 g 3 d z 2 1 d x 2 - y 2 0 A0.5La1.5Li0.5Fe0.5O4
A=Ca, Sr, Ba
(SrLa)M0.5Fe0.5O4
M=Mg, Zn
Fe Fe(Ⅴ) t 2 g 3 e g 0 La2LiFeO6
Co Co(Ⅲ) LS→HS
LS→HS		 LnCoO3
(Ln=La→Lu)
SrLnCoO4
Co Co(Ⅳ) t 2 g 6 e g 0 (Sr0.5La1.5)Li0.5Co0.5O4
Ni Ni(Ⅲ) t 2 g 6 σ * 1 LnNiO3(Ln=La→Lu)
SrLnNiO4
Cu Cu(Ⅳ) t 2 g 6 d z 2 2 d x 2 - y 2 2
t 2 g 6 σ * 2 		La2Li0.5Cu0.5O4
LaCuO3
SrLaCuO4
图15 BaFeO3- x 的生成相图。加点的区域是BaFeO3- x 的高温和低温形式纯相形成区域。氧等压线为空心圆圈所标直线,破折线表示为推测的关系[46]
Fig.15 Phase relations involving BaFeO3- x . Stippled areas are single-phase regions for high- and low-temperature forms of BaFeO3- x . Oxygen isobars are shown as light lines with experimental points as open circles. Dashed lines indicate inferred relations[46]
图16 cis-[Pt(NO3)2(en)2](1b)与4,4'-bpy(2) 的固体和cis-[Pd(NO3)2(en)2](1a)与三嗪基配体(4)的固体通过室温固相研磨制备超分子材料[56, 57]
Fig.16 Preparation of supramolecular materials via grinding the mixture of cis-[Pt(NO3)2(en)2](1b) and 4,4'-bpy(2) and cis-[Pd(NO3)2(en)2](1a) and triazine based ligand(4) at ambient temperature[56, 57]
表7 固态反应类型[59]
Table 7 Solid-state reaction types[59]
Inclusion reactions
Condensation of carbonyls
Electron transfers
Cycloadditions
Proton transfers
Cycloreversions
Oxygen transfers
Substitutions with RX
Oxygenations
Aromatic substitutions
Hydrogenations
Cyclizations
Additions of RR’NH, H2O, ROH
Methylations
Additions of halogens and HX
Nitrations at N and C
Eliminations
Diazotizations
Rearrangement
Azocouplings
C-C bond formations
Sandmeyer reactions
Carboxylation with CO2
Cascade reactions
表8 固相反应定量合成一些亚胺类化合物[66]
Table 8 Quantitatively formed azomethines by solid-solid reaction[66]
Ar Ar’ Reaction condition Yield/(%)
4-MePh 4-ClPh 6 h, r.t. 100
4-BrPh 2 h, r.t. 100
4-NO2Ph 24 h, r.t. 100
4-HOPh 6 h, r.t. 100
4-MeOPh 4-ClPh 6 h, r.t. 100
4-BrPh 6 h, r.t. 100
4-NO2Ph 24 h, 50 ℃ 100
4-ClPh 4-HOPh 6 h, r.t. 100
4-HOPh 4-ClPh 24 h, r.t. 100
4-NO2Ph 4-ClPh 36 h, r.t. 100
图17 机械化学:富勒烯的反应[67]
Fig.17 Mechanochemistry: reactions of fullerene[67]
图18 三甲氧基苯45的固态和液态氧化反应的差异[68]
Fig.18 Difference in the oxidation of 45 by mechanochemical activation and in solution phase[68]
图19 (a) 扁桃体环磷胺“59”的固相合成;(b)从同样的化合物“58”出发,在液相中就得不到扁桃体环磷胺“59”[68]
Fig.19 (a) First synthesis of adamantoid cyclophosphazanes 59 facilitated by mechanochemical activation.(b) Initial unsuccessful attempts to prepare 59[68]
图20 由羧酸二聚合成子结合成的结构 (a)一维直线条带;(b)一维曲折条带;(c)二维层状;(d)三维骨架[69]
Fig.20 (a)One-dimensional linear tape and(b)crinkled(or zigzag) tape,(c) two dimensional sheet(or layer) and(d) three dimensional network(or framework) held together by the carboxylic acid dimer synthon[69]
图21 浓碱溶液中存在的硅酸根物种[72]
Fig.21 Aqueous silicate structures identified in concentrated alkaline solution. Each line in the stick figures represents a Si-O-Si(siloxane) linkage. Of these 48 structures, 41 contain multiple chemically distinct Si sites, making them amenable to characterization by29Si-29Si COSY NMR spectroscopy. All the structural assignments are definitive except for species 6B, 6C, and 7A, for which they were unable to resolve the various isomeric forms[72]
表9 不同模数R硅酸钠溶液中多硅酸根离子的存在状态与分布[71]
Table 9 Effect of silicate ratio on the percentage of SiO2 in a given silicate ion[71]
图式1 Pt/SiO2催化剂的浸渍还原制备过程[78]
Scheme 1 Pt/SiO2 catalyst prepared by direct reduction[78]
图式2 SMSI效应对Pt/SiO2催化丙烷脱氢活性的影响[78]
Scheme 2 The effect of SMSI on the catalytic behaviors of Pt/SiO2 catalysts in propane dehydrogenation[78]
图22 SMSI效应对Pt/SiO2催化丙烷脱氢活性的影响[78]
Fig.22 The effect of reduction temperature in a H2 atmosphere on the activity of Pt/SiO2 catalysts[78]
表10 Pt/SiO2催化剂的物理性质以及对CO的吸附值[78]
Table 10 Physical properties and CO adsorption values of Pt/SiO2 catalysts[78]
Catalyst Surface area/
m2·g-1 		Average particle sizea/nm Mass ratio of Pt:Si O 2 b CO adsorptionc/mmol·g-1
SiO2 325 - -
Pt/SiO2_773 K H2 340 2.4±1.2 3.5/96.5 54.9
Pt/SiO2_1073 K H2 320 2.2±0.9 3.9/96.1 40.3
Pt/SiO2_1273 K H2 217 3.2±1.1 4.1/95.9 not detectable
图23 氧化硅表面的悬空键≡Si·(E’s中心)模型(a),一个金属原子(Cu、Pd、Cs)吸附在悬空键上的结构模型≡Si-M(b)[79]
Fig.23 Cluster models of(a) a E’s center, ≡Si·, at the silica surface and(b) a metal atom(Cu, Pd, Cs) adsorbed on the E’s center, ≡Si-M[79]
图式3 用Mo掺杂的W18O49纳米管光催化固氮合成NH3·H2O的反应路径示意图[92]
Scheme 3 Proposed reaction pathway for photocatalytic N2 fixation to NH3·H2O using MWO-1 UTNWs as a catalyst[92]
图24 孔道拓扑结构图:(a)ZSM-5(MFI);(b) ZSM-11(MEL);(c) 与共生结构(比例可变)[106]
Fig.24 Topology of channels in(a) ZSM-5(MFI);(b) ZSM-11(MEL);(c) intergrowth of MFI and MEL with varied ratios[106]
图25 ZSM-5以及具有不同共生比例的ZSM-5/ZSM-11共生结构(共生相)的模拟XRD谱图(2θ角从6°到55°,未包括石英相的模拟XRD谱图)[107]
Fig.25 Simulated XRPD patterns for the evaluation of MFI/MEL contribution of ZSM-5, composite-a, -b and -c, from 6° to 55° 2 h(quartz phase was not included in the simulation)[107]
图26 ZSM-5以及具有不同共生比例的ZSM-5/ZSM-11共生结构(共生相)在MTP反应中的选择性[107]
Fig.26 Product selectivity of ZSM-5, composite-a, -b and -c. at 450 ℃ at a representative time on stream of 4 h. Propene is the dominant product. The product grouping was carried out in order to highlight the most relevant products in the MTA reaction. C4-C5 isomers: C4 are the 2-butene(cis and trans) and C5 are pentenes derivatives(1-, 2- and the corresponding cis and trans forms). C6-C8 isomers: comprises: hexene isomers, epatanes/eptenes, octanes/octanes with all their possible combinations of double bond in different position, cis and trans form and branched alkanes. C9+ isomers: include branched and unsaturated aromatics products either with alkyl chain or unsaturated branched substituents[107]
图27 ZSM-5以及具有不同共生比例的ZSM-5/ZSM-11共生结构(共生相)在MTP反应中对丙烯的选择性以及转化率[107]
Fig.27 Catalytic behaviour of: ZSM-5(squares), composite-a(circles), composite-b(triangles), and composite-c(diamonds) versus time on stream at 450 ℃. Filled and open symbols correspond to conversion and selectivity to propene respectively[107]
表11 MFI以及具有不同共生比例的ZSM-5/ZSM-11共生结构(共生相)的相对结晶度、孔容、比表面、晶粒尺寸以及Si/Al比[107]
Table 11 MFI and MEL contributions, relative crystallinity, micropore volume, surface area and crystallite size for ZSM-5, composite-a, -b and -c[107]
Material ZSM-5 ZSM-11 Relative crysrallinity Micropore volunm Surface area Crystallite size Si:Al ratio
MFI(%) MEL(%) (%) (mL·g-1) (m2·g-1) (μm)
ZSM-5 100 0 100 0.26 229 0.4 16
Composite-a 53 47 82 0.21 242 0.6 50
Composite-b 43 57 71 0.27 286 0.5 58
Composite-c 40 60 50 0.16 62 0.2 56
图28 EMT/FAU共生分子筛担载CoMo纳米催化剂精炼FCC汽油的辛烷值(右侧纵坐标)和硫含量(左侧纵坐标)[108]
Fig.28 The RON values and the sulfur contents of the hydrogenated gasoline products over different catalysts[108]
图29 EMT/FAU共生分子筛担载CoMo纳米催化剂精炼FCC汽油的异构化选择性[108]
Fig.29 The isomerization(ISO) selectivity over different catalysts[108]
图30 EMT/FAU共生分子筛担载CoMo纳米催化剂精炼FCC汽油的辛烷值和烯烃滞留率的关系[108]
Fig.30 The relationship of RON and the retentions of olefin over different catalysts[108]
表12 EMT/FAU共生分子筛担载CoMo纳米催化剂精炼FCC汽油结果[108]
Table 12 The hydro-upgrading results of FCC gasoline over different catalysts[108]
Items Catalyst series
Feedstock CoMo/AE-1 CoMo/AE-2 CoMo/AE-3 CoMo/AE-4 CoMo/AE-5 CoMo/AE-6 CoMo/AF CoMo/γ-Al2O3
Lumped composition of the liquid product(wt%)
n-Paraffin 6.0 12.5 11.1 13.8 10.7 11.2 11.1 11.4 13.0
i-Paraffin 36.6 47.1 47.8 50.8 51.3 52.7 48.6 43.3 47.3
Olefin 27.9 10.3 11.4 5.0 5.2 8.1 10.0 13.0 10.5
Naphthene 6.8 9.8 9.7 10.2 10.4 9.6 8.0 10.4 9.1
Aromatics 22.7 20.3 20.0 20.2 19.5 21.3 22.3 21.9 20.1
RON 90.2 88.6 88.9 87.9 88.5 89.7 89.3 90.1 88.0
ARON -1.6 -1.3 -2.3 -1.7 -0.5 -0.9 -0.1 -2.2
S(mg/L) 401 34.1 44.4 16.8 25.1 22.5 42.1 63.3 46.7
HDS(%) 91.5 88.9 96.1 93.7 94.6 89.5 84.2 88.3
图31 Beta沸石的多形体A、B和C的层堆积及孔道走向[109]
Fig.31 The projections and channel stacking sequences of polymorphs A, B, and C along the a or b direction: the 12-ring channel stacking sequences are ABAB...(a), ABCABC...(b) and AA...(c) types, respectively[109]
图32 Ti-β和Ti-ITQ-17对烯烃环氧化的催化活性[110]
Fig.32 Intrinsic activity of Ti-β and Ti-ITQ-17, expressed as turnover frequency number(mmol alkene converted/mmol Ti.h), on the epoxidation of different substrates with H2O2 [110]
表13 Ti-β and Ti-ITQ-17催化环己烯和正己烯环氧化结果[110]
Table 13 Cyclohexene and 1-hexene epoxidation over Ti-β and Ti-ITQ-17(Ti-PolC)[110]
Substrate catalyst Si/Ti Time Conversion % S % S % S % S
(min) (%of maximum) epoxide diola H2O2 TBHP
1-hexene Ti-β 59 45 20.1 97.0 2.6 89.9
1-hexene Ti-PolC 240 120 13 97.1 2.2 40.3
cyclohexene Ti-β 59 90 31.2 57.8 28.6 81.8
cyclohexene Ti-PolC 240 90 25.4 70.4 20.2 89.7
cyclohexeneb Ti-β 59 325 40.8 72.4 16.8 90.4
cyclohexeneb Ti-PolC 240 135 43.9 83.7 10.5 93.8
cyclohexene Ti-β 59 90 44.2 98.1 1.7 87.3
cyclohexene Ti-PolC 240 90 69.8 98.5 1.4 96.5
表14 Beta型沸石和ITQ-17的孔道尺寸以及由分子动力学计算的扩散系数[111]
Table 14 Channel sizes and diffusion coefficients obtained from the molecular dynamics[111]
Structure Channel size(Å) <100>a Diffusion coefficient
(106 cm2·s-1) [001]		 2-MNb
(10.0×6.0×2.8 Å)		 2-AMN
(12.3×6.2×2.8 Å)		 1-AMN (10.3×8.1×4.1 Å)
Betac 6.2×7.2 5.5×5.5 21.71 10.44 3.90
ITQ-17 6.2×6.6 6.3×6.3 13.90 9.74 0.33
表15 Beta型沸石和ITQ-17的物理化学性质[111]
Table 15 Physicochemical characteristics of zeolites tested in the present work[111]
Sample Si/Gea (Si+Ge)/Ala Area Micropore Crystal Acidity(μmol py)c
BET Volumn Size Brönsted Lewis
(m2·g-1) (cm3·g-1) (μm)b 423 523 623 423 523 623
BEC-1 1.2 48 468 0.216 0.6~1.5×0.2×0.2 20 12 4 1 0 0
BEC-2 9.5 48 436 0.194 0.1~0.2 21 15 8 11 9 8
1.5~1×0.2×0.2
BEC-3 10.2 73 358 0.143 0.1~0.2 8 6 2 10 9 7
1.5~2.5×0.2×0.2
BETA - 50 484 0.192 0.3~0.5 23 20 7 10 7 6
表16 Beta型沸石和ITQ-17催化2-甲氧基萘和乙酐酰化反应结果a[111]
Table 16 Acylation of 2-methoxynaphthalene with acetic anhydride over ITQ-17 in a batch reactor and comparison with Beta zeolitea[111]
Catalyst $r_{1-AMN}^b$ $R_{2-AMN}^b$ $r_{AMN}^b$ $S_{1-AMN}^c\\(M\%)$ $S_{2-AMN}^c\\(M\%)$ $S_{AMN}^c\\(M\%)$ X T2-MN 24 h $S_{1-AMN}^d\\(M\%)$ $S_{2-AMN}^d\\(M\%)$ $S_{AMN}^d\\(M\%)$ $S_{2-NOH}^d\\(M\%)$ $S_{2-dAMN}^d\\(M\%)$
(M%) (M%) (M%) (M%)d (M%) (M%) (M%) (M%) (M%)
BEC-1 15.38 19.39 0 44.2 55.8 0 28 35.7 62.9 1.4 0 0
BEC-2 26.37 21.28 0 55.3 44.7 0 67 44.7 49.8 4.8 0 0.7
BEC-3 38.44 16.14 0 70.4 29.6 0 52 61.4 34.5 3.5 0 0.5
BETA 54.46 41.74 4.24 54.2 41.6 4.2 90 32.1 54.7 11.5 0.4 1.3
图33 2-甲氧基萘和乙酐反应示意图[111]
Fig.33 Reaction scheme of the acylation of 2-MN with acetic anhydride over zeolites and possible alternative processes:(1) direct acylation;(2) intermolecular transacylation of 1-AMN with 2-MN;(3) protodeacylation of 1-AMN;(4) intramolecular transacylation of 1-AMN;(5) consecutive acylation of monoacylated products;(6) hydrolysis of the terminal O—C bond of 2-MN;(7) transalkylation of 2-MN[111]
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