CN1151224C - Preparation method of selective infrared absorbing material with anion layer column structure - Google Patents
Preparation method of selective infrared absorbing material with anion layer column structure Download PDFInfo
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- 239000011358 absorbing material Substances 0.000 title claims abstract description 9
- 150000001450 anions Chemical class 0.000 title claims description 17
- 238000002360 preparation method Methods 0.000 title claims description 8
- 239000000203 mixture Substances 0.000 claims abstract description 20
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- 239000000243 solution Substances 0.000 claims description 20
- 239000010410 layer Substances 0.000 claims description 19
- 239000003513 alkali Substances 0.000 claims description 11
- 229910021645 metal ion Inorganic materials 0.000 claims description 11
- 239000012266 salt solution Substances 0.000 claims description 10
- 239000002002 slurry Substances 0.000 claims description 10
- 239000011229 interlayer Substances 0.000 claims description 9
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 8
- 150000003839 salts Chemical class 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 4
- 229910052751 metal Inorganic materials 0.000 claims description 4
- 239000002184 metal Substances 0.000 claims description 4
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 2
- 239000004202 carbamide Substances 0.000 claims description 2
- 150000004679 hydroxides Chemical class 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 238000010521 absorption reaction Methods 0.000 abstract description 23
- 239000000463 material Substances 0.000 abstract description 21
- 239000002245 particle Substances 0.000 abstract description 20
- 239000013078 crystal Substances 0.000 abstract description 9
- 238000009826 distribution Methods 0.000 abstract description 8
- 125000000129 anionic group Chemical group 0.000 abstract description 6
- 238000000034 method Methods 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 238000005516 engineering process Methods 0.000 abstract description 2
- 238000009830 intercalation Methods 0.000 abstract description 2
- 230000002687 intercalation Effects 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 230000002349 favourable effect Effects 0.000 abstract 2
- 239000002648 laminated material Substances 0.000 abstract 1
- 239000011268 mixed slurry Substances 0.000 description 12
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 8
- 235000011121 sodium hydroxide Nutrition 0.000 description 7
- 230000015572 biosynthetic process Effects 0.000 description 6
- 239000011777 magnesium Substances 0.000 description 6
- 238000003786 synthesis reaction Methods 0.000 description 6
- 150000002500 ions Chemical class 0.000 description 5
- -1 sulfate group anion Chemical class 0.000 description 4
- 239000011701 zinc Substances 0.000 description 4
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 3
- 238000002425 crystallisation Methods 0.000 description 3
- 230000008025 crystallization Effects 0.000 description 3
- 235000017550 sodium carbonate Nutrition 0.000 description 3
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 2
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 2
- 238000000862 absorption spectrum Methods 0.000 description 2
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 description 2
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 2
- 229940010048 aluminum sulfate Drugs 0.000 description 2
- 229940077388 benzenesulfonate Drugs 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000011572 manganese Substances 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical group [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- VVDHJOLQGATEBD-UHFFFAOYSA-N [N+](=O)([O-])[O-].[Al+3].[Mn+2].[N+](=O)([O-])[O-].[N+](=O)([O-])[O-].[N+](=O)([O-])[O-].[N+](=O)([O-])[O-] Chemical compound [N+](=O)([O-])[O-].[Al+3].[Mn+2].[N+](=O)([O-])[O-].[N+](=O)([O-])[O-].[N+](=O)([O-])[O-].[N+](=O)([O-])[O-] VVDHJOLQGATEBD-UHFFFAOYSA-N 0.000 description 1
- XQYCUFOSMOQDCI-UHFFFAOYSA-N [N+](=O)([O-])[O-].[Co+2].[Al+3].[N+](=O)([O-])[O-].[N+](=O)([O-])[O-].[N+](=O)([O-])[O-].[N+](=O)([O-])[O-] Chemical compound [N+](=O)([O-])[O-].[Co+2].[Al+3].[N+](=O)([O-])[O-].[N+](=O)([O-])[O-].[N+](=O)([O-])[O-].[N+](=O)([O-])[O-] XQYCUFOSMOQDCI-UHFFFAOYSA-N 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- HWICWUPUYYJJLM-UHFFFAOYSA-L aluminum magnesium zinc carbonate Chemical compound C([O-])([O-])=O.[Al+3].[Mg+2].[Zn+2] HWICWUPUYYJJLM-UHFFFAOYSA-L 0.000 description 1
- ZPCFDBGVDLCXSO-UHFFFAOYSA-N aluminum nickel(2+) pentanitrate Chemical compound [N+](=O)([O-])[O-].[Ni+2].[Al+3].[N+](=O)([O-])[O-].[N+](=O)([O-])[O-].[N+](=O)([O-])[O-].[N+](=O)([O-])[O-] ZPCFDBGVDLCXSO-UHFFFAOYSA-N 0.000 description 1
- UJOHNXQDVUADCG-UHFFFAOYSA-L aluminum;magnesium;carbonate Chemical group [Mg+2].[Al+3].[O-]C([O-])=O UJOHNXQDVUADCG-UHFFFAOYSA-L 0.000 description 1
- SRSXLGNVWSONIS-UHFFFAOYSA-M benzenesulfonate Chemical group [O-]S(=O)(=O)C1=CC=CC=C1 SRSXLGNVWSONIS-UHFFFAOYSA-M 0.000 description 1
- SRSXLGNVWSONIS-UHFFFAOYSA-N benzenesulfonic acid Chemical compound OS(=O)(=O)C1=CC=CC=C1 SRSXLGNVWSONIS-UHFFFAOYSA-N 0.000 description 1
- 229940092714 benzenesulfonic acid Drugs 0.000 description 1
- 235000013877 carbamide Nutrition 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 description 1
- 229910001981 cobalt nitrate Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000004925 denaturation Methods 0.000 description 1
- 230000036425 denaturation Effects 0.000 description 1
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 description 1
- UZUODNWWWUQRIR-UHFFFAOYSA-L disodium;3-aminonaphthalene-1,5-disulfonate Chemical compound [Na+].[Na+].C1=CC=C(S([O-])(=O)=O)C2=CC(N)=CC(S([O-])(=O)=O)=C21 UZUODNWWWUQRIR-UHFFFAOYSA-L 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 229910001629 magnesium chloride Inorganic materials 0.000 description 1
- 229910052943 magnesium sulfate Inorganic materials 0.000 description 1
- 235000019341 magnesium sulphate Nutrition 0.000 description 1
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 125000001273 sulfonato group Chemical group [O-]S(*)(=O)=O 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011592 zinc chloride Substances 0.000 description 1
- 235000005074 zinc chloride Nutrition 0.000 description 1
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 1
- 229960001763 zinc sulfate Drugs 0.000 description 1
- 229910000368 zinc sulfate Inorganic materials 0.000 description 1
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- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
Description
本发明涉及一种阴离子层柱结构选择性红外吸收材料的制备方法。The invention relates to a preparation method of an anion layer column structure selective infrared absorbing material.
目前，国内外农膜中广为采用的红外吸收材料主要为滑石粉等天然无机产物，其红外吸收效果(膜的保温性)与可见光透过率等性能无法兼顾，滑石粉添加量少，红外吸收效果(膜的保温性)差，添加量大，则造成大幅度降低可见光的透过率。At present, the infrared absorbing materials widely used in agricultural film at home and abroad are mainly natural inorganic products such as talcum powder. The absorption effect (film insulation) is poor, and the amount added will greatly reduce the transmittance of visible light.
近年来阴离子层状结构材料已成为国际上新兴的研究热点，阴离子层状材料其化学组成为[M2+ 1-xM3+ x(OH)2]An- x/nmH2O，其中：M2+和M3+为二价和三价金属离子，An-为n价负离子，其最为典型的结构特征是：纳米量级的二维层板纵向有序排列形成三维晶体结构，层板内原子间为共价键合，层间为弱化学键，如离子键、氢键。层板骨架带有正电荷，层间为相反电荷离子与之平衡，整体呈电中性，层间离子具有可交换性，且层间距随层间离子大小不同呈规律性变化。层板化学组成、层间离子种类和数量、层间距等均可随设计要求而改变，因此可表现出不同且多样的物理化学性质，使其广泛应用于石油化工、医药、农业等行业中(见Cavani et al.的《Catal.Today》，1997，11：173)。由于这种材料在7-14μm波长(此为散热红外范围)范围内具有红外吸收性能，可作为选择性红外吸收材料，替代传统的保温剂，用于农膜等，提高保温效果。In recent years, anionic layered materials have become an emerging research hotspot in the world. The chemical composition of anionic layered materials is [M 2+ 1-x M 3+ x (OH) 2 ]A n- x/n mH 2 O, Among them: M 2+ and M 3+ are divalent and trivalent metal ions, A n- is n-valent negative ions, and its most typical structural features are: nanometer-scale two-dimensional laminates are arranged vertically and orderly to form a three-dimensional crystal structure , The atoms in the laminate are covalently bonded, and the interlayers are weak chemical bonds, such as ionic bonds and hydrogen bonds. The laminate skeleton is positively charged, and the interlayer is balanced by oppositely charged ions. The whole is electrically neutral, and the interlayer ions are exchangeable, and the interlayer distance changes regularly with the size of the interlayer ions. The chemical composition of the laminate, the type and quantity of interlayer ions, and the interlayer spacing can all be changed with the design requirements, so it can exhibit different and diverse physical and chemical properties, making it widely used in petrochemical, pharmaceutical, agricultural and other industries ( See Cavani et al., Catal. Today, 1997, 11:173). Since this material has infrared absorption properties in the range of 7-14 μm wavelength (this is the infrared range of heat dissipation), it can be used as a selective infrared absorption material to replace traditional heat preservation agents, used in agricultural films, etc., to improve heat preservation effects.
但上述结构([M2+ 1-xM3+ x(OH)2]An- x/nmH2O)的阴离子层状材料在7-14μm波长范围内，存在红外吸收范围固定和在选择性红外吸收范围内存在缺陷及红外吸收性能低的弱点，限制了这一无机非金属晶体材料的广泛应用。However, the anionic layered material with the above structure ([M 2+ 1-x M 3+ x (OH) 2 ]A n- x/n mH 2 O) has a fixed infrared absorption range and a The defects in the selective infrared absorption range and the weakness of low infrared absorption performance limit the wide application of this inorganic non-metallic crystal material.
本发明的目的：提供一种阴离子层柱结构选择性红外吸收材料的制备方法，使其较传统的红外吸收材料在7-14μm波长范围内，具有更高的选择性红外吸收性能和选择性红外吸收可调变性能，以适合不同的使用条件。The purpose of the present invention: to provide a preparation method of selective infrared absorption material with anion layer column structure, so that it has higher selective infrared absorption performance and selective infrared absorption performance than traditional infrared absorption materials in the 7-14 μm wavelength range. Absorption can be adjusted to suit different conditions of use.
本发明的发明要点：Invention points of the present invention:
一种阴离子层柱结构选择性红外吸收材料，其化学组成和结构为：A kind of anion layer pillar structure selective infrared absorbing material, its chemical composition and structure are:
[M(II)1-xM(III)x(OH)2]An1- a/nBn2- b/nmH2O，其中M(II)为二价金属离子，M(III)为三价金属离子，An1-和Bn2-为不同的阴离子或阴离子基团，n1、n2＝1-3，a+b＝x，0＜a/b≤1，0.15≤x≤0.5，m通常为1-20。其为层柱结构，层板为M(II)和M(III)的氢氧化物，层间支撑柱为An1-和Bn2-。[M(II) 1-x M(III) x (OH) 2 ]A n1- a/n B n2- b/n mH 2 O, where M(II) is a divalent metal ion and M(III) is Trivalent metal ions, A n1- and B n2- are different anions or anion groups, n1, n2=1-3, a+b=x, 0<a/b≤1, 0.15≤x≤0.5, m Usually 1-20. It is a layer-column structure, the laminates are M(II) and M(III) hydroxides, and the interlayer support columns are A n1- and B n2- .
上述二价金属离子M(II)为Mg2+Zn2+Cu2+Ni2+Fe2+Mn2+Ca2+中的任何一种，三价金属离子M(III)为Al3+Cr3+Fe3+V3+Co3+Ga3+Ti3+中的任何一种，An1-为Cl-CO3 2-NO3 -中的任何一种，Bn2-为F-Br-I-SO4 2-ClO3 -OH-H2PO4 -WO4 2-有机磺酸阴离子中的任何一种。The above divalent metal ion M(II) is any one of Mg 2+ Zn 2+ Cu 2+ Ni 2+ Fe 2+ Mn 2+ Ca 2+ , and the trivalent metal ion M(III) is Al 3+ Cr Any one of 3+ Fe 3+ V 3+ Co 3+ Ga 3+ Ti 3+ , A n1- is any one of Cl - CO 3 2- NO 3 - , B n2- is F - Br - Any one of I - SO 4 2- ClO 3 - OH - H 2 PO 4 - WO 4 2- organosulfonic acid anions.
上述阴离子层柱结构选择性红外吸收材料的制备方法，具体步骤为：The preparation method of the above-mentioned anion layer pillar structure selective infrared absorbing material, the specific steps are:
A：将可溶性二价无机金属盐和可溶性三价无机金属盐配制成混合盐溶液，二价金属离子的摩尔浓度为0.2-2.5M，三价金属离子的浓度为0.1-1.25M；A: Mix soluble divalent inorganic metal salt and soluble trivalent inorganic metal salt to prepare mixed salt solution, the molar concentration of divalent metal ions is 0.2-2.5M, and the concentration of trivalent metal ions is 0.1-1.25M;
B：将步骤A中的混合盐溶液与碱溶液混合，得到pH值为8.5-13的浆液，步骤A两种盐或步骤B碱溶液中至少有一种含有An1-；B: Mix the mixed salt solution in step A with the alkali solution to obtain a slurry with a pH value of 8.5-13, at least one of the two salts in step A or the alkali solution in step B contains A n1- ;
C：将步骤B所得浆液在70-120℃下搅拌晶化2-24小时后；加入含有Bn2-的酸溶液，调节pH值为4.5-7.5，搅拌2-10小时，然后过滤、洗涤、干燥收集产物。C: Stir and crystallize the slurry obtained in step B at 70-120°C for 2-24 hours; add an acid solution containing Bn2- , adjust the pH value to 4.5-7.5, stir for 2-10 hours, then filter, wash, The product was collected by drying.
步骤B中的碱溶液最好为氢氧化钠、氨水、碳酸钠、尿素中任何一种或它们的混合溶液。The alkaline solution in step B is preferably any one of sodium hydroxide, ammonia water, sodium carbonate, urea or their mixed solutions.
本发明根据阴离子层柱结构材料组成和结构的可调变性特点，利用插层化学原理，通过改变原料种类和调节原料组成、浓度、比例、晶化温度、溶液pH值、晶化时间、加料顺序等方法组装出具有优良选择性红外吸收性能的阴离子层柱材料，材料晶粒分布均匀和细小，与传统的阴离子层状材料相比，本发明所制备的高选择性红外吸收阴离子层柱材料具有更高的选择性红外吸收性能和适用范围广泛等优点。同时本发明的制备方法工艺简单、设备投资少、生产时间短、能耗低、无环境污染。本发明提供的技术还可用于合成不同组成和结构的阴离子层柱结构选择性红外吸收材料。According to the adjustable denaturation characteristics of the composition and structure of the anion layer column structure materials, the present invention utilizes the principle of intercalation chemistry to change the types of raw materials and adjust the composition, concentration, ratio, crystallization temperature, solution pH value, crystallization time, and feeding sequence. The anion layer column material with excellent selective infrared absorption performance is assembled by methods such as , and the grain distribution of the material is uniform and small. Compared with the traditional anion layer material, the highly selective infrared absorption anion layer column material prepared by the present invention has It has the advantages of higher selective infrared absorption performance and wide application range. Simultaneously, the preparation method of the present invention has simple process, less equipment investment, short production time, low energy consumption and no environmental pollution. The technology provided by the invention can also be used for synthesizing anion layer column structure selective infrared absorbing materials with different compositions and structures.
下面结合附图和实施例对本发明作进一步的描述：Below in conjunction with accompanying drawing and embodiment the present invention will be further described:
图1：Mg4Al2(OH)12·CO3·mH2O的红外吸收谱图Figure 1: Infrared absorption spectrum of Mg 4 Al 2 (OH) 12 ·CO 3 ·mH 2 O
图2：Mg4Al2(OH)12·(CO3)0.4(SO4)0.6·mH2O(实施例1)的红外吸收谱图Figure 2: Infrared absorption spectrum of Mg 4 Al 2 (OH) 12 ·(CO 3 ) 0.4 (SO 4 ) 0.6 ·mH 2 O (Example 1)
实施例1：镁铝-碳酸根和硫酸根阴离子层柱材料的合成Embodiment 1: the synthesis of magnesium aluminum-carbonate group and sulfate group anion layer column material
选取1.6摩尔硫酸镁和0.8摩尔硫酸铝配成1升盐溶液，取4.8摩尔NaOH和2.5摩尔Na2CO3配成1升碱溶液，将两溶液混合，混合浆液pH＝11.0，混合浆液在100℃晶化4小时，加入硫酸至浆液pH＝7，再晶化2小时，过滤，洗涤、干燥，得到的产物为Mg4Al2(OH)12·(CO3)0.4(SO4)0.6·mH2O。产物晶相结构良好，粒径0.2μ，粒子分布(粒径＝0.2μ)大于99％，红外吸收率大于85％。Select 1.6 moles of magnesium sulfate and 0.8 moles of aluminum sulfate to make 1 liter of salt solution, take 4.8 moles of NaOH and 2.5 moles of Na2CO3 to make 1 liter of alkali solution, mix the two solutions, the pH of the mixed slurry is 11.0, and the mixed slurry is at 100 ℃ to crystallize for 4 hours, add sulfuric acid to the slurry pH = 7, recrystallize for 2 hours, filter, wash and dry, the product obtained is Mg 4 Al 2 (OH) 12 ·(CO 3 ) 0.4 (SO 4 ) 0.6 · mH 2 O. The crystal phase structure of the product is good, the particle size is 0.2μ, the particle distribution (particle size=0.2μ) is greater than 99%, and the infrared absorption rate is greater than 85%.
实施例2：锌铝-碳酸根和硫酸根阴离子层柱材料的合成Embodiment 2: the synthesis of zinc aluminum-carbonic acid radical and sulfate radical anion layer column material
选取1.0摩尔硫酸锌和0.5摩尔硫酸铝配成1升盐溶液，取4摩尔NaOH和1.5摩尔Na2CO3配成1升碱溶液，将两溶液混合，混合浆液pH＝10.0，混合浆液在80℃晶化时间20小时，加入硫酸至浆液pH＝6.8，再晶化12小时，过滤，洗涤、干燥。得到的产物为Zn4Al2(OH)12·(CO3)0.5(SO4)0.5·mH2O。产物晶相结构良好，粒径0.3μ，粒子分布(粒径＝0.3μ)大于99％，红外吸收率大于85％。Select 1.0 moles of zinc sulfate and 0.5 moles of aluminum sulfate to make 1 liter of salt solution, take 4 moles of NaOH and 1.5 moles of Na2CO3 to make 1 liter of alkali solution, mix the two solutions, the pH of the mixed slurry is 10.0 , and the mixed slurry is at 80 The crystallization time was 20 hours at ℃, and sulfuric acid was added to the pH of the slurry to 6.8, and recrystallized for 12 hours, filtered, washed, and dried. The product obtained is Zn 4 Al 2 (OH) 12 ·(CO 3 ) 0.5 (SO 4 ) 0.5 ·mH 2 O. The crystal phase structure of the product is good, the particle size is 0.3μ, the particle distribution (particle size=0.3μ) is greater than 99%, and the infrared absorption rate is greater than 85%.
实施例3：钴铝-硝酸根和硫酸根阴离子层柱材料的合成Embodiment 3: the synthesis of cobalt aluminum-nitrate and sulfate radical anion layer column material
选取1.2摩尔硝酸钴和0.4摩硝酸铝配成1升盐溶液，取3.5摩尔NaOH配成1升碱溶液，将两溶液混合，混合浆液pH＝9.5，将混合浆液在140℃晶化时间6小时，加入硫酸至浆液pH＝6.5，再晶化4小时，过滤，洗涤、干燥。得到的产物为Co6Al2(OH)16·(NO3)0.2(SO4)0.8·mH2O。产物晶相结构良好，粒径0.3μ，粒子分布(粒径＝0.3μ)大于99％，红外吸收率大于90％Select 1.2 moles of cobalt nitrate and 0.4 moles of aluminum nitrate to make 1 liter of salt solution, take 3.5 moles of NaOH to make 1 liter of alkali solution, mix the two solutions, the pH of the mixed slurry is 9.5, and crystallize the mixed slurry at 140 ° C for 6 hours , adding sulfuric acid to the slurry pH = 6.5, recrystallized for 4 hours, filtered, washed and dried. The product obtained is Co 6 Al 2 (OH) 16 ·(NO 3 ) 0.2 (SO 4 ) 0.8 ·mH 2 O. The crystal phase structure of the product is good, the particle size is 0.3μ, the particle distribution (particle size=0.3μ) is greater than 99%, and the infrared absorption rate is greater than 90%.
实施例4：镍铝-硝酸根和磺酸根阴离子层柱材料的合成Embodiment 4: the synthesis of nickel aluminum-nitrate and sulfonate anion layer column material
选取2.2摩尔硝酸镍和1.1摩尔硝酸铝配成1升盐溶液，取8.5摩尔NaOH配成1升碱溶液，将两溶液混合，混合浆液pH＝9，将混合浆液在100℃晶化时间6小时，加入磺酸至浆液pH＝6.7，再晶化4小时，过滤，洗涤、干燥。得到的产物为Ni4Al2(OH)12·(NO3)0.4(A)0.6·mH2O，A为磺酸根。产物晶相结构良好，粒径0.3μ，粒子分布(粒径＝0.3μ)大于99％，红外吸收率大于90％。Select 2.2 moles of nickel nitrate and 1.1 moles of aluminum nitrate to make 1 liter of salt solution, take 8.5 moles of NaOH to make 1 liter of alkali solution, mix the two solutions, the pH of the mixed slurry is 9, and crystallize the mixed slurry at 100 ° C for 6 hours , adding sulfonic acid until the slurry pH = 6.7, recrystallized for 4 hours, filtered, washed and dried. The obtained product is Ni 4 Al 2 (OH) 12 ·(NO 3 ) 0.4 (A) 0.6 ·mH 2 O, A is a sulfonate group. The crystal phase structure of the product is good, the particle size is 0.3μ, the particle distribution (particle size=0.3μ) is greater than 99%, and the infrared absorption rate is greater than 90%.
实施例5：锰铝-硝酸根和苯磺酸根阴离子层柱材料的合成Embodiment 5: the synthesis of manganese aluminum-nitrate and benzenesulfonate anion layer column material
选取1.6摩尔硝酸锰和0.8摩尔硝酸铝配成1升盐溶液，取9摩尔NaOH配成1升碱溶液，将两溶液混合，混合浆液pH＝9，将混合浆液在80℃晶化时间24小时，加入苯磺酸至浆液pH＝5.0，再晶化2小时，过滤，洗涤、干燥。得到的产物为Mn4Al2(OH)12·(NO3)0.1(B)0.9·mH2O，B为苯磺酸根。产物晶相结构良好，粒径0.3μ，粒子分布(粒径＝0.3μ)大于99％，红外吸收率大于90％。Select 1.6 moles of manganese nitrate and 0.8 moles of aluminum nitrate to make 1 liter of salt solution, take 9 moles of NaOH to make 1 liter of alkali solution, mix the two solutions, the pH of the mixed slurry is 9, and crystallize the mixed slurry at 80 ° C for 24 hours , adding benzenesulfonic acid until the slurry pH = 5.0, recrystallized for 2 hours, filtered, washed and dried. The obtained product is Mn 4 Al 2 (OH) 12 ·(NO 3 ) 0.1 (B) 0.9 ·mH 2 O, B is benzenesulfonate. The crystal phase structure of the product is good, the particle size is 0.3μ, the particle distribution (particle size=0.3μ) is greater than 99%, and the infrared absorption rate is greater than 90%.
实施例6：锌镁铝-碳酸根和硫酸根阴离子层柱材料的合成Embodiment 6: the synthesis of zinc magnesium aluminum-carbonate and sulfate radical anion layer column material
选取0.8摩尔氯化镁和0.8摩尔氯化锌(镁和锌的摩尔组成可在0-1范围调变)及0.8摩尔氯化铝配成1升盐溶液，取4.8摩尔NaOH和1.2摩尔Na2CO3配成1升碱溶液，将两溶液混合，混合浆液pH＝12，将混合浆液在100℃晶化时间4小时，加入硫酸至浆液pH＝7，再晶化4小时，过滤，洗涤、干燥。得到的产物为Mg2Zn2Al2(OH)12·(NO3)0.3(SO4)0.7·mH2O。产物晶相结构良好，粒径0.3μ，粒子分布(粒径＝0.3μ)大于99％，红外吸收率大于85％。Select 0.8 moles of magnesium chloride and 0.8 moles of zinc chloride (the molar composition of magnesium and zinc can be adjusted in the range of 0-1) and 0.8 moles of aluminum chloride to make 1 liter of salt solution, take 4.8 moles of NaOH and 1.2 moles of Na 2 CO 3 Make 1 liter of alkali solution, mix the two solutions, the mixed slurry pH=12, crystallize the mixed slurry at 100°C for 4 hours, add sulfuric acid until the slurry pH=7, recrystallize for 4 hours, filter, wash and dry. The product obtained is Mg 2 Zn 2 Al 2 (OH) 12 ·(NO 3 ) 0.3 (SO 4 ) 0.7 ·mH 2 O. The crystal phase structure of the product is good, the particle size is 0.3μ, the particle distribution (particle size=0.3μ) is greater than 99%, and the infrared absorption rate is greater than 85%.
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