CN107469800A - 一种苯酐催化剂载体 - Google Patents
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- 239000003054 catalyst Substances 0.000 title claims abstract description 31
- NOGFHTGYPKWWRX-UHFFFAOYSA-N 2,2,6,6-tetramethyloxan-4-one Chemical compound CC1(C)CC(=O)CC(C)(C)O1 NOGFHTGYPKWWRX-UHFFFAOYSA-N 0.000 title claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 16
- UHOVQNZJYSORNB-UHFFFAOYSA-N monobenzene Natural products C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims abstract description 15
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 13
- LGRFSURHDFAFJT-UHFFFAOYSA-N Phthalic anhydride Natural products C1=CC=C2C(=O)OC(=O)C2=C1 LGRFSURHDFAFJT-UHFFFAOYSA-N 0.000 claims abstract description 12
- JHIWVOJDXOSYLW-UHFFFAOYSA-N butyl 2,2-difluorocyclopropane-1-carboxylate Chemical compound CCCCOC(=O)C1CC1(F)F JHIWVOJDXOSYLW-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000000395 magnesium oxide Substances 0.000 claims abstract description 12
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 11
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000002803 maceration Methods 0.000 claims abstract description 10
- 239000000853 adhesive Substances 0.000 claims abstract description 9
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- 238000000034 method Methods 0.000 claims abstract description 7
- 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 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 6
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- 238000001354 calcination Methods 0.000 claims description 10
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- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 claims description 5
- 239000001095 magnesium carbonate Substances 0.000 claims description 5
- 229910000021 magnesium carbonate Inorganic materials 0.000 claims description 5
- 235000014380 magnesium carbonate Nutrition 0.000 claims description 5
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 4
- 239000005995 Aluminium silicate Substances 0.000 claims description 2
- 235000012211 aluminium silicate Nutrition 0.000 claims description 2
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 2
- 235000010216 calcium carbonate Nutrition 0.000 claims description 2
- 235000011132 calcium sulphate Nutrition 0.000 claims description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 2
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 2
- 239000011707 mineral Substances 0.000 claims description 2
- 235000010755 mineral Nutrition 0.000 claims description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims 1
- 238000006555 catalytic reaction Methods 0.000 claims 1
- 229910052739 hydrogen Inorganic materials 0.000 claims 1
- 239000001257 hydrogen Substances 0.000 claims 1
- 238000011068 loading method Methods 0.000 abstract description 6
- 239000011248 coating agent Substances 0.000 abstract description 5
- 238000000576 coating method Methods 0.000 abstract description 5
- 230000003647 oxidation Effects 0.000 abstract description 4
- 238000007254 oxidation reaction Methods 0.000 abstract description 4
- -1 benzene anhydride Chemical class 0.000 abstract description 3
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- 238000004519 manufacturing process Methods 0.000 description 3
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000000314 lubricant Substances 0.000 description 2
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 2
- 239000000347 magnesium hydroxide Substances 0.000 description 2
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
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- 230000001590 oxidative effect Effects 0.000 description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- 230000010718 Oxidation Activity Effects 0.000 description 1
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- 238000010521 absorption reaction Methods 0.000 description 1
- 238000004026 adhesive bonding Methods 0.000 description 1
- 229910000272 alkali metal oxide Inorganic materials 0.000 description 1
- 229920000180 alkyd Polymers 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
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- 239000007788 liquid Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 230000001404 mediated effect Effects 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical class CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- 229920001225 polyester resin Polymers 0.000 description 1
- 239000004645 polyester resin Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 229910052701 rubidium Inorganic materials 0.000 description 1
- IGLNJRXAVVLDKE-UHFFFAOYSA-N rubidium atom Chemical compound [Rb] IGLNJRXAVVLDKE-UHFFFAOYSA-N 0.000 description 1
- 239000011265 semifinished product Substances 0.000 description 1
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- 238000007873 sieving Methods 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/082—Decomposition and pyrolysis
- B01J37/088—Decomposition of a metal salt
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/10—Magnesium; Oxides or hydroxides thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/61—Surface area
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/0009—Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0201—Impregnation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
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Abstract
本发明公开了一种苯酐催化剂载体,由氧化镁载体和苯酐浸渍液制成,其特征在于:所述苯酐催化剂的制备工艺为:1)将滑石粉、胶粘剂、助熔剂原料分别粉碎、过筛,取得粒径为50~150μm的原料;2)将各原料按配比充分混合并均匀送入成型设备,成型为一定尺寸的环形或圆柱形;3)将所述环形或圆柱形原料放入高温煅烧炉中烘干、煅烧,得到所述氧化镁载体;4)采用浸渍液法将所述苯酐浸渍液涂覆在所述氧化镁载体上,经干燥制得成品苯酐催化剂载体;这种苯酐催化剂载体具有压降小,比表面积大,在相同厚度涂层下载体载持量多,可延长催化剂寿命及提高催化剂负荷;而在相同的负载下,涂层变薄,减小产物的扩散阻力,减少深度氧化,提高催化剂选择性。
Description
技术领域
本发明涉及催化剂技术领域,具体为一种苯酐催化载体。
背景技术
苯酐是制造PVC增塑剂、聚酯树脂、醇酸树脂、染料中间体和医药的重要原料。以往生产苯酐的技术方法是以邻二甲苯氧化法,但该方法制造苯酐技术的先进性在很大程度上取决于其所用氧化催化剂综合性能的先进程度。目前国内外性能较先进的催化剂大都是将含有少量铷、铯等碱金属氧化物的V2O5-TiO2系氧化活性物料喷涂在碳化硅质、氧化铝质或其它瓷质的球形或环形载体上经一定温度(约270℃左右)低温烧制而成的,作为催化剂重要组成部分的载体的物理化学性状(如化学组成、相组成、显微结构、表面粗糙度等)和几何形状及尺寸对催化剂活性涂层之附着强度、载持量、相同载持量时的涂层厚度、扩散阻力、选择性、寿命以及生产装置的压降、能耗和热点温度等性能均有一定影响。
目前,市面上用于催化剂载体主要是氧化铝、氧化硅等氧化物,此类载体虽具有制备简单、原料易于获得、高比表面积等优点,但在一些苛刻的反应条件下,比如高温高压、原料中混有杂质时,将导致催化剂活性的降低和寿命的减短,机械强度不是很高,在催化剂的再生过程中,由于氧化铝载体导热性能不优良,很容易因为飞温造成催化剂活性组分烧结。因此,需要找出一种适合的材料合成催化剂载体。
发明内容
为了解决上述问题,我们发明了一种苯酐催化剂载体,由氧化镁载体和苯酐浸渍液制成,其苯酐催化剂载体制备工艺为:
1)各种原料的预处理:将优质滑石粉、胶粘剂、助熔剂分别粉碎、过筛,取得粒径为50~150μm的原料;
2)将各原料按配比充分混合后均匀送入成型设备,成型为一定尺寸的环形或圆柱形;
3)将混合后的环形或圆柱形原料放入高温煅烧炉中烘干、煅烧,得到氧化镁载体;
4)采用浸渍液法将苯酐浸渍液涂覆在氧化镁载体上,经干燥制得成品苯酐催化剂载体。
进一步地,胶粘剂可为粘性好、烧结范围宽的高岭土和氢氧化镁;助熔剂为含钙、镁的矿物质,如碳酸钙、硫酸钙、碳酸镁、菱镁石等;各原料配比可为滑石粉55~90%,胶粘剂5~40%,助熔剂2~6%。
进一步地,成型设备可为圆柱形或环形模具与自动液压机,或捏合机;成型尺寸可为柱直径16~24mm、长度16~24mm的圆柱形或内径4~8mm、外径8~16mm、高度4~12mm的环形。
进一步地,圆柱形或环形原料在烘干过程中,保持80~120℃温度下烘15~40小时,然后置于高温煅烧炉中煅烧,煅烧温度为1600~1850℃,煅烧时间为3~7小时,最好的煅烧温度是1680~1750℃。
本发明的有益效果为:苯酐催化剂氧化镁载体具有压降小,有利于节能,比表面积大,在相同厚度涂层下载体载持量多,可延长催化剂寿命及提高催化剂负荷;而在相同的负载下,涂层变薄,减小产物的扩散阻力,减少深度氧化,提高催化剂的选择性。
具体实施方式
本发明提供了一种苯酐催化剂载体,其具体制备工艺如下:
1)滑石粉经粉碎、过筛后的颗粒粒径为0.147~0.074mm(-100目+200目)的占20~40%,小于0.074毫米(-200目)占60~80%;以硫酸钙、碳酸镁主的助熔剂,其颗粒度均小于0.074毫米(-200目),占2~6%;以氢氧化镁为主的粘胶剂均小于0.074毫米(-200目),占5~40%。
2)将混合均匀的原料送入捏合机中,逐渐加入粘胶剂进行捏合至物料软硬适中,捏合时间20~40分钟。然后将原料造粒,加入一定量的成型润滑剂拌匀后压制成环型,外形尺寸为Φ6mm~Φ8mm,高度为4~7mm,壁厚为1.4~1.5mm。成型润滑剂可以是石墨或硬脂酸类,加入量按成型物料重量计为2~5%。
3)将成型好的半成品在80~120℃温度下烘24小时,然后置于高温煅烧炉中煅烧,煅烧温度为1700℃,煅烧时间为4小时,煅烧气氛为惰性气氛和或氧化气氛。通过成型煅烧后的强度可达轴向≥25Kg/cm2,径向≥7Kg/cm2;吸水率0.3~0.4%,气孔率0.85~0.9%,体积密度2.57~2.88g/cm3,堆积密度0.71~0.75g/ml。
4)将制备好的环形氧化镁载体置于浸渍液中浸渍1小时,浸渍液温度保持在85℃,然后在175℃烘干5小时,最后将完成浸渍操作的物料置于煅烧炉中,在600℃下于氧化气氛中煅烧5小时,使硝酸盐完全分解。
以上所述仅是本发明的优选实施方式,本发明的保护范围并不仅局限于上述实施例,凡属于本发明思路下的技术方案均属于本发明的保护范围。应当指出,对于本技术领域的普通技术人员来说,在不脱离本发明原理前提下的若干改进和润饰,这些改进和润饰也应视为本发明的保护范围。
Claims (4)
1.一种苯酐催化剂载体,由氧化镁载体和苯酐浸渍液制成,其特征在于:所述苯酐催化剂的制备工艺为:
1)原料的预处理:将滑石粉、胶粘剂、助熔剂原料分别粉碎、过筛,取得粒径为50~150μm的原料;
2)将各原料按配比充分混合并均匀送入成型设备,成型为一定尺寸的环形或圆柱形;
3)将所述环形或圆柱形原料放入高温煅烧炉中烘干、煅烧,得到所述氧化镁载体;
4)采用浸渍液法将所述苯酐浸渍液涂覆在所述氧化镁载体上,经干燥制得成品苯酐催化剂载体。
2.根据权利要求1所述的一种苯催化剂载体,其特征在于:所述胶粘剂可为高岭土或氢氧化镁;所述助熔剂为碳酸钙、硫酸钙、碳酸镁、菱镁石矿物质中的一种或多种;各原料配比为滑石粉55~90%,胶粘剂5~40%,助熔剂2~6%。
3.根据权利要求1所述的一种苯催化剂载体,其特征在于:所述成型设备可为捏合机或自动液压机;所述成型尺寸可为柱直径16~24mm、长度16~24mm的圆柱形或内径4~8mm、外径8~16mm、高度4~12mm的环形。
4.根据权利要求1所述的一种苯催化剂载体,其特征在于:所述烘干工序中的烘干温度为80~120℃,烘干时间15~40小时;高温煅烧炉中的煅烧温度为1600~1850℃,煅烧时间为3~7小时。
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