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CN1017685B - 聚烯烃提纯用的吸附剂及其制法 - Google Patents

聚烯烃提纯用的吸附剂及其制法

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Publication number
CN1017685B
CN1017685B CN90100255A CN90100255A CN1017685B CN 1017685 B CN1017685 B CN 1017685B CN 90100255 A CN90100255 A CN 90100255A CN 90100255 A CN90100255 A CN 90100255A CN 1017685 B CN1017685 B CN 1017685B
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aluminum oxide
purification
compound
butylene
sorbent material
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CN1044415A (zh
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艾瑞斯·哲陈
克苏得-博尼亚得·卡特
艾瑞斯·昆博
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Rhodia Chimie SAS
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Rhone Poulenc Chimie SA
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Publication of CN1044415A publication Critical patent/CN1044415A/zh
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C7/00—Purification; Separation; Use of additives
    • C07C7/12—Purification; Separation; Use of additives by adsorption, i.e. purification or separation of hydrocarbons with the aid of solids, e.g. with ion-exchangers
    • 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
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
    • 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
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
    • B01J20/041—Oxides or hydroxides
    • 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
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
    • B01J20/046—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium containing halogens, e.g. halides
    • 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
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
    • B01J20/08—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04 comprising aluminium oxide or hydroxide; comprising bauxite
    • 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
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
    • B01J20/28057—Surface area, e.g. B.E.T specific surface area
    • 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
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/3078—Thermal treatment, e.g. calcining or pyrolizing
    • 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
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
    • B01J20/3202—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating characterised by the carrier, support or substrate used for impregnation or coating
    • B01J20/3204—Inorganic carriers, supports or substrates
    • 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
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
    • B01J20/3231—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating characterised by the coating or impregnating layer
    • B01J20/3234—Inorganic material layers
    • B01J20/3236—Inorganic material layers containing metal, other than zeolites, e.g. oxides, hydroxides, sulphides or salts

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
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  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)

Abstract

本发明涉及烯烃，特别是在配位催化剂存在下烯烃聚合所得聚烯烃提纯用的催化剂。该吸附剂包括氧化铝和至少一种选自碱金属和碱土金属的元素，该元素用量为15-100mmol/100g氧化铝。该吸附剂的异构能力相当低。

Description

本发明涉及烯烃提纯用的吸附剂，特别是烯烃在配位催化剂存在下聚合所得聚烯烃提纯所用氧化铝吸附剂。
烯烃聚合一般在含元素周期表中ⅣB，ⅤB，Ⅴ1B族的元素，特别是Ⅴ，Ti和Zr的聚合催化剂存在下进行。这些催化剂同时还含有机金属化合物（烃基金属化合物），金属氢化物或氢氧化合物作为还原剂。这类催化剂一般称为转化催化剂，对烯烃聚合的催化活性大。
不过，所得聚烯烃会受到来自这些催化剂的金属残余物的污染，因此必须在其应用前进行提纯，以避免着色，降解并降低毒性。
此外，烯烃聚合方法一般包括聚烯烃中所含溶剂或单体的回收步骤，回收的溶剂和单体循环送入聚合步骤。这些化合物中存在的金属会带来设备腐蚀问题。
为了提纯烯烃，已知可用各种吸附剂，特别是氧化铝。
在所用吸附剂中，可有效地采用球状吸收剂，其制法比各种粉或块状容易。实际上，在气动提纯柱的填充或除料过程中，球状产品均易于传送。
吸附剂中，氧化铝易于制成球状。但是，有利于制备并且金属吸附性能好的氧化铝还有很大的缺点，即易于使聚烯烃中所含溶剂如1-丁烯异物。因此，回收的溶剂不能完全循环使用，一般要进行后续提纯而除去异物化产物。
本发明目的是弥补这些缺陷，其中提出氧化铝吸附剂，其异物化能力低，易于制成球形，而一般是制成易于制取的形状。
因此，本发明提出烯烃提纯用的氧化铝吸附剂，其中含至少一种碱金属或碱土金属的化合物，含量为15-100mmol元素/100g氧化铝。
除另有说明而外，浓度均以mmol元素/100g300℃下熔烧3小时的氧化铝计。
该吸附剂的烯烃异物化能力低。
吸附剂异物化能力由以下试验测定：
进行1-丁烯异构成顺和反式2-丁烯的能力即可确定这些产物的异构化能力。
为此，将500mg粉碎吸附剂（粒径约400-500mm）引入反应器。250℃下向该产品吹氦气，历时2小时，流量为2.5l/h。
然后将该产品加热到400℃，用氦气引入1ml丁烯。
色谱分析流出的气体即可确定1-丁烯量以及回收到的顺和反式2-丁烯量。
计算出势力平衡常数Kth（T），实测出真实平衡常数K（T）。
Kth（T）＝ ([顺式2-丁烯]e+[反式2-丁烯]e)/([1-丁烯]e+[顺式2-丁烯]e+[反式2-丁烯]e)
K（T）＝ ([顺式2-丁烯]+[反式2-丁烯])/([1-丁烯]+[顺式2-丁烯]+[反式2-丁烯])
T为反应器出口处丁烯的温度，其它值为温度T下反应器出口处或平衡「」e时的浓度。
异物化能力或异物率A（T）如下式：
A（T）＝ (K（T）)/(Kth(T)) ×100
本发明中各元素化合物为氧化物，氢氧化物或盐。当然，用其混合物也属本发明。
这些化合物例子可举出氢氧化物，硫酸盐，硝酸盐，卤化物，乙酸盐，甲酸盐，碳酸盐，一般用羧酸盐。
本发明优选化合物为氢氧化物和氯化物。这些化合物很经济，可制成异物率相当低的吸附剂。
还可用这些元素的混合物，不过，其总含量应优选在15-100mmol/100g氧化铝范围内。
优选元素可举出/钠，钾和钙。
但是，采用钠时，含量应优选达到15-80mmol。
本发明氧化铝可举出其比表面积足以达到工业化金属吸附率的氧化铝。一般来说，其比表面积大于50m2/g。
这些氧化铝制法是常规方法如沉淀或凝胶法以及氢氧化铝快速脱水法。
后一方法制成的氧化铝为本发明优选。
将一种或多种元素加入氧化铝可用各种方法进行，如将元素与氧化铝共沉积或在氧化铝成形之前或之后用一种或多种元素的一种或多种化合物的溶液浸渍。
本发明优选吸附剂制法是用待加入元素的盐或氢氧化物水溶液浸渍球状氧化铝，然后干燥并在必要时进行热处理以使其比表面积稳定。
热处理温度与应用温度或要求比表面积有关。
还可在更高温度下进行热处理以使化合物至少部分热解成氧化物。但是，这样热解并不必须，特别是在应用氯化物，硝酸盐，氢氧化物时并不必须。
本发明吸附剂可用于提纯烯烃在配位催化剂存在下聚合所得聚烯烃，其中将来自催化剂的金属吸附出来。因此，反应混合物中所含烯烃得以提纯，同时又不会异物，所以说可完全循环使用。
该法也可用于提纯聚烯烃。
以下非限制性实例详述本发明。
以下吸附剂制法是处理球状氧化铝，其粒径为1.5-2.5mm，BET比表面积为295m2/g，总孔体积为0.5cm2/g，剩余钠含量为0.2-0.4wt%。
这种氧化铝球由罗纳一布郎克公司以商名“A1.5-2.5”出售。
该氧化铝球在空气中300℃下活化3小时，然后用一种或多种元素的盐或化合物如其氢氧化合物溶液浸渍。该溶液的体积和浓度应使氧化铝中元素达到要求的浓度。
浸渍产品在空气中于110℃干燥12小时。
其异物能力由上述试验确定。
所得结果及吸附剂特性列于下表。
结果清楚地表明含元素钠，钾，钙素的氧化铝的异物能力大大低于未处理氧化铝的异物能力（实例1）。而且，这些实例还表明在规定浓度范围内可降低氧化铝的异物能力。
此外，含杂质钠的未处理氧化铝不能用，因为钠浓度太低。
用于吸附酸性杂质的含高百分比钠（5%或以上）氧化铝也是一样。
含铝，锶和镁的氧化铝的异构能力同样大大低于未处理氧化铝的异构能力（实例1）。
元素
实例    x    浸渍溶液    吸附剂中X的浓度    异构能力
A%
mmole/100gAl2O3
1（1）    -    -    0    63%
2    Na    NaOH    25    14%
3    Na    NaOH    62    5%
4（1）    Na    NaOH    250    54%
5    K    KOH    26    8%
6    K    KOH    68    14%
7    K    KOH    15    16%
8（2） Ca Ca（COOCH3）244 13%
9（2） Ca Ca（OOCCH3）218 21%
10（2） Na NaOOCCH336 9%
11（2） Na CH3COONa 90 9%
12    Na    NaCl    65    1%
13（1）    Na    NaOH    12    42%
14（1）    K    KOH    130    77%
15（2） Li CH3COOLi 45 14%
16（2） Sr Sr（OOCCH3）265 36%
17（2） Mg Mg（OOCH3）265 36%
18 Ca CaCl245 11%
（1）比较试验
（2）浸渍后600℃下焙烧3小时

Claims (9)

1、在配位催化剂体系存在下聚合所得聚烯烃提纯方法，其特征在于该方法在一种氧化铝吸附剂存在下进行，该吸附剂中包含至少一种选自碱金属，碱土金属的元素化合物，该元素含量为15-100mmol/100g氧化铝。
2、权利要求1的方法，其特征在于元素化合物为氧化物，氢氧化物或盐。
3、权利要求1或2的方法，其特征在于元素化合物为硫酸盐，硝酸盐，卤化物，乙酸盐，甲酸盐，碳酸盐或羧酸盐。
4、权利要求1-3之一的方法，其特征在于元素化合物为氯化物或氢氧化物。
5、权利要求1-4之一的方法，其特征在于元素选自钠，钾，钙。
6、权利要求5的方法，其特征在于钾用量为15-80mmol/100g氧化铝。
7、前述权利要求之一的方法，其特征在于氧化铝比表面积为50m2/g。
8、前述权利要求之一的方法，其特征在于吸附剂呈球形。
9、前述权利要求之一的方法，其特征在于氧化铝由氢氧化铝快速脱水而得。
CN90100255A 1989-01-18 1990-01-18 聚烯烃提纯用的吸附剂及其制法 Expired CN1017685B (zh)

Applications Claiming Priority (2)

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FR8900530A FR2641711B1 (fr) 1989-01-18 1989-01-18 Adsorbant pour purification de polyolefines et procede de fabrication de celui-ci
FR89/00530 1989-01-18

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CN1044415A CN1044415A (zh) 1990-08-08
CN1017685B true CN1017685B (zh) 1992-08-05

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BR9000167A (pt) 1990-10-23
JPH0628725B2 (ja) 1994-04-20
MX172197B (es) 1993-12-06
CA2007937C (fr) 1998-11-03
CA2007937A1 (fr) 1990-07-18
DE69007989D1 (de) 1994-05-19
JPH02233137A (ja) 1990-09-14
FR2641711A1 (fr) 1990-07-20
KR900011506A (ko) 1990-08-01
DK0379394T3 (da) 1994-05-16
ES2055348T3 (es) 1994-08-16
DE69007989T2 (de) 1994-08-18
ATE104172T1 (de) 1994-04-15
CN1044415A (zh) 1990-08-08
BG90933A (bg) 1993-12-24
AU4797390A (en) 1990-07-26
AU634740B2 (en) 1993-03-04
AR244574A1 (es) 1993-11-30
TW203016B (zh) 1993-04-01
BG60545B1 (bg) 1995-08-28
EP0379394A1 (fr) 1990-07-25
EP0379394B1 (fr) 1994-04-13
KR960000497B1 (ko) 1996-01-08
FR2641711B1 (fr) 1993-10-22

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