公开(公告)号：EP1043051A3

公开(公告)日：2002-12-11

申请号：EP00101051.1

申请日：2000-01-20

申请人： F. HOFFMANN-LA ROCHE AG

发明人： Fleck, Ute

IPC分类号： B01D15/00 ,  B01J20/30 ,  C07D311/72

CPC分类号： B01D15/00 ,  B01J20/08 ,  B01J20/103 ,  B01J20/18 ,  B01J20/20 ,  B01J20/3433 ,  B01J20/3475 ,  B01J20/3483 ,  B01J20/3491 ,  B01J2220/56 ,  B01J2220/58 ,  C11B1/104 ,  Y02P20/544

摘要： The invention relates to a process for preparing a highly loaded adsorbent, which process comprises the steps of a) extracting an oil from an oil crude product by means of supercritical fluid extraction thus, obtaining a loaded supercritical fluid (SCF); b) expanding the loaded SCF of step a) followed by heating to obtain a liquid phase and a in-loading reduced SCF phase; c) optionally decreasing the pressure and/ or raising the temperature of the SCF phase of step b) to conditions of adsorption; d) introducing the SCF of step b) or step c) into a fixed bed adsorber to obtain an adsorbent loaded with the purified oil and pure SCF; e) feeding the liquid phase of step b) as a reflux to the extraction device of step a) ; f) compressing and tempering the pure SCF of step d) to extraction conditions; g) recycling the pure SCF to the extraction device of step a). The invention further comprises a process for purifying an oil from an oil crude product by desorbing the adsorbed oil. The invention further comprises 16 A process for purifying an oil, optionally combined with a process for preparing a highly loaded adsorbent, which process comprises the steps of: A) extracting a fraction containing the oil together with high volatile components from a crude synthetic or natural oil mixture by means of supercritical fluid extraction (SFE) thus, obtaining a loaded supercritical fluid (SCF) and a raffinate containing the low volatile components of the crude product; B) expanding the loaded SCF of step A) followed by heating to obtain a liquid phase containing the oil and high volatile components and an unloaded gas phase (step B-1) or to obtain an in-loading reduced SCF and a liquid phase (step B-2); C) optionally decreasing the pressure and/ or raising the temperature of the in-loading reduced SCF phase of step B-2) to conditions of adsorption; D) optionally introducing the in-loading reduced SCF of step B-2) or of step C) into a fixed bed adsorber to obtain an unloaded gas phase and an adsorbent loaded with oil; E) collecting the unloaded gas phase of step B-1) or of step D) in a vessel and controlling the content of the gas components; F) optionally feeding pure gas into the vessel of step E) to guarantee the same gas composition over the whole process time; G) feeding part of the liquid phase of step B-1) or all of the liquid phase of step B-2) at the same temperature and pressure of the column as a reflux to the extraction device of step A); H) pressurizing the gas phase of step E) or of step F) followed by cooling to separation conditions; I) recycling the SCF of step H to the extraction device of step A); J) optionally feeding the liquid phase of step B-1) to a second extraction device; K) extracting a fraction of high volatile components from the extract of step B-1) by means of SFE thus obtaining a loaded SCF and the pure oil as raffinate; L) treating the reflux and the SCF as described in the steps B-1 - I); M) collecting the oil at the bottom of the column as a raffinate.

公开(公告)号：EP1043051A2

公开(公告)日：2000-10-11

申请号：EP00101051.1

申请日：2000-01-20

申请人： F. HOFFMANN-LA ROCHE AG

发明人： Fleck, Ute

IPC分类号： B01D15/00 ,  B01J20/30 ,  C07D311/72

CPC分类号： B01D15/00 ,  B01J20/08 ,  B01J20/103 ,  B01J20/18 ,  B01J20/20 ,  B01J20/3433 ,  B01J20/3475 ,  B01J20/3483 ,  B01J20/3491 ,  B01J2220/56 ,  B01J2220/58 ,  C11B1/104 ,  Y02P20/544

摘要： The invention relates to a process for preparing a highly loaded adsorbent, which process comprises the steps of

a) extracting an oil from an oil crude product by means of supercritical fluid extraction thus, obtaining a loaded supercritical fluid (SCF);
b) expanding the loaded SCF of step a) followed by heating to obtain a liquid phase and a in-loading reduced SCF phase;
c) optionally decreasing the pressure and/ or raising the temperature of the SCF phase of step b) to conditions of adsorption;
d) introducing the SCF of step b) or step c) into a fixed bed adsorber to obtain an adsorbent loaded with the purified oil and pure SCF;
e) feeding the liquid phase of step b) as a reflux to the extraction device of step a) ;
f) compressing and tempering the pure SCF of step d) to extraction conditions;
g) recycling the pure SCF to the extraction device of step a).

The invention further comprises a process for purifying an oil from an oil crude product by desorbing the adsorbed oil.
The invention further comprises 16 A process for purifying an oil, optionally combined with a process for preparing a highly loaded adsorbent, which process comprises the steps of:

A) extracting a fraction containing the oil together with high volatile components from a crude synthetic or natural oil mixture by means of supercritical fluid extraction (SFE) thus, obtaining a loaded supercritical fluid (SCF) and a raffinate containing the low volatile components of the crude product;
B) expanding the loaded SCF of step A) followed by heating to obtain a liquid phase containing the oil and high volatile components and an unloaded gas phase (step B-1) or to obtain an in-loading reduced SCF and a liquid phase (step B-2);
C) optionally decreasing the pressure and/ or raising the temperature of the in-loading reduced SCF phase of step B-2) to conditions of adsorption;
D) optionally introducing the in-loading reduced SCF of step B-2) or of step C) into a fixed bed adsorber to obtain an unloaded gas phase and an adsorbent loaded with oil;
E) collecting the unloaded gas phase of step B-1) or of step D) in a vessel and controlling the content of the gas components;
F) optionally feeding pure gas into the vessel of step E) to guarantee the same gas composition over the whole process time;
G) feeding part of the liquid phase of step B-1) or all of the liquid phase of step B-2) at the same temperature and pressure of the column as a reflux to the extraction device of step A);
H) pressurizing the gas phase of step E) or of step F) followed by cooling to separation conditions;
I) recycling the SCF of step H to the extraction device of step A);
J) optionally feeding the liquid phase of step B-1) to a second extraction device;
K) extracting a fraction of high volatile components from the extract of step B-1) by means of SFE thus obtaining a loaded SCF and the pure oil as raffinate;
L) treating the reflux and the SCF as described in the steps B-1 - I);
M) collecting the oil at the bottom of the column as a raffinate.

摘要翻译： 本发明涉及一种制备高负载吸附剂的方法，该方法包括以下步骤：a）通过超临界流体萃取从油粗产物中提取油，从而获得负载的超临界流体（SCF）; b）扩展步骤a）的加载SCF，然后加热以获得液相和负载减少的SCF相; c）任选地将步骤b）的SCF相的压力和/或升高温度降低至吸附条件; d）将步骤b）或步骤c）的SCF引入固定床吸附器中以获得负载纯化油和纯SCF的吸附剂; e）将步骤b）的液相作为回流进料到步骤a）的萃取装置中; f）将步骤d）的纯SCF压缩回火至萃取条件; g）将纯SCF回收到步骤a）的提取装置。 本发明还包括通过解吸吸附的油从油粗产物中提纯油的方法。 本发明还包括用于纯化油的方法，任选地与制备高负载吸附剂的方法组合，该方法包括以下步骤：A）从粗合成或天然的粗制提取含有油的馏分和高挥发性组分 通过超临界流体萃取（SFE）的油混合物，从而获得装载的超临界流体（SCF）和含有粗产物的低挥发性组分的萃余液; B）扩展步骤A）的加载SCF，然后加热以获得含有油和高挥发性组分和无载气相（步骤B-1）的液相，或获得负载减小的SCF和液相（ 步骤B-2）; C）任选地将步骤B-2的负载降低的SCF相的压力和/或升高温度降低至吸附条件; D）任选地将步骤B-2）或步骤C）的负载减小的SCF引入固定床吸附器中以获得负载的气相和装载油的吸附剂; E）在容器中收集步骤B-1）或步骤D）的无载气相并控制气体组分的含量; F）任选地将纯气体进入到步骤E）的容器中以在整个处理时间内保证相同的气体组成; G）将步骤B-1）的液相的一部分或步骤B-2的所有液相）在塔的相同温度和压力下进料到步骤A）的提取装置; H）对步骤E）或步骤F）的气相加压，然后冷却至分离条件; I）将步骤H的SCF再循环到步骤A）的提取装置中; J）任选地将步骤B-1）的液相进料送入第二提取装置; K）通过SFE从步骤B-1的提取物中提取一部分高挥发性组分，从而获得负载的SCF，纯油作为提余液; L）如步骤B-1-I）所述处理回流和SCF; M）作为萃余液收集柱底部的油。