CN108325567A - A kind of regeneration method of supported ruthenium catalyst - Google Patents
A kind of regeneration method of supported ruthenium catalyst Download PDFInfo
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- CN108325567A CN108325567A CN201810202233.8A CN201810202233A CN108325567A CN 108325567 A CN108325567 A CN 108325567A CN 201810202233 A CN201810202233 A CN 201810202233A CN 108325567 A CN108325567 A CN 108325567A
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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
- B01J38/00—Regeneration or reactivation of catalysts, in general
- B01J38/48—Liquid treating or treating in liquid phase, e.g. dissolved or suspended
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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
- B01J38/00—Regeneration or reactivation of catalysts, in general
- B01J38/04—Gas or vapour treating; Treating by using liquids vaporisable upon contacting spent 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
- B01J38/00—Regeneration or reactivation of catalysts, in general
- B01J38/48—Liquid treating or treating in liquid phase, e.g. dissolved or suspended
- B01J38/50—Liquid treating or treating in liquid phase, e.g. dissolved or suspended using organic liquids
- B01J38/52—Liquid treating or treating in liquid phase, e.g. dissolved or suspended using organic liquids oxygen-containing
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Abstract
The invention discloses the regeneration methods that a kind of supercritical fluid is used for supported ruthenium catalyst, include the following steps：Inactivation ruthenium catalyst is detached with reaction solution, the catalyst distilled water flushing that will be isolated；Ruthenium catalyst after flushing is put into the hanging basket of autoclave, and adds a small amount of cosolvent, then seals reaction kettle；Reaction kettle is heated to 50 DEG C~120 DEG C, carbon dioxide is injected thereto to preset 7.5~12.0MPa of pressure by 80 simplex pumps of high pressure DB, impregnate 60~180 min, it is down to room temperature, carbon dioxide therein is slowly discharged into the container equipped with water by air bleeding valve, it is emptied after water absorbs, dismantles reaction kettle, take out hanging basket.The present invention utilizes the strong diffusivity of supercritical fluid, strong solubility, and the load ruthenium catalyst of inactivation can be made to obtain efficient, free of contamination regeneration, and there is regenerating medium environmental protection to be easy to get, and the recovery time is short, and regeneration efficiency is high, advantage at low cost.
Description
Technical field
The present invention relates to a kind of regeneration methods of supported ruthenium catalyst, are produced for glucose hydrogenation more particularly to one kind
The sorbierite regeneration method of ruthenium/carbon loaded type catalyst, belongs to technical field of fine.
Background technology
Noble metal catalyst is since its excellent catalytic performance in catalytic field occupies extremely important status, in support type
In your catalyst, load ruthenium is important noble metal catalyst, and ruthenium has in the catalysis oxidation of organic matter such as alkene and alcohol
Activity;Hydrogenation also with good carbonyl etc. simultaneously, realizes the industrialization of synthesis ammonia under low-temp low-pressure, bears
It is extensive to carry ruthenium catalyst application field.
Sorbierite is the abbreviation of D-sorbite, is emerging in recent years important fine chemical product.Sorbierite has extensive
Purposes, be a kind of important raw material of industry, it is pleasantly sweet due to odorless, nontoxic, be approved as by the additive committee of the United Nations
The unrestricted food additives of dosage；It has unique moisture retention, and the product after addition can be made to keep moisture stable；It is
Excellent emulsifier simultaneously plays the role of that microorganism is inhibited to prevent corruption；It still synthesizes other compounds (such as vitamin C, department
Disk -60 etc.) intermediate etc., thus in the industrial circles such as food, daily-use chemical industry, tobacco, pharmacy, papermaking, weaving, coating
It has been more and more widely used.Industrial sorbierite is mainly produced by glucose hydrogenation, and catalyst is glucose hydrogenation production
The key of sorbierite.From nineteen forty-two, Japan by glucose in suspended catalyst since hydro-reduction production sorbierite, for
The various problems occurred in catalytic hydrogenation, people are constantly improved catalyst, to improve activity, the choosing of catalyst
Selecting property, stability etc., the catalyst that traditional handicraft uses are Raney's nickels, due to supported ruthenium catalyst have it is high active, mild
The advantages such as reaction condition, high hydrogenation selectivity, more and more made by people in the new process of production sorbierite
With.
There are the deactivation prob of catalyst during the use of catalyst, the main reason for inactivation, has：Catalyst poison
For example occupy activated centre containing halogen, sulfur-bearing, phosphorous compound；Macromolecules adsorption in reactant is in activated centre or blocking
The duct of catalyst；For the ruthenium catalyst that glucose hydrogenation uses, it is the mistake for producing glucose to lead to the main reason for inactivating
The organic macromolecules such as remaining acid group chlorion, maltose and protein in journey.Especially now widely used enzyme process sugar life
It is to cause to load ruthenium that the organic macromolecules such as production. art, maltose and protein, which are adsorbed on activated centre or the duct of blocking catalyst,
The main reason for catalyst inactivation, this makes the access times of catalyst reduce, and efficiency declines, and use cost increases, this point
Seem for noble metal catalyst and particularly most wants.Therefore carrying out regeneration treatment to such decaying catalyst has important show
Sincere justice, regeneration method mainly wash or with high temperature steam treatment repeatedly by useful highly basic hot solution at present, such as：
ZL001267.7 discloses a kind of palladium catalyst of fixed bed hydrogen dioxide solution production by anthraquinone process, and this method uses steam regeneration, utilizes
The high temperature of low pressure water vapor（100~120 DEG C）With the dissolubility of condensed water, it is molten that organic impurities of palladium catalyst etc. will be adsorbed on
Solution, dredges the duct of catalyst carrier, to make the activity of catalyst be restored, though the regeneration techniques are economical, simple, this
A little methods are inefficient, it is difficult to the tamper in catalyst duct is cleaned out, and regeneration times are limited, catalyst is through multiple
Activity declines quickly after regeneration, and causes largely to dispose waste liquid, and causes certain environmental pollution.In order to solve present on
Problem, people have been working hard seek a kind of ideal technical solution.
Supercritical fluid (SCF) technology is new technology developed in recent years, and supercritical fluid refers to being in stagnation temperature
Degree（Tc）And critical pressure（Pc）On special fluid, supercritical fluid have a series of properties：Its viscosity is relatively low,
Diffusion coefficient is big, these properties are sufficiently close to gas, thus supercritical fluid is made to have the biographies such as good flowing, mass transfer, heat transfer
Pass performance；For its density and solvability in close proximity to liquid, supercritical fluid is higher than gas to the solvability of solid by 10
~100 times, supercritical fluid can be by pressure come modulation to the solvability of solid；Supercritical fluid has very low surface
Tension makes it have excellent surface wettability and penetrating power；Supercritical fluid has good compatibility with gas.Due to
High diffusibility and permeability, strong dissolubility, the excellent surface wettability etc. of supercritical fluid make it become all kinds of chemistry
The potential good medium of new material is reacted, synthesized and prepared, the hot spot that domestic and international research prepares new material is become.Common
In supercritical fluid, most commonly used research is supercritical carbon dioxide (SCCO2), because supercritical carbon dioxide has not
Combustion, nontoxic, inexpensive, environmentally friendly and critical-temperature close to room temperature and lower critical pressure (Tc=31.1 DEG C, Pc=
7.38MPa), physics and chemical property differ markedly from traditional organic liquid solvent, this multi-functional " green haveing excellent performance
Solvent " has become the new motive force of chemistry and material subject development, and is just showing wide application prospect.
Therefore the effective removing of production practices needs is adsorbed on catalyst active center or blocking catalyst duct and has
Machine macromolecular makes the activity of catalyst obtain regeneration method.
Invention content
The characteristics of it is an object of the invention to using supercritical fluid media, provide a kind of regeneration side of supported ruthenium catalyst
Method.Its principle is reliable, and preparation process is simple, non-environmental-pollution, can effectively remove and be adsorbed on catalyst active center or stifled
The organic macromolecule for filling in catalyst duct, makes the activity of catalyst be regenerated, reduces the use cost of noble metal catalyst.
Technical scheme of the present invention：
A kind of regeneration method of supported ruthenium catalyst, this method include the following steps：
1）The ruthenium catalyst of inactivation is detached with reaction solution;
2）Catalyst distilled water flushing after above-mentioned separation is clean；
3）One magnetic stir bar is put into autoclave, and cosolvent is added；
4) the above-mentioned inactivation ruthenium catalyst rinsed well is put into the hanging basket of autoclave, and seals reaction kettle；
5）The temperature of reaction kettle is adjusted to 50 DEG C~120 DEG C；
6）Carbon dioxide is injected into autoclave to 7.5~12.0 MPa of preset pressure by high pressure DB-80 simplex pumps；
6）Magnetic stirring apparatus is started, 60~180min of impregnation time is controlled；
7）Reaction kettle is cooled to room temperature, carbon dioxide therein is slowly discharged into the container equipped with water by air bleeding valve, through water
It is emptied after absorption.
8）Reaction kettle is dismantled, hanging basket is taken out, you can obtains regeneration ruthenium catalyst.
Further, the cosolvent is one kind in methanol, ethyl alcohol, acetone or combinations thereof object；A small amount of cosolvent is 1~
3ml。
Further, the ruthenium catalyst of the inactivation includes filter filtering, sedimentation separation with liquid separating method is reacted
Or centrifugation.
Further, the supported ruthenium catalyst is a series of catalyst that ruthenium is carried on carrier.
Further, the carrier includes：Activated carbon, activated alumina, ZSM-5 molecular sieve, silica, carbon nanometer
Pipe.
The beneficial effects of the present invention are：
It is steeping medium by using supercritical carbon dioxide, utilizes the high diffusibility of supercritical fluid, strong dissolubility, excellent
Surface wettability and strong penetrating power, by the temperature of adjusting control supercritical fluid, pressure, and pass through add cosolvent
The organic macromolecule for being adsorbed on catalyst active center or blocking catalyst duct is cleaned out, the activity of catalyst is made to obtain
Effectively restore.
Carbon dioxide regenerating medium used is cheap and easy to get, and regenerative process does not generate waste liquid, will not cause dirt to environment
Dye.
The inventive method regeneration technology is simple, and the recovery time is short, easy to operate, at low cost, makes the active regeneration of catalyst
It is efficient, the access times of catalyst can be effectively increased, the use cost of noble metal catalyst is effectively reduced.
Specific implementation mode
Below by specific embodiment, the present invention is described in further detail.
Embodiment 1
The ruthenium catalyst of inactivation and reaction product sorbierite mixed liquor are subjected to sedimentation separation；By the catalyst distillation after separation
Water is rinsed well, is filtered with filter；One magnetic stir bar is put into 50ml autoclaves, and anhydrous second is added
Alcohol cosolvent 1ml；It takes above-mentioned clean filtered inactivation ruthenium catalyst 2g to be put into the hanging basket of autoclave, and seals reaction
Kettle；The temperature of reaction kettle is adjusted to 50 DEG C；Then carbon dioxide is injected into autoclave by high pressure DB-80 simplex pumps to super to face
8.0 MPa of boundary's pressure；Magnetic stirring apparatus is started, impregnation time 60min is controlled；Hypothermic response kettle temperature degree passes through to room temperature
Carbon dioxide therein is slowly discharged into the container equipped with water by air bleeding valve, is emptied after water absorbs；Reaction kettle is dismantled, taking-up is hung
Basket, you can obtain regeneration ruthenium catalyst.
The activity of regenerated catalyst reaches the 90.3% of fresh ruthenium catalyst.
Embodiment 2
The ruthenium catalyst of inactivation and reaction product sorbierite mixed liquor are subjected to sedimentation separation；By the catalyst distillation after separation
Water is rinsed well, is filtered with filter；One magnetic stir bar is put into 50ml autoclaves, and is added without water beetle
Alcohol cosolvent 1ml；It takes above-mentioned clean filtered inactivation ruthenium catalyst 2g to be put into the hanging basket of autoclave, and seals reaction
Kettle；The temperature of reaction kettle is adjusted to 60 DEG C；Then carbon dioxide is injected into autoclave by high pressure DB-80 simplex pumps to super to face
8.0 MPa of boundary's pressure；Magnetic stirring apparatus is started, impregnation time 60min is controlled；Hypothermic response kettle temperature degree passes through to room temperature
Carbon dioxide therein is slowly discharged into the container equipped with water by air bleeding valve, is emptied after water absorbs；Reaction kettle is dismantled, taking-up is hung
Basket, you can obtain regeneration ruthenium catalyst.
The activity of regenerated catalyst reaches the 89.5% of fresh ruthenium catalyst.
Embodiment 3
The ruthenium catalyst of inactivation and reaction product sorbierite mixed liquor are subjected to sedimentation separation；By the catalyst distillation after separation
Water is rinsed well, is filtered with filter；One magnetic stir bar is put into 50ml autoclaves, and is added anhydrous
Ethanol co-solvent 1ml；It takes above-mentioned clean filtered inactivation ruthenium catalyst 2g to be put into the hanging basket of autoclave, and seals anti-
Answer kettle；The temperature of reaction kettle is adjusted to 80 DEG C；Then carbon dioxide is injected into autoclave to super by high pressure DB-80 simplex pumps
10.0 MPa of critical pressure；Magnetic stirring apparatus is started, impregnation time 60min is controlled；Hypothermic response kettle temperature degree leads to room temperature
It crosses air bleeding valve and carbon dioxide therein is slowly discharged into the container equipped with water, emptied after water absorbs.Reaction kettle is dismantled, is taken out
Hanging basket, you can obtain regeneration ruthenium catalyst.
The activity of regenerated catalyst reaches the 92.6% of fresh ruthenium catalyst.
Embodiment 4
The ruthenium catalyst of inactivation and reaction product sorbierite mixed liquor are subjected to sedimentation separation；By the catalyst distillation after separation
Water is rinsed well, is filtered with filter；One magnetic stir bar is put into 50ml autoclaves, and anhydrous second is added
Alcohol cosolvent 1ml；It takes above-mentioned clean filtered inactivation ruthenium catalyst 2g to be put into the hanging basket of autoclave, and seals reaction
Kettle；The temperature of reaction kettle is adjusted to 100 DEG C；Then carbon dioxide is injected into autoclave to super by high pressure DB-80 simplex pumps
11.0 MPa of critical pressure；Magnetic stirring apparatus is started, impregnation time 100min is controlled；Hypothermic response kettle temperature degree to room temperature,
Carbon dioxide therein is slowly discharged into the container equipped with water by air bleeding valve, is emptied after water absorbs；Reaction kettle is dismantled, is taken
Go out hanging basket, you can obtain regeneration ruthenium catalyst.
The activity of regenerated catalyst reaches the 91.8% of fresh ruthenium catalyst.
Embodiment 5
The ruthenium catalyst of inactivation and reaction product sorbierite mixed liquor are subjected to sedimentation separation；By the catalyst distillation after separation
Water is rinsed well, is filtered with filter；One magnetic stir bar is put into 50ml autoclaves, and is added anhydrous
Ethanol co-solvent 1ml；It takes above-mentioned clean filtered inactivation ruthenium catalyst 2g to be put into the hanging basket of autoclave, and seals anti-
Answer kettle；The temperature of reaction kettle is adjusted to 100 DEG C；Then carbon dioxide is injected extremely into autoclave by high pressure DB-80 simplex pumps
12.0 MPa of supercritical pressure；Magnetic stirring apparatus is started, 120 min of impregnation time is controlled；Hypothermic response kettle temperature degree is to room
Carbon dioxide therein is slowly discharged into the container equipped with water by air bleeding valve, is emptied after water absorbs by temperature.Dismantle reaction
Kettle takes out hanging basket, you can obtains regeneration ruthenium catalyst.
The activity of regenerated catalyst reaches the 93.2% of ruthenium fresh catalyst.
Embodiment 6
The ruthenium catalyst of inactivation and reaction product sorbierite mixed liquor are subjected to sedimentation separation；By the catalyst distillation after separation
Water is rinsed well, is filtered with filter；One magnetic stir bar is put into 50ml autoclaves, and acetone is added
Cosolvent 2ml；It takes above-mentioned clean filtered inactivation ruthenium catalyst 2g to be put into the hanging basket of autoclave, and seals reaction
Kettle；The temperature of reaction kettle is adjusted to 90 DEG C；Then carbon dioxide is injected into autoclave by high pressure DB-80 simplex pumps to super to face
12.0 MPa of boundary's pressure；Magnetic stirring apparatus is started, 120 min of impregnation time is controlled；Hypothermic response kettle temperature degree leads to room temperature
It crosses air bleeding valve and carbon dioxide therein is slowly discharged into the container equipped with water, emptied after water absorbs.Reaction kettle is dismantled, is taken out
Hanging basket, you can obtain regeneration ruthenium catalyst.
The activity of regenerated catalyst reaches the 93.6% of ruthenium fresh catalyst.
Claims (5)
1. a kind of regeneration method of supported ruthenium catalyst, it is characterised in that:Supercritical fluid is supercritical carbon dioxide, the party
Method includes the following steps：
1）The ruthenium catalyst of inactivation is detached with reaction solution;
2）Catalyst distilled water flushing after above-mentioned separation is clean；
3）One magnetic stir bar is put into autoclave, and cosolvent is added；
4) the above-mentioned inactivation ruthenium catalyst rinsed well is put into the hanging basket of autoclave, and seals reaction kettle；
5）The temperature of reaction kettle is adjusted to 50 DEG C~120 DEG C；
6）Carbon dioxide is injected into autoclave to 7.5~12.0 MPa of preset pressure by high pressure DB-80 simplex pumps；
6）Magnetic stirring apparatus is started, 60~180min of impregnation time is controlled；
7）Reaction kettle is cooled to room temperature, carbon dioxide therein is slowly discharged into the container equipped with water by air bleeding valve, through water
It is emptied after absorption;
8）Reaction kettle is dismantled, hanging basket is taken out, you can obtains regeneration ruthenium catalyst.
2. requiring a kind of regeneration method of supported ruthenium catalyst according to right 1, it is characterised in that：The cosolvent is first
One kind in alcohol, ethyl alcohol, acetone or combinations thereof object；A small amount of cosolvent is 1~3ml.
3. requiring a kind of regeneration method of supported ruthenium catalyst according to right 1, it is characterised in that：The ruthenium of the inactivation
Catalyst includes filter filtering, sedimentation separation or centrifugation with liquid separating method is reacted.
4. requiring a kind of regeneration method of supported ruthenium catalyst according to right 1, it is characterised in that：The load ruthenium is urged
Agent is a series of catalyst that ruthenium is carried on carrier.
5. requiring a kind of regeneration method of supported ruthenium catalyst according to right 1, it is characterised in that：The carrier includes：
Activated carbon, activated alumina, ZSM-5 molecular sieve, silica, carbon nanotube.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111760598A (en) * | 2020-07-08 | 2020-10-13 | 西安闪光能源科技有限公司 | Catalyst regeneration method and regenerator |
| CN112169847A (en) * | 2020-09-25 | 2021-01-05 | 南京大学 | Ruthenium-based catalyst activation regeneration method and application thereof |
| CN115805103A (en) * | 2021-09-14 | 2023-03-17 | 万华化学集团股份有限公司 | Regeneration method of deactivated titanium-silicon molecular sieve |
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| CN1762601A (en) * | 2004-10-22 | 2006-04-26 | 中国石油化工股份有限公司 | A kind of process of reproducing catalyst by supercritical fluid |
| JP2012143754A (en) * | 2011-01-11 | 2012-08-02 | Eurecat Sa | Off-site regeneration method of solid catalyst |
| CN104588133A (en) * | 2015-01-04 | 2015-05-06 | 河海大学 | Heterogeneous ruthenium catalyst regeneration method |
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2018
- 2018-03-12 CN CN201810202233.8A patent/CN108325567A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1762601A (en) * | 2004-10-22 | 2006-04-26 | 中国石油化工股份有限公司 | A kind of process of reproducing catalyst by supercritical fluid |
| JP2012143754A (en) * | 2011-01-11 | 2012-08-02 | Eurecat Sa | Off-site regeneration method of solid catalyst |
| CN104588133A (en) * | 2015-01-04 | 2015-05-06 | 河海大学 | Heterogeneous ruthenium catalyst regeneration method |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111760598A (en) * | 2020-07-08 | 2020-10-13 | 西安闪光能源科技有限公司 | Catalyst regeneration method and regenerator |
| CN112169847A (en) * | 2020-09-25 | 2021-01-05 | 南京大学 | Ruthenium-based catalyst activation regeneration method and application thereof |
| CN115805103A (en) * | 2021-09-14 | 2023-03-17 | 万华化学集团股份有限公司 | Regeneration method of deactivated titanium-silicon molecular sieve |
| CN115805103B (en) * | 2021-09-14 | 2024-04-09 | 万华化学集团股份有限公司 | Regeneration method of deactivated titanium-silicon molecular sieve |
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Application publication date: 20180727 |