CN109395754A - A method of recycling heteropolyacid catalyst from chloro propylene epoxidation oil reservoir - Google Patents
A method of recycling heteropolyacid catalyst from chloro propylene epoxidation oil reservoir Download PDFInfo
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- CN109395754A CN109395754A CN201811268760.5A CN201811268760A CN109395754A CN 109395754 A CN109395754 A CN 109395754A CN 201811268760 A CN201811268760 A CN 201811268760A CN 109395754 A CN109395754 A CN 109395754A
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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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/14—Phosphorus; Compounds thereof
- B01J27/186—Phosphorus; Compounds thereof with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J27/188—Phosphorus; Compounds thereof with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium with chromium, molybdenum, tungsten or polonium
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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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/14—Phosphorus; Compounds thereof
- B01J27/186—Phosphorus; Compounds thereof with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J27/188—Phosphorus; Compounds thereof with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium with chromium, molybdenum, tungsten or polonium
- B01J27/19—Molybdenum
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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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/14—Phosphorus; Compounds thereof
- B01J27/186—Phosphorus; Compounds thereof with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J27/195—Phosphorus; Compounds thereof with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium with vanadium, niobium or tantalum
- B01J27/198—Vanadium
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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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/28—Regeneration or reactivation
- B01J27/285—Regeneration or reactivation of catalysts comprising compounds of phosphorus
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D301/00—Preparation of oxiranes
- C07D301/32—Separation; Purification
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D303/00—Compounds containing three-membered rings having one oxygen atom as the only ring hetero atom
- C07D303/02—Compounds containing oxirane rings
- C07D303/08—Compounds containing oxirane rings with hydrocarbon radicals, substituted by halogen atoms, nitro radicals or nitroso radicals
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/584—Recycling of catalysts
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Abstract
The method that the invention discloses a kind of to recycle heteropolyacid catalyst from chloro propylene epoxidation oil reservoir.The described method includes: (1) fills adsorbent into fixed bed；(2) chloro propylene epoxidation oil reservoir is made to flow through the fixed bed containing the adsorbent；(3) it after having handled the chloro propylene epoxidation oil reservoir, will be washed in the fixed bed with water, washing discharging carries out grease layering, and oil reservoir therein is incorporated to untreated chloro propylene epoxidation oil reservoir；(4) fixed bed is flowed through with peroxide solutions, the heteropolyacid catalyst can be oxidized at this time, it is parsed from the adsorbent, after the fixed bed after parsing is washed with the water layer in step (3), the adsorbent be can be recycled；(5) it by the solution vacuum distillation of the heteropolyacid catalyst after parsing, recycles more than kettle.The rate of recovery of the present invention is high, adsorbent is recyclable is recycled, and reduces production cost, is suitble to industrialized production.
Description
Technical field
The present invention relates to catalyst recycling fields, recycle heteropoly acid from chloro propylene epoxidation oil reservoir more particularly to one kind
The method of catalyst.
Background technique
Chloropropene and the hydrogen peroxide Direct Epoxidation under catalyst prepare epoxychloropropane, are a kind of works of green
Skill route meets the technique requirement of clean and environmental protection.Common catalyst is titanium-silicon molecular sieve catalyst in this preparation reaction at present
And heteropolyacid catalyst.When using heteropoly acid to carry out epoxidation reaction for catalyst, catalyst is in and mixes in reaction process
In system, catalyst is precipitated after reaction, is recycled by multi-phase separation.The product generallyd use at present
(epoxychloropropane) separation method is that oil reservoir is first distilled to recover excessive chloropropene, then negative pressure rectification and purification epoxychloropropane.The party
The problem of method is: heteropoly acid has a certain solubility in epoxychloropropane, and there are 0.1~5.0% catalyst in oil reservoir.It is miscellaneous
It can decompose at 80 DEG C of polyacid catalyst or more, release oxygen, there are risk of explosion.And catalyst is acidity, oil reservoir negative pressure
In distillation process, the easy ring opening hydrolysis of epoxychloropropane.
Using hydrogen peroxide as oxidant in Chinese patent CN200610136923, excessive chloropropene is miscellaneous more in catalyst phosphorus tungsten
Synthesizing epoxy chloropropane under the catalysis of sour quaternary amine and co-catalyst alkyl phenol polyoxyethylene ether.Solid-phase catalyst returns in reaction solution
It is recycled after receipts, chloropropene is recovered by distillation in oil reservoir, then is evaporated under reduced pressure purification epoxychloropropane.The patent also indicates that reaction
It is dissolved with catalyst in oil reservoir, in distillation and vacuum distillation process the problem of no more than 80 DEG C of temperature, but does not refer in oil reservoir
The method of catalyst recycling.
A kind of method of catalyst-solvent recycling in epoxychloropropane oil reservoir is described in Chinese patent CN102309993.
It is higher than 130 DEG C of diluent by the way that boiling point is added into oil reservoir, will be clear with water more than kettle after being evaporated under reduced pressure out epoxychloropropane
It washes, recycles catalyst.Catalyst distills for a long time in oil reservoir when this method is distilled, and epoxychloropropane is easy in acid condition
Hydrolysis generates the chloro- 1,2- propylene glycol of 3-.
Chinese patent CN206232636 describes a kind of device of the catalyst recycling recycling of epoxychloropropane processed.
The device includes the groups such as subsider, screw pump, liquid-solid separator, water phase dashpot, water phase membrane filter, oily phase membrane filter
At.The catalyst of device processing is catalyst solid slurry, carries out catalyst recycling by way of sedimentation and film filtering.It should
Device is not described the recycling of a small amount of catalyst dissolved in oil reservoir, and does not provide catalyst actual recovered effect.In the presence of
It is complicated for operation, the long defect of process flow.
Therefore, be badly in need of providing a kind of new method of dissolution recycling heteropolyacid catalyst in slave chloro propylene epoxidation oil reservoir with
Solve existing issue.
Summary of the invention
A kind of the purpose of the present invention is to provide chloropropene and hydrogen peroxide under heteropolyacid catalyst catalysis direct epoxy
After change prepares epoxychloropropane, not only efficiently but also epoxychloropropane hydrolysis ground had been avoided in oil reservoir from chloro propylene epoxidation oil reservoir
The method for recycling heteropolyacid catalyst.
Chloropropene and hydrogen peroxide are prepared the oil reservoir after epoxychloropropane by containing by the present invention under heteropolyacid catalyst
The fixed bed of adsorbent carries out serialization absorption, must recycle catalyst by parsing and vacuum distillation.Catalyst Adsorption rate is high, drop
Low production cost, while can effectively reduce process risk, it is suitble to industrialized production.
To achieve the object of the present invention, the present invention is with the following method: a fills the absorption of certain volume into fixed bed
Agent；B chloro propylene epoxidation oil reservoir flows through the fixed bed containing adsorbent with certain flow rate, and catalyst is adsorbed；C is a certain amount of when handling
Oil reservoir after, is washed with a certain amount of water in fixed bed, washing discharging carries out grease layering, and oil reservoir is incorporated to untreated epoxy
Carburetion layer；D flows through fixed bed with a certain amount of peroxide solutions, and catalyst can be oxidized at this time, parses from adsorbent
Come, after the fixed bed after parsing is washed with the water layer in step c, adsorbent be can be recycled；Catalyst after e parsing
Solution passes through vacuum distillation, and remaining kettle is recycling catalyst.
Heretofore described adsorbent is one of active carbon, molecular sieve, zeolite, activated silica gel, activated alumina etc.
Or it is a variety of.Product comprising above-mentioned adsorbent different model and form, as column-shaped active carbon, cocoanut active charcoal, 5A molecular sieve,
10X molecular sieve etc..
The heteropolyacid catalyst is the transition metal heteropolyacid catalysts such as phosphorus tungsten/molybdenum/vanadic acid.
The adsorption process, adsorption temp are 10~60 DEG C, and preferably 20-30 DEG C, oil reservoir flow velocity is 0.1~5BV/h, preferably
0.5~2BV/h.Wherein BV is bed volume, and BV/h is the flow rate of liquid for flowing through the fixed bed bed volume multiple per hour.
The adsorbance (weight for the catalyst being adsorbed onto) of the adsorbent is the 10%~50% of adsorbent weight.
The flow velocity of water is 0.1~2BV/h in the washing process, and preferably 0.1~0.9BV/h, dosage is adsorbent weight
50~200%, preferably 50~100%, the wash temperature be 10~50 DEG C, preferably 20~30 DEG C.
The parsing agent is peroxide solutions, aqueous hydrogen peroxide solution, 5%-20% peroxide such as concentration 5%-20%
Ethanol solution, 5%-20% sodium carbonate perhydrate aqueous solution and the concentration 0.001%-0.01% ozone water solution of the tert-butyl alcohol
Deng preferred aqueous hydrogen peroxide solution.
In the resolving, parsing agent flow velocity is 0.1~3BV/h, and preferably 0.2~1.2BV/h, dosage is adsorbent weight
50~300%, preferably the 100~200% of amount.
Temperature is 10~60 DEG C when the parsing, preferably 10~50 DEG C, most preferably 20~30 DEG C.
In the distillation process, 20~80 DEG C of temperature, preferably 30~60 DEG C, most preferably 40~50 DEG C, the pressure be-
0.1MPa~0MPa, preferably -0.1~-0.05MPa.
The present invention has the advantages that
(1) of the invention to carry out serialization absorption and parsing catalyst using fixed bed, Catalyst Adsorption rate is high, can be recycled and follows
Ring uses, and reduces production cost, is suitble to industrialized production.
(2) after catalyst is removed by effective absorption in chloro propylene epoxidation oil reservoir, oil reservoir is in neutrality, subsequent purification Shi Keyou
Effect inhibit epoxychloropropane hydrolysis, while can eliminate catalyst thermally decomposed caused by risk of explosion, improve entire technique
Safety.
Specific embodiment
The preparation method of chloro propylene epoxidation oil reservoir: raw material chloropropene and hydrogen peroxide molar ratio 5:1, heteropolyacid catalyst
With hydrogen peroxide molar ratio 1:100,45-50 DEG C of reaction temperature, 4h is reacted.Reaction material liquid grease point after cooling separating catalyst
Layer, obtains chloro propylene epoxidation oil reservoir.
Embodiment 1
Fixed bed is having a size of diameter 5cm, height 30cm, and inside filling 300g granular active carbon, bed volume is (BV)
588.7mL.Catalyst is phosphotungstic acid quaternary phase transfer catalyst (epoxychloropropane 25%, chlorine in chloro propylene epoxidation oil reservoir
Propylene 73%, W content 0.28%), oil reservoir adds up to oil inlet layer 5.0Kg with the flow velocity of 0.5BV/h by fixed bed at 30 DEG C.
Fixed bed is rinsed with the flow velocity of 0.1BV/h with 150g water at 10 DEG C, recycles a small amount of material liquid in fixed bed gap,
The layering of cleaning solution grease, oil reservoir are incorporated in untreated epoxidation oil reservoir, and water layer is for washing fixed bed.
10% aqueous hydrogen peroxide solution that 300g is used at 20 DEG C, flows through fixed bed with the flow velocity of 0.2BV/h, will be adsorbed on
Catalyst on active carbon is parsed, and desorbed solution is carried out vacuum distillation, and 50 DEG C of vapo(u)rizing temperature, pressure -0.1MPa.Kettle mores than 50
Catalyst 30.44g, Catalyst Adsorption rate 93.54% are dried in vacuo to obtain at DEG C.
Parsing terminates, and separates water layer washing fixed bed with step washing, treated, and activated carbon and fixed bed can be carried out directly
It uses next time.
Embodiment 2
Fixed bed is having a size of diameter 5cm, height 30cm, and inside filling 300g granular active carbon, bed volume is (BV)
588.7mL.Catalyst is phosphomolybdic acid quaternary ammonium salt phase transfer catalyst (epoxychloropropane 25%, chlorine in chloro propylene epoxidation oil reservoir
Propylene 73%, molybdenum content 0.18%) at 60 DEG C with the flow velocity of 0.3BV/h by fixed bed, add up to oil inlet layer 10Kg.
Fixed bed is rinsed with the flow velocity of 0.9BV/h with 300g water at 40 DEG C, recycles a small amount of material liquid in fixed bed gap,
The layering of cleaning solution grease, oil reservoir are incorporated in untreated epoxidation oil reservoir, and water layer is for washing fixed bed.
5% aqueous hydrogen peroxide solution that 600g is used at 10 DEG C, flows through fixed bed with the flow velocity of 1.2BV/h, will be adsorbed on
Catalyst on active carbon is parsed, and desorbed solution is carried out vacuum distillation, and 60 DEG C of vapo(u)rizing temperature, pressure -0.095MPa.More than kettle
Catalyst 72.72g, Catalyst Adsorption rate 90.5% are dried in vacuo to obtain at 50 DEG C.
Parsing terminates, and separates water layer washing fixed bed with step washing, treated, and activated carbon and fixed bed can be carried out directly
It uses next time.
Embodiment 3
Fixed bed loads the granulated activated aluminium oxide of 300g having a size of diameter 5cm, height 30cm, inside, and bed volume is
(BV)588.7mL.Catalyst is phosphorus vanadic acid quaternary ammonium salt phase transfer catalyst (epoxychloropropane in chloro propylene epoxidation oil reservoir
25%, chloropropene 73%, content of vanadium 0.41%) at 20 DEG C with the flow velocity of 2.0BV/h by fixed bed, add up to oil inlet layer
5.0Kg。
Fixed bed is rinsed with the flow velocity of 0.5BV/h with 450g water at 50 DEG C, recycles a small amount of material liquid in fixed bed gap,
The layering of cleaning solution grease, oil reservoir are incorporated in untreated epoxidation oil reservoir, and water layer is for washing fixed bed.
The 10% tert-Butanol peroxide ethanol solution that 400g is used at 30 DEG C, flows through fixed bed with the flow velocity of 0.7BV/h, will inhale
Attached catalyst on the activated carbon is parsed, and desorbed solution is carried out vacuum distillation, and 80 DEG C of vapo(u)rizing temperature, pressure
- 0.05MPa, kettle, which is moreed than, is dried in vacuo to obtain catalyst 105.21g, Catalyst Adsorption rate 88.99% at 50 DEG C.
Parsing terminates, and separates water layer washing fixed bed with step washing, treated, and activated carbon and fixed bed can be carried out directly
It uses next time.
Embodiment 4
Fixed bed is having a size of diameter 5cm, height 30cm, and inside filling 300g 10X molecular sieve, bed volume is (BV)
588.7mL.Catalyst is phosphotungstic acid quaternary phase transfer catalyst (epoxychloropropane 25%, chlorine in chloro propylene epoxidation oil reservoir
Propylene 73%, W content 0.28%), oil reservoir adds up to oil inlet layer 5.0Kg with the flow velocity of 0.1BV/h by fixed bed at 10 DEG C.
Fixed bed is rinsed with the flow velocity of 2BV/h with 600g water at 10 DEG C, a small amount of material liquid in fixed bed gap is recycled, washes
The layering of liquid grease is washed, oil reservoir is incorporated in untreated epoxidation oil reservoir, and water layer is for washing fixed bed.
10% aqueous hydrogen peroxide solution that 150g is used at 20 DEG C, flows through fixed bed with the flow velocity of 0.1BV/h, will be adsorbed on
Catalyst on molecular sieve is parsed, and desorbed solution is carried out vacuum distillation, and 50 DEG C of vapo(u)rizing temperature, pressure -0.1MPa.Kettle mores than 50
Catalyst 28.83g, Catalyst Adsorption rate 90.04% are dried in vacuo to obtain at DEG C.
Embodiment 5
Method same as Example 1 recycles catalyst, the difference is that oil reservoir passes through fixed bed and use with 5BV/h flow velocity
Adsorbent be activated silica gel, after vacuum drying catalyst 24.64g, Catalyst Adsorption rate be 75.24%.
Embodiment 6
Method same as Example 1 recycles catalyst, the difference is that parsing agent is water-soluble for the ozone of concentration 0.005%
Liquid, obtains catalyst 29.68g after vacuum drying, Catalyst Adsorption rate is 91.21%.
Embodiment 7
Method same as Example 2 recycles catalyst, the difference is that parsing agent uses the hydrogen peroxide of 900g concentration 5%
Aqueous sodium carbonate is closed, agent flow velocity 3BV/h is parsed, catalyst 73.52g is obtained after vacuum drying, Catalyst Adsorption rate is 91.5%.
Embodiment 8
Method same as Example 3 recycles catalyst, the difference is that temperature is 60 DEG C when absorption and parsing, vacuum drying
Catalyst 101.9g is obtained afterwards, and Catalyst Adsorption rate is 86.21%.
Comparative example 1
Method same as Example 2 recycles catalyst, the difference is that parsing agent is water-soluble for the Peracetic acid of concentration 5%
Liquid obtains catalyst 21.89g, Catalyst Adsorption rate 67.15% after vacuum drying.
Content of the present invention is not limited in embodiment content of the present invention.
Specific case used herein is expounded structure of the invention and embodiment, the explanation of above embodiments
It is merely used to help understand the core idea of the present invention.It should be pointed out that for those skilled in the art,
Without departing from the principles of the invention, can be with several improvements and modifications are made to the present invention, these improvement and modification are also fallen
Enter in the protection scope of the claims in the present invention.
Claims (10)
1. a kind of method for recycling heteropolyacid catalyst from chloro propylene epoxidation oil reservoir, which is characterized in that the described method includes:
(1) adsorbent is filled into fixed bed；
(2) chloro propylene epoxidation oil reservoir is made to flow through the fixed bed containing the adsorbent, in the chloro propylene epoxidation oil reservoir
Heteropolyacid catalyst be adsorbed；
(3) it after having handled the chloro propylene epoxidation oil reservoir, will be washed in the fixed bed with water, washing discharging carries out oil
Water stratification, oil reservoir therein are incorporated to untreated chloro propylene epoxidation oil reservoir；
(4) fixed bed is flowed through with peroxide solutions, the heteropolyacid catalyst can be oxidized at this time, from the adsorbent
In parse, after the fixed bed after parsing is washed with the water layer in step (3), the adsorbent is recyclable to be made
With；
(5) it by the solution vacuum distillation of the heteropolyacid catalyst after parsing, recycles more than kettle.
2. a kind of method for recycling heteropolyacid catalyst from chloro propylene epoxidation oil reservoir as described in claim 1, feature
It is, the adsorbent is one of active carbon, molecular sieve, zeolite, activated silica gel, activated alumina or a variety of.
3. a kind of method for recycling heteropolyacid catalyst from chloro propylene epoxidation oil reservoir as described in claim 1, feature
It is, the heteropolyacid catalyst is phosphorus tungsten/molybdenum/vanadic acid heteropolyacid catalyst.
4. a kind of method for recycling heteropolyacid catalyst from chloro propylene epoxidation oil reservoir as described in claim 1, feature
It is, in step (2), adsorption temp is 10 DEG C~60 DEG C, preferably 20 DEG C~30 DEG C.
5. a kind of method for recycling heteropolyacid catalyst from chloro propylene epoxidation oil reservoir as described in claim 1, feature
It is, in step (2), the flow velocity of the chloro propylene epoxidation oil reservoir is 0.1BV/h~5BV/h, preferably 0.5BV/h~2BV/
H, wherein BV is bed volume, and BV/h is the bed volume multiple for flowing through the fixed bed per hour.
6. a kind of method for recycling heteropolyacid catalyst from chloro propylene epoxidation oil reservoir as described in claim 1, feature
It is, in step (3), after the chloro propylene epoxidation oil reservoir flows through the fixed bed, the adsorbance of the adsorbent is institute
State the 10%~50% of adsorbent weight.
7. a kind of method for recycling heteropolyacid catalyst from chloro propylene epoxidation oil reservoir as described in claim 1, feature
It is, in step (3), the flow velocity of the water is 0.1BV/h~2BV/h, preferably 0.1BV/h~0.9BV/h, the use of the water
Amount is the 50%~200%, preferably 50%~100% of the adsorbent weight, and wash temperature is 10 DEG C~50 DEG C, preferably 20 DEG C
~30 DEG C.
8. a kind of method for recycling heteropolyacid catalyst from chloro propylene epoxidation oil reservoir as described in claim 1, feature
Be, the peroxide solutions be concentration be 5%-20% aqueous hydrogen peroxide solution, concentration be 5%-20% peroxide uncle
Sodium carbonate perhydrate aqueous solution that the ethanol solution of butanol, concentration are 5%-20%, concentration are 0.001%-0.01%'s
Ozone water solution.
9. a kind of method for recycling heteropolyacid catalyst from chloro propylene epoxidation oil reservoir as described in claim 1, feature
It is, in step (4), the flow velocitys of the peroxide solutions is 0.1BV/h~3BV/h, preferably 0.2BV/h~1.2BV/h,
The dosage of the peroxide solutions is the 50%~300%, preferably 100%~200% of the adsorbent weight, resolution temperature
It is 10 DEG C~60 DEG C, preferably 10 DEG C~50 DEG C, most preferably 20 DEG C~30 DEG C.
10. a kind of method for recycling heteropolyacid catalyst from chloro propylene epoxidation oil reservoir as described in claim 1, feature
It is, in the step (5), vapo(u)rizing temperature is 20 DEG C~80 DEG C, preferably 30 DEG C~60 DEG C, most preferably 40 DEG C~50 DEG C, is distilled
Pressure is -0.1MPa~0MPa, preferably -0.1MPa~-0.05MPa.
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| CN102834176A (en) * | 2010-03-29 | 2012-12-19 | 日本化药株式会社 | Method for manufacturing catalyst from recovered catalyst |
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