CN107652263A - Catalytic distillation device prepares the industrialization continuation method of solketal - Google Patents
Catalytic distillation device prepares the industrialization continuation method of solketal Download PDFInfo
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- CN107652263A CN107652263A CN201710948403.2A CN201710948403A CN107652263A CN 107652263 A CN107652263 A CN 107652263A CN 201710948403 A CN201710948403 A CN 201710948403A CN 107652263 A CN107652263 A CN 107652263A
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- catalytic
- catalyst
- solketal
- distillation device
- catalytic distillation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D317/00—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms
- C07D317/08—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms having the hetero atoms in positions 1 and 3
- C07D317/10—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms having the hetero atoms in positions 1 and 3 not condensed with other rings
- C07D317/14—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms having the hetero atoms in positions 1 and 3 not condensed with other rings with substituted hydrocarbon radicals attached to ring carbon atoms
- C07D317/18—Radicals substituted by singly bound oxygen or sulfur atoms
- C07D317/20—Free hydroxyl or mercaptan
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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
- Y02P20/10—Process efficiency
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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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- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses the industrialization continuation method that a kind of catalytic distillation device prepares solketal, specific method is：Using acetone and glycerine as raw material, solketal is prepared using catalytic distillation device serialization under catalyst action；Catalytic bed in catalytic distillation device is shell and tube or column plate type, the height of catalytic bed is 0.5 20 times of its width, material is reacted by Catalytic Layer, the reaction unit is directly connected to the separation that rectifier unit carries out raw material and product, raw material returns to again completes continuous operation in catalytic tower, product is directly connected to product storage tank by rectifying；The present invention is with load-type solid acid, and heteropoly acid or acid-exchange resin are catalyst, and there is the present invention catalyst easily to reclaim, long lifespan is reused, conversion per pass is high, it is not necessary to adds water entrainer and drier, high income, the advantages that not producing waste water in production substantially.
Description
Technical field
The present invention relates to the synthesis preparation method technical field of fine chemical product, specifically a kind of catalysis is steamed
Distillation unit prepares the industrialization continuation method of solketal.
Background technology
Solketal, also known as solketal (the entitled solketal of English), isopropylidene glycerine, 2,2- diformazans
Base-DOX -4- methanol, 2,2- dimethyl -4- methylol -1,3- dioxolanes, it is a kind of important organic molten
Agent, plasticizer and important organic synthesis intermediate.Brazilian researcher replaces first with solketal first within 2010
Additive of the base tertbutyl ether (MTBE) as Fuel Petroleum, mutually reconciles with regular gasoline, and the octane number of gasoline improves 2.5 lists
The generation of colloidal substance is reduced in position simultaneously, while the distillation curve of gasoline will not be made to produce significant change, is added for the height of glycerine
Value processing provides a new approach.The synthesis of solketal is broadly divided into two kinds of direct method and indirect method.In acid bar
The condensation that acetone and glycerine directly occur under part is referred to as direct method, under certain conditions, a kind of intermediate and methanol or acetone
Reaction is referred to as indirect method, and generally use is direct method, and its reaction equation is as follows:
It is strict to equipment requirement with strong acid as catalyst, it is unfavorable for industrial production.Many researchs are directed to solid acid at present
(Chemical Industry in Guangzhou 2017,45 (3), 39-41), storng-acid cation exchange resin (colleges and universities' Chemical Engineering journal, 2015,29 (4),
948-954),:Appl.Catal.A:Gen.,2001,221,45-62:Org.Process Res.Dev.,2001,5,630-
635), heteropoly acid (Journal of Molecular Catalysis, 2003,17 (1), 61-64) etc. catalyzes and synthesizes the third intoxicated contracting glycerine, can to a certain extent gram
Take insufficient existing for traditional liquid acid catalyst catalysis process.But the presence reaction time of these methods is longer, post processing is numerous
It is trivial, because thering is water to generate in course of reaction to add water entrainer or deicer, add the shortcomings of industrializing cost.
The content of the invention
In view of the defects and deficiencies of the prior art, the present invention intends to provide a kind of catalytic distillation device prepares acetone
The industrialization continuation method of contracting glycerine, with load-type solid acid, heteropoly acid or acid-exchange resin are catalyst, this method
Easily reclaimed with catalyst, reuse long lifespan, conversion per pass is high, it is not necessary to adds water entrainer and drier, yield
Height, the advantages that not producing waste water in production substantially.
To achieve the above object, the technical solution adopted by the present invention is：
The industrialization continuation method that catalytic distillation device prepares solketal is：Using acetone and glycerine as raw material, urging
Agent effect is lower to prepare solketal using catalytic distillation device serialization；Catalytic bed in catalytic distillation device is shell and tube
Or column plate type, the height of catalytic bed are 0.5-20 times of its width, material is reacted by Catalytic Layer, and the reaction unit is directly connected to
Rectifier unit carries out the separation of raw material and product, and raw material returns to again completes continuous operation in catalytic tower, product passes through rectifying
It is directly connected to product storage tank.
Further, the catalyst is selected from heteropolyacid catalyst, solid acid catalyst or ion-exchange resin catalyst, urges
The porosity of agent is 40%-50%.
Further, the proportioning of the acetone and glycerine is 0.6:1-10:1, reaction temperature is：35-120 DEG C, reaction pressure
For 0-1.5MPa, quality rate controlling is：0.5-3.0.
After said structure, beneficial effects of the present invention are：The present invention with load-type solid acid, heteropoly acid or it is acid from
Sub-exchange resin is catalyst, and there is the present invention catalyst easily to reclaim, and reuses long lifespan, conversion per pass is high, is not required to
Add water entrainer and drier, high income, the advantages that not producing waste water in production substantially.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, it is right below in conjunction with embodiment
The present invention is further elaborated.It should be appreciated that embodiment described herein is only to explain the present invention, and
It is not used in the restriction present invention.
Embodiment 1
Reactor is fixed-bed tube reactor, internal diameter 30mm, pipe range 600mm, loading catalyst 350g, and catalyst is
Highly acidic resin catalyst, temperature is entered as 54 DEG C of catalyst using 200g/h speed after 200g glycerine and 500g acetone heating
Bed, control pressure 0.5MPa, conversion zone directly carry out rectifying, it is anti-that fixed bed progress are returned after acetone rectifying and dewatering after terminating
Should, unreacted glycerine is returned by tower reactor to be continued to react.The conversion per pass of glycerine is 40%, synthesizes the selection of solketal
Property is 92%.
Embodiment 2
Reactor is fixed-bed tube reactor, internal diameter 30mm, pipe range 600mm, loading catalyst 350g, and catalyst is
Highly acidic resin catalyst, temperature is entered as 54 DEG C of catalyst using 100g/h speed after 200g glycerine and 500g acetone heating
Bed, control pressure 0.2MPa, conversion zone directly carry out rectifying, it is anti-that fixed bed progress are returned after acetone rectifying and dewatering after terminating
Should, unreacted glycerine is returned by tower reactor to be continued to react.The conversion per pass of glycerine is 52%, synthesizes the selection of solketal
Property is 94%.
Embodiment 3
Reactor is fixed-bed tube reactor, internal diameter 30mm, pipe range 600mm, loading catalyst 350g, and catalyst is
Highly acidic resin catalyst, temperature is entered as 54 DEG C of catalyst using 100g/h speed after 200g glycerine and 800g acetone heating
Bed, control pressure 0.2MPa, conversion zone directly carry out rectifying, it is anti-that fixed bed progress are returned after acetone rectifying and dewatering after terminating
Should, unreacted glycerine is returned by tower reactor to be continued to react.The conversion per pass of glycerine is 65%, synthesizes the selection of solketal
Property is 95%.
Embodiment 4
Reactor is fixed-bed tube reactor, internal diameter 30mm, pipe range 600mm, loading catalyst 200g, and catalyst is
Heteropoly acid spheric catalyst, temperature is entered as 54 DEG C of catalyst using 100g/h speed after 200g glycerine and 800g acetone heating
Bed, control pressure 0.2MPa, conversion zone directly carry out rectifying, it is anti-that fixed bed progress are returned after acetone rectifying and dewatering after terminating
Should, unreacted glycerine is returned by tower reactor to be continued to react.The conversion per pass of glycerine is 59%, synthesizes the selection of solketal
Property is 90%.
Embodiment 5
Reactor is fixed-bed tube reactor, internal diameter 30mm, pipe range 600mm, loading catalyst 200g, and catalyst is
Solid acid spheric catalyst, temperature is entered as 54 DEG C of catalyst using 200g/h speed after 200g glycerine and 800g acetone heating
Bed, control pressure 0.5MPa, conversion zone directly carry out rectifying, it is anti-that fixed bed progress are returned after acetone rectifying and dewatering after terminating
Should, unreacted glycerine is returned by tower reactor to be continued to react.The conversion per pass of glycerine is 60%, synthesizes the selection of solketal
Property is 88%.
It is obvious to a person skilled in the art that the invention is not restricted to the details of above-mentioned one exemplary embodiment, Er Qie
In the case of without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, embodiment all should be regarded as exemplary, and be nonrestrictive, the scope of the present invention is by appended power
Profit requires rather than described above limits, it is intended that all in the implication and scope of the equivalency of claim by falling
Change is included in the present invention.
Moreover, it will be appreciated that although the present specification is described in terms of embodiments, not each embodiment is only wrapped
Containing an independent technical scheme, this narrating mode of specification is only that those skilled in the art should for clarity
Using specification as an entirety, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art
It is appreciated that other embodiment.
Claims (3)
1. catalytic distillation device prepares the industrialization continuation method of solketal, it is characterised in that：Specific method is：With acetone
It is raw material with glycerine, solketal is prepared using catalytic distillation device serialization under catalyst action；Catalytic distillation device
In catalytic bed be shell and tube or column plate type, the height of catalytic bed is 0.5-20 times of its width, and material is reacted by Catalytic Layer,
The reaction unit is directly connected to the separation that rectifier unit carries out raw material and product, and raw material returns to and serialization is completed in catalytic tower again
Operation, product are directly connected to product storage tank by rectifying.
2. catalytic distillation device according to claim 1 prepares the industrialization continuation method of solketal, its feature exists
In：The catalyst is selected from heteropolyacid catalyst, solid acid catalyst or ion-exchange resin catalyst, the porosity of catalyst
For 40%-50%.
3. catalytic distillation device according to claim 1 prepares the industrialization continuation method of solketal, its feature exists
In：The proportioning of the acetone and glycerine is 0.6:1-10:1, reaction temperature is：35-120 DEG C, reaction pressure 0-1.5MPa, matter
Measuring rate controlling is：0.5-3.0.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201710948403.2A CN107652263A (en) | 2017-10-12 | 2017-10-12 | Catalytic distillation device prepares the industrialization continuation method of solketal |
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| CN201710948403.2A CN107652263A (en) | 2017-10-12 | 2017-10-12 | Catalytic distillation device prepares the industrialization continuation method of solketal |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109485629A (en) * | 2018-11-21 | 2019-03-19 | 浙江工业大学 | A kind of production technology of anhydrous propanone contracting glycerol |
| CN109535121A (en) * | 2019-01-17 | 2019-03-29 | 江苏天音化工有限公司 | A method of preparing 2- methyl -2- isobutyl group -4- methylol -1,3-dioxolane |
| CN112604687A (en) * | 2020-12-23 | 2021-04-06 | 重庆工商大学 | Application of boroaluminate catalyst in catalyzing ketal reaction of glycerol and acetone |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103619829A (en) * | 2011-06-24 | 2014-03-05 | 伊士曼化工公司 | Production of cyclic acetals or ketals using solid acid catalysts |
| RU2625318C2 (en) * | 2015-12-28 | 2017-07-13 | Федеральное государственное бюджетное учреждение науки Ордена Трудового Красного Знамени Институт нефтехимического синтеза им. А.В. Топчиева Российской академии наук (ИНХС РАН) | Method of obtaining solketal (versions) |
-
2017
- 2017-10-12 CN CN201710948403.2A patent/CN107652263A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103619829A (en) * | 2011-06-24 | 2014-03-05 | 伊士曼化工公司 | Production of cyclic acetals or ketals using solid acid catalysts |
| RU2625318C2 (en) * | 2015-12-28 | 2017-07-13 | Федеральное государственное бюджетное учреждение науки Ордена Трудового Красного Знамени Институт нефтехимического синтеза им. А.В. Топчиева Российской академии наук (ИНХС РАН) | Method of obtaining solketal (versions) |
Non-Patent Citations (1)
| Title |
|---|
| 樊春妮: "酸催化甘油-丙酮缩醛反应制丙酮缩甘油的催化剂及工艺研究", 《中国优秀硕士学位论文全文数据库工程科技I辑》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109485629A (en) * | 2018-11-21 | 2019-03-19 | 浙江工业大学 | A kind of production technology of anhydrous propanone contracting glycerol |
| CN109535121A (en) * | 2019-01-17 | 2019-03-29 | 江苏天音化工有限公司 | A method of preparing 2- methyl -2- isobutyl group -4- methylol -1,3-dioxolane |
| CN112604687A (en) * | 2020-12-23 | 2021-04-06 | 重庆工商大学 | Application of boroaluminate catalyst in catalyzing ketal reaction of glycerol and acetone |
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