CN104788465B - Method for continuous preparation of isosorbide from sorbitol - Google Patents
Method for continuous preparation of isosorbide from sorbitol Download PDFInfo
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- CN104788465B CN104788465B CN201510068551.6A CN201510068551A CN104788465B CN 104788465 B CN104788465 B CN 104788465B CN 201510068551 A CN201510068551 A CN 201510068551A CN 104788465 B CN104788465 B CN 104788465B
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- C07—ORGANIC CHEMISTRY
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- C07D493/00—Heterocyclic compounds containing oxygen atoms as the only ring hetero atoms in the condensed system
- C07D493/02—Heterocyclic compounds containing oxygen atoms as the only ring hetero atoms in the condensed system in which the condensed system contains two hetero rings
- C07D493/04—Ortho-condensed systems
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Abstract
The invention discloses a method for continuous preparation of isosorbide from sorbitol, preparation devices used in the method include a raw material premixing device (1), a first stage dehydration reactor (2), an intermediate dehydration device (3), a secondary dehydration reactor (4), a neutralization acid removal reactor (5), a rectifying column or a stripping tower(6), an isosorbide condenser (7), a salt and impurity removal device (8), equipment connection pipelines, control instruments and various accessories; the preparation process is as follows: the sorbitol and a dehydration catalyst enter in proportion into the raw material premixing device (1), then enter the first stage dehydration reactor (2), pass through the intermediate dehydration device (3), then enter the secondary dehydration reactor (4) for further completion of the dehydration reaction; the method can be used for continuous preparation of isosorbide from the sorbitol, product quality is good, by-product is less, raw material utilization rate is high, preparation process is stable, and elasticity of operation is large.
Description
Technical field
The present invention relates to a kind of preparation method of isosorbide, is more particularly to prepared as raw material serialization with Sorbitol and is made
The method of standby isosorbide.
Background technology
Isosorbide is widely used in the fields such as medicine, food, cosmetics, plastics and polymer.Such as medically, it is different
Sorbitol is a kind of oral dehydration and diuresis medicine of effective permeability；Industrially, isosorbide is to prepare Span and Tween class tables
The important intermediate of face activating agent, because of its special chirality, can be applied to the synthesis of liquid crystal material as intermediate, extensively should
For fields such as electronics national defence；In Material Field, isosorbide can be used for the polymer such as polyethers, polyester, polyurethane, Merlon
It is modified, be remarkably improved the optical property of polyurethane, thermal property and mechanical property；The raw material Sorbitol of isosorbide is certainly
So it is widely present in boundary, it easily can be prepared by the renewable material of the wide material sources such as starch, sucrose and glucose.
It is due to abundant raw material source, low price and renewable, therefore isosorbide is described as following important bio-based medicine, chemical industry
Raw material, with the extensive market demand.
Isosorbide is mainly prepared by two step evaporation of Sorbitol, i.e., by Sorbitol mono- steps of Jing in the presence of a dehydration catalyst
Anhydrous sorbitol is dehydrated to obtain, further dehydration obtains isosorbide.
Research of the China in terms of the preparation of isosorbide at present is still in starting stage, its preparation technology and preparation dress
The standby simple amplification for being laboratory preparation process.Different mountain is obtained using autoclave intermittent reaction, simple distillation and crystallization operation more
Pears alcohol crude product, then crude product isosorbide is carried out being refining to obtain product isosorbide.Interval produces the main of isosorbide
Problem is that raw material availability is low, and preparation process is unstable, and product quality is difficult to ensure that product purification ＆ isolation is difficult.
Exploitation prepares the new preparation facilitiess and preparation method of isosorbide with Sorbitol as raw material, prepares isosorbide
Realize prepared by serialization, the preparation level to improving China's isosorbide meets the market demand of the future market to isosorbide
It is significant.
The content of the invention
It is an object of the invention to provide one kind is with Sorbitol, and as raw material, serialization dehydration is anti-in the presence of a dehydration catalyst
The method that isosorbide should be prepared, including serialization prepares the preparation facilitiess and preparation process of isosorbide.The method prepares energy
Power is big, and raw material availability is high, and energy expenditure is low, and preparation process is stable and easy to control, and operating flexibility is big.
The purpose of the present invention is achieved through the following technical solutions：
A kind of continuous preparation method by Pyrusussuriensiss dehydration of alcohols isosorbide, including following preparation facilitiess and prepared
Journey：
A. preparation facilitiess include：Raw material premix device, one-level dehydration reactor, middle dehydration device, two grades of dehydrations
Device, neutralization deacidifying device, essence（Carry）Evaporate tower, isosorbide condenser, desalination and impurity device, equipment room connecting pipeline, control
Instrument and adnexa etc.；
B. preparation process includes：
A. Sorbitol and dehydration catalyst continuously enter raw material premix device in proportion；
B. the mixed material after premixing enters one-level dehydration reactor；
C. the material for going out one-level dehydration reactor enters two grades of dehydration reactors after dehydration device dehydration in the middle of；
D. there is unconverted raw material in the material for going out two grades of dehydration reactors（Sorbitol and anhydrous sorbitol）When, a part is returned
Return raw material premix device or one-level dehydration reactor participates in dehydration again, another partial material is entered to neutralize deacidification reactor Jing and added
It is in alkali and rear into essence（Carry）Evaporate tower；Go out the material of two grades of dehydration reactors without unconverted raw material（Sorbitol and anhydrous sorbitol）
When fully enter neutralization deacidification reactor Jing in adding alkali and after enter essence（Carry）Evaporate tower；
E. it is smart（Carry）Evaporate that column overhead distillates water and isosorbide mixed vapour Jing isosorbide condensers condense to obtain different Pyrusussuriensiss
Alcohol liquid phase, part backflow, another part is isosorbide product；
F. it is smart（Carry）Evaporating tower bottoms has unconverted raw material（Sorbitol and anhydrous sorbitol）When enter desalination and impurity device,
After removing salt and impurity, return system participates in dehydration again；Essence（Carry）Tower bottoms is evaporated without unconverted raw material（Sorbitol and mistake
Water Sorbitol）When by tower reactor discharge system.
A kind of described continuous preparation method by Pyrusussuriensiss dehydration of alcohols isosorbide, raw material premix device, one-level take off
Water reactor, two grades of dehydration reactors, neutralization deacidification reactors are material is had with or without interior setting of blank pipe or pipe of chuck
The dynamic and static turbulent element of perturbation action or chemical filler.
A kind of described continuous preparation method by Pyrusussuriensiss dehydration of alcohols isosorbide, middle dehydration device are located at one-level
After dehydration reactor or after being located at two grades of dehydration reactors.
A kind of described continuous preparation method by Pyrusussuriensiss dehydration of alcohols isosorbide, middle dehydration device are located at two grades
When after dehydration reactor, one-level dehydration reactor and two grades of dehydration reactors are used in series, into the circulation of raw material premix device
Material can be drawn by drawing after two grades of dehydration reactors or by middle dehydration device.
A kind of described continuous preparation method by Pyrusussuriensiss dehydration of alcohols isosorbide, can arrange multiple stage dehydration
Device, configures the middle dehydration device of configuration one after middle dehydration device or several dehydration reactors after every dehydration reactor.
A kind of described continuous preparation method by Pyrusussuriensiss dehydration of alcohols isosorbide, two grades of dehydration reactors and neutralization
Between deacidification reactor and neutralization deacidification reactor with essence（Carry）Evaporate.
A kind of described continuous preparation method by Pyrusussuriensiss dehydration of alcohols isosorbide, raw material premix device can use autoclave
Agitator, jet mixer or other mixing arrangements replace, and one-level dehydration reactor, two grades of dehydration reactors, neutralization deacidifications are anti-
Answer device be replaced with tank reactor, fixed bed reactors or other types of reactor.
A kind of described continuous preparation method by Pyrusussuriensiss dehydration of alcohols isosorbide, the invention are applied to vacuum, often
Operate under pressure, pressurized conditions.
A kind of described continuous preparation method by Pyrusussuriensiss dehydration of alcohols isosorbide, as needed can be to by essence（Carry）
Evaporate the isosorbide that column overhead obtains further to be refined.
Advantages of the present invention with effect is：
1. make isosorbide preparation process realize serialization；
2., using the tubular dehydration reactor that turbulent element is set in peripheral hardware chuck, raw material is contacted fully with catalyst mixing,
Heat and mass transport effect is good, and reaction rate is fast；
3. it is dehydrated using between reactor region, is conducive to the carrying out of dehydration；
4. using essence（Carry）Evaporate operation and obtain isosorbide, overcome traditional simple distillation and operate in a certain boiling point range
Steaming thing as product, the not high shortcoming of isosorbide product purity.
Description of the drawings
Fig. 1 is dehydration device in the middle of arranging between one-level dehydration reactor and two grades of dehydration reactors, goes out two grades of dehydrations anti-
Answer the material parts of device to be recycled back into raw material premix device, have kettle liquid return system Jing after desalination and the desalination of impurity device and impurity
Again the isosorbide serialization preparation facilitiess for reacting are participated in；
Fig. 2 is after middle dehydration device is located at two grades of dehydration reactors, one-level dehydration reactor and two grades of dehydration reactors
Series connection, the material parts for going out middle dehydration device return raw material premix device, have the desalination of kettle liquid Jing and the desalination of impurity device and take off
The isosorbide serialization preparation facilitiess of return system after impurity.
Specific embodiment
Embodiment 1
The isosorbide serialization preparation facilitiess that embodiment 1 is given include raw material premix device 1, one-level dehydration reactor 2,
3, two grades of dehydration reactors 4 of middle dehydration device, neutralization deacidification reactor 5, essence（Carry）Evaporate tower 6, isosorbide condenser 7, take off
Salt and impurity device 8, equipment room connecting pipeline, control instrument and adnexa etc..Raw material premix device 1, one-level dehydration used is anti-
2, two grades of dehydration reactors 4 of device, neutralization deacidification reactor 5 are answered to be the tube type apparatus that chemical filler is set in peripheral hardware chuck；It is middle de-
Water installations 3 are arranged between one-level dehydration reactor 2 and two grades of dehydration reactors 4.Raw material enters raw material premix device 1 in proportion
Enter after entering one-level dehydration reactor 2 afterwards after middle dehydration device 3 is dehydrated and enter two grades of dehydration reactors 4；Go out two grades of dehydrations
A material part for reactor 4 is recycled back into raw material premix device 1 and participates in reaction again, goes out the another portion of two grades of dehydration reactors 4
Point material enter neutralization deacidification reactor 5 Jing in alkali and after enter essence（Carry）Evaporate tower 6；Water and isosorbide that rectifying tower top is distillated
Mixed vapour Jing isosorbide condenses to obtain isosorbide liquid phase, and part backflow is a part of as isosorbide product.Essence（Carry）
Evaporating 6 tower bottoms of tower has unconverted raw material（Sorbitol and dehydration isosorbide）, tower bottoms enters desalination and impurity device 8 is removed
Raw material premix device 1 is returned after salt and impurity and participates in reaction again.Embodiment 1 is as shown in Figure 1.
Embodiment 2
Embodiment 2 is substantially the same manner as Example 1, and difference is that middle dehydration device 3 is arranged on two grades of dehydrations
After device 4, one-level dehydration reactor 2 is used in series with two grades of dehydration reactors 4.Embodiment 2 is as shown in Figure 2.
Embodiment 3
Embodiment 3 is substantially the same manner as Example 1, and difference is that the material for two grades of dehydration reactors 4 is fully entered
Neutralization deacidification reactor 5, without unconverted raw material（Sorbitol and anhydrous sorbitol）It is recycled back into system and participates in dehydration again
Operation.
Embodiment 4
Embodiment 4 is substantially the same manner as Example 1, and difference is raw material premix device 1, one-level dehydration reactor 2, two
Level dehydration reactor 4, neutralization deacidification reactor 5 are commercially available tubular static mixer.
Embodiment 5
Embodiment 5 is substantially the same manner as Example 1, and difference is raw material premix device 1, one-level dehydration reactor 2, two
Level dehydration reactor 4, neutralization deacidification reactor 5 are stirring autoclave equipment.
Claims (9)
1. a kind of continuous preparation method by Pyrusussuriensiss dehydration of alcohols isosorbide, it is characterised in that described method includes following
Preparation facilitiess and preparation process：
A. described preparation facilitiess include：Raw material premix device（1）, one-level dehydration reactor（2）, middle dehydration device（3）, two
Level dehydration reactor（4）, neutralization deacidifying device（5）, rectifying column or stripping tower（6）, isosorbide condenser（7）, desalination and miscellaneous
Matter device（8）, equipment room connecting pipeline, control instrument and adnexa；
B. described preparation process includes：
A Sorbitol and dehydration catalyst continuously enter raw material premix device in proportion；
B. the mixed material after premixing enters one-level dehydration reactor（2）；
C. go out dehydration device in the middle of the material Jing of one-level dehydration reactor（3）Two grades of dehydration reactors are entered after dehydration（4）；
D. two grades of dehydration reactors are gone out（4）Material in when having unconverted raw material Sorbitol and anhydrous sorbitol, a part is returned
Raw material premix device（1）Or one-level dehydration reactor（2）Dehydration is participated in again, and another partial material enters to neutralize deacidification reactor
（5）Jing in adding alkali into rectifying column or stripping tower with after（6）；Go out two grades of dehydration reactors（4）Material without unconverted raw material mountain
Neutralization deacidification reactor is fully entered when pears alcohol and anhydrous sorbitol（5）Jing in adding alkali into rectifying column or stripping tower with after（6）；
E. rectifying column or stripping tower（6）Tower top distillates water and isosorbide mixed vapour Jing isosorbide condensers（7）Condense
Isosorbide liquid phase, part backflow, another part is isosorbide product；
F. rectifying column or stripping tower（6）Kettle liquid enters desalination and impurity device when having unconverted raw material Sorbitol and anhydrous sorbitol
（8）, after removing salt and impurity, return system participates in dehydration again；Rectifying column or stripping tower（6）Kettle liquid is without unconverted raw material
By tower reactor discharge system when Sorbitol and anhydrous sorbitol.
2. a kind of continuous preparation method by Pyrusussuriensiss dehydration of alcohols isosorbide according to claim 1, its feature exist
In described raw material premix device（1）, one-level dehydration reactor（2）, two grades of dehydration reactors（4）, neutralization deacidification reactor（5）
It is that the dynamic and static turbulent element or chemical filler for having perturbation action to material is set in the blank pipe or pipe with or without chuck.
3. a kind of continuous preparation method by Pyrusussuriensiss dehydration of alcohols isosorbide according to claim 1, its feature exist
In described middle dehydration device（3）It is located at one-level dehydration reactor（2）Afterwards or it is located at two grades of dehydration reactors（4）Afterwards.
4. a kind of serialization preparation side by Pyrusussuriensiss dehydration of alcohols isosorbide according to claim 1 and claim 3
Method, it is characterised in that described middle dehydration device（3）It is located at two grades of dehydration reactors（4）When afterwards, one-level dehydration reactor（2）
With two grades of dehydration reactors（4）It is used in series, into raw material premix device（1）Recycle stock can be by two grades of dehydration reactors
（4）Draw afterwards or by middle dehydration device（3）Draw.
5. a kind of continuous preparation method by Pyrusussuriensiss dehydration of alcohols isosorbide according to claim 1, its feature exist
Configure after dehydration device or several dehydration reactors in the middle of multiple stage dehydration reactor can be set, configuring after every dehydration reactor
Dehydration device in the middle of one.
6. a kind of continuous preparation method by Pyrusussuriensiss dehydration of alcohols isosorbide according to claim 1, its feature exist
In two grades of dehydration reactors（4）With neutralization deacidification reactor（5）Between and neutralization deacidification reactor（5）With rectifying column or stripping tower
（6）Between material pans can be set.
7. a kind of continuous preparation method by Pyrusussuriensiss dehydration of alcohols isosorbide according to claim 1, its feature exist
In raw material premix device（1）Available autoclave agitator, jet mixer or other mixing arrangements replace, one-level dehydration reactor
（2）, two grades of dehydration reactors（4）, neutralization deacidification reactor（5）Available tank reactor, fixed bed reactors or other types
Reactor replace.
8. a kind of continuous preparation method by Pyrusussuriensiss dehydration of alcohols isosorbide according to claim 1, its feature exist
It is applied under vacuum, normal pressure, pressurized conditions in the invention and operates.
9. a kind of continuous preparation method by Pyrusussuriensiss dehydration of alcohols isosorbide according to claim 1, its feature exist
In as needed can be to rectifying column or stripping tower（6）The isosorbide that tower top is obtained further is refined.
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| CN107540683B (en) * | 2016-06-27 | 2019-11-12 | 中国科学院大连化学物理研究所 | A kind of method of knapsack reaction and rectification device production anhydrosugar alcohol |
| CN106632371A (en) * | 2016-08-26 | 2017-05-10 | 山东绿健生物技术有限公司 | Method using dehydrated sorbitol liquid to produce high-purity isosorbide solution |
| CN107955012B (en) * | 2017-12-05 | 2020-06-09 | 中国科学院过程工程研究所 | Product preparation and separation system for byproduct with boiling point lower than that of product and raw material, and treatment method and application thereof |
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| EP1294727A2 (en) * | 2000-05-26 | 2003-03-26 | E.I. Dupont De Nemours And Company | Continuous process for the manufacture of anhydro sugar alcohols |
| FR2994183B1 (en) * | 2012-08-06 | 2015-07-31 | Roquette Freres | PROCESS FOR PREPARING DIALKYLOXYDIANHYDROHEXITOLS BY ETHERIFYING DIANHYDROHEXITOLS WITH LIGHT ALCOHOL IN THE PRESENCE OF AN ACIDIC CATALYST |
| CN103980286B (en) * | 2014-06-09 | 2016-12-07 | 长春大成实业集团有限公司 | The method of continuous prodution isosorbide and the device used thereof |
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