CN108355372A - A kind of the distillation method of reseptance and device of maltol - Google Patents
A kind of the distillation method of reseptance and device of maltol Download PDFInfo
- Publication number
- CN108355372A CN108355372A CN201810038451.2A CN201810038451A CN108355372A CN 108355372 A CN108355372 A CN 108355372A CN 201810038451 A CN201810038451 A CN 201810038451A CN 108355372 A CN108355372 A CN 108355372A
- Authority
- CN
- China
- Prior art keywords
- kettle
- distillation
- horizontal
- reception
- steam
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D7/00—Sublimation
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D309/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only ring hetero atom, not condensed with other rings
- C07D309/34—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only ring hetero atom, not condensed with other rings having three or more double bonds between ring members or between ring members and non-ring members
- C07D309/36—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only ring hetero atom, not condensed with other rings having three or more double bonds between ring members or between ring members and non-ring members with oxygen atoms directly attached to ring carbon atoms
- C07D309/40—Oxygen atoms attached in positions 3 and 4, e.g. maltol
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
- Saccharide Compounds (AREA)
- Soy Sauces And Products Related Thereto (AREA)
Abstract
The present invention relates to a kind of distillation method of reseptances of maltol, include the following steps：A. the distillation steam from 160 220 DEG C of kettle of distillation enters horizontal reception kettle upper entrance, in horizontal reception kettle under the stirring of multistage rotating blender, so that cooling water comes into full contact with absorption in steam material and kettle, at the same horizontal reception kettle with cooling water control absorbing liquid temperature at 70 80 DEG C；B. enter the vertical reception kettle of two level from horizontal reception kettle upper outlet without absorbed steam material, the vertical kettle outside chuck that receives carries out conventional absorption using 12 DEG C -15 DEG C of brine to steam material in kettle.The advantage of the invention is that, using horizontal reception kettle, lengthen residence time of the distillation material in receiving kettle, improve the ability for receiving material, number of devices is reduced, the stability of vacuum degree is maintained, also achievees the purpose that reinforcing distillation receives sedimentation, production yield is improved, there is larger economic benefit.
Description
Technical field
The production process of maltol is divided into grignard workshop section, chlorination workshop section, distillation workshop section, crystallization workshop section, drying workshop section.Wherein
The workshop section's yield that distils is relatively low always, main reason is that distillation reception device is excessively traditional, what is used in production is vertical anti-
The three-level of autoclave is answered to receive mode, material quickly passes in and out, and heat exchange efficiency is poor, great limitation is caused to production, in offgas outlet
Still large-tonnage product takes out of；And reception link is excessive, vacuum degree is difficult to control, and rate of sublimation receives influence, and partial material is long
Time is heated and is decomposed into by-product, has seriously affected product quality and yield.
Invention content
The purpose of the present invention is exactly in order to which the efficiency existing for reception device that solves to distil in the prior art is low, poor product quality
The shortcomings that, a kind of distillation reception device of the maltol provided.
The technical solution adopted by the present invention is as follows：
1, the distillation method of reseptance of a kind of maltol, it is characterised in that include the following steps：
A. the distillation steam from 160-220 DEG C of kettle of distillation enters horizontal reception kettle upper entrance, multistage in horizontal reception kettle
Under the stirring of rotating blender so that steam material comes into full contact with absorption with cooling water in kettle, while horizontal reception kettle cools down
Water management absorbing liquid temperature is at 70-80 DEG C；
B. enter the vertical reception kettle of two level from horizontal reception kettle upper outlet without absorbed steam material, outside vertical reception kettle
The brine of -12 DEG C--15 DEG C of face chuck use carries out conventional absorption to steam material in kettle.
2, it is a kind of realize maltol distillation method of reseptance device, it is characterised in that by distillation kettle, horizontal reception kettle with
And vertical reception kettle passes through pipeline connection composition, it is characterised in that horizontal reception kettle includes：The round autoclave body of horizontal type level, it is round
Autoclave body center is equipped with horizontal agitating shaft and its connected motor, and agitating shaft is equipped with one group of spiral agitator, round autoclave body two
End is respectively equipped with material inlet and material outlet.
It is an advantage of the current invention that using horizontal reception kettle, distillation material is mainly lengthened in the stop in receiving kettle
Between, material can be allowed to exchange heat with liquid phase more abundant, substantially increase the ability for receiving material, reduce number of devices, maintain
The stability of vacuum degree.With new-type reception device, the vacuum cooled condition before not only ensureing is unaffected, also reaches reinforcement
Distillation receives the purpose of sedimentation, improves production yield, has larger economic benefit.
Description of the drawings
Fig. 1 is the system flow chart of the present invention；
Fig. 2 is the horizontal structure chart for receiving kettle in Fig. 1.
Specific implementation mode
One, shown in Fig. 1, Fig. 2, a kind of device of distillation method of reseptance that realizing maltol provided by the invention, by distilling
Kettle, horizontal reception kettle and vertical reception kettle are connected by pipeline and are formed, wherein horizontal reception kettle includes：The circle of horizontal type level
Autoclave body 1, round autoclave body center are equipped with horizontal agitating shaft 4 and its connected motor 5, and agitating shaft is equipped with one group of spiral agitator
3, round autoclave body both ends are respectively equipped with material inlet and material outlet, and round autoclave body is equipped with chuck 2, the upper and lower side point of chuck 2
Not She You refrigerant inlet and outlet, one side bottom of round autoclave body be equipped with baiting valve.Round autoclave body is connected on one holder 6 of setting.
Two, as shown in Figure 1 and Figure 2, the present invention provides a kind of distillation method of reseptance of maltol,
1, present invention is mainly applied to maltol distillation post condensations to receive the crude product maltol used in material, generated by reaction
Containing a large amount of asphaltic by-products, in order to by product initial gross separation, by the way of Decompression Sublimation；This system material comes from chlorination
After hydrolysis process, the dirty oil of two kettles hydrolysis generation is put into a distillation kettle and distils, and about 1 cube of dirty oil volume rises
Magnificent kettle is 1.5 cubes, and the horizontal kettle that receives is 2 cubes.
2, material is put into distillation kettle and opens stirring progress jacket oil heating, waits for that temperature in the kettle rises to 160 DEG C or so, opens vacuum
Pump, vacuum degree ensure to be not less than -0.8MPa, and horizontal 1 side of receptions kettle water distribution, which opens, to stir, and starts to distil, according to receiving kettle
Go out the amount of evaporating and regulates oil temperature（Oil temperature must not be higher than 280 DEG C）, as maltol distils out, kettle temperature gradually rises, and about distils 4 hours
Kettle temperature rises to 230 ~ 240 DEG C, observes remaining pitch state in kettle, judges that distillation terminal puts pitch.
3, the distillation steam from 160-220 DEG C of kettle of distillation enters horizontal reception kettle upper entrance, in horizontal reception kettle
Under the stirring of multistage rotating blender 4 so that steam material comes into full contact with absorption with cooling water in kettle, while horizontal reception kettle is used
Cooling water control absorbing liquid temperature is in 70-80 degree in chuck 2；There is no absorbed steam material from horizontal reception kettle upper outlet
Into the vertical reception kettle of two level, the vertical brine for receiving -12 DEG C--15 DEG C of chuck use outside kettle carries out steam material in kettle
Conventional absorption.
The present invention receives kettle by first now and transform horizontal reception device as, mainly improves：1）High-temperature material is receiving
Increased resident time in device, 2）Multi-stage stirring can preferably driving device cooling water exchange heat with high-temperature material, improve sedimentation
Effect, 3）Material is timely settled down, and no longer largely compensation vacuum, vacuum degree are obviously improved, vacuum pump acting effect table
It is now more preferable, 4）Original reception kettle has three-level, be respectively the kettle one of 2 sides, 1 side kettle 2；Improve now is 2 sidesIt is horizontal Receive kettleIt can meet production needs with the reception kettle of 1 side.4, the improvement of vacuum kettle makes sublimation temperature reduce, when distillation
Between shorten, reduce material pyrolytic, improve one-pot yield, while reducing higher boiling magazine and bringing into and receiving kettle, product matter
Amount is more preferable；It can distil and be not easy to wrap up in band material in thorough asphaltic by-products, one-pot by-product pitch amount is less slightly.
Claims (2)
1. a kind of distillation method of reseptance of maltol, it is characterised in that include the following steps：
A. the distillation steam from 160-220 DEG C of kettle of distillation enters horizontal reception kettle upper entrance, multistage in horizontal reception kettle
Under the stirring of rotating blender so that steam material comes into full contact with absorption with cooling water in kettle, while horizontal reception kettle cools down
Water management absorbing liquid temperature is at 70-80 DEG C；
B. enter the vertical reception kettle of two level from horizontal reception kettle upper outlet without absorbed steam material, outside vertical reception kettle
The brine of -12 DEG C--15 DEG C of face chuck use carries out conventional absorption to steam material in kettle.
2. a kind of device of distillation method of reseptance that realizing maltol, it is characterised in that by distillation kettle, horizontal reception kettle and stand
Formula receives kettle and passes through pipeline connection composition, it is characterised in that horizontal reception kettle includes：The round autoclave body of horizontal type level（1）, round
Autoclave body center is equipped with horizontal agitating shaft（4）And its connected motor（5）, agitating shaft is equipped with one group of spiral agitator（3）, circle
Shape autoclave body both ends are respectively equipped with material inlet and material outlet, and round autoclave body is equipped with chuck（2）, chuck（2）Upper and lower side point
It She You not refrigerant inlet and outlet.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810038451.2A CN108355372B (en) | 2018-01-13 | 2018-01-13 | Method and device for sublimating and receiving maltol |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810038451.2A CN108355372B (en) | 2018-01-13 | 2018-01-13 | Method and device for sublimating and receiving maltol |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN108355372A true CN108355372A (en) | 2018-08-03 |
| CN108355372B CN108355372B (en) | 2020-09-08 |
Family
ID=63006108
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810038451.2A Active CN108355372B (en) | 2018-01-13 | 2018-01-13 | Method and device for sublimating and receiving maltol |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108355372B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109503536A (en) * | 2018-12-10 | 2019-03-22 | 安徽金禾实业股份有限公司 | A kind of ethylmaltol method of purification and device |
| CN109535113A (en) * | 2018-12-10 | 2019-03-29 | 安徽金禾实业股份有限公司 | A kind of maltol lyophilization method and device |
| CN112742061A (en) * | 2020-12-11 | 2021-05-04 | 安徽金禾实业股份有限公司 | Cooling device and cooling method for maltol sublimation section |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2135394Y (en) * | 1992-09-15 | 1993-06-09 | 曹丽娜 | Water absorption chamber |
| CA2259481A1 (en) * | 1998-02-09 | 1999-08-09 | Kemestrie Inc. | Direct extraction and/or purification of high purity maltol and essential oils by sublimation process |
| CN101993428A (en) * | 2010-11-10 | 2011-03-30 | 广东省肇庆香料厂有限公司 | Method for purifying ethyl maltol |
| CN103113339A (en) * | 2012-11-11 | 2013-05-22 | 安徽金禾实业股份有限公司 | Maltol separation and purification method |
| CN106310700A (en) * | 2015-07-08 | 2017-01-11 | 陕西天汉生物科技有限公司 | Ethyl maltol crystallization sublimation process capable of reducing energy consumption |
-
2018
- 2018-01-13 CN CN201810038451.2A patent/CN108355372B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2135394Y (en) * | 1992-09-15 | 1993-06-09 | 曹丽娜 | Water absorption chamber |
| CA2259481A1 (en) * | 1998-02-09 | 1999-08-09 | Kemestrie Inc. | Direct extraction and/or purification of high purity maltol and essential oils by sublimation process |
| CN101993428A (en) * | 2010-11-10 | 2011-03-30 | 广东省肇庆香料厂有限公司 | Method for purifying ethyl maltol |
| CN103113339A (en) * | 2012-11-11 | 2013-05-22 | 安徽金禾实业股份有限公司 | Maltol separation and purification method |
| CN106310700A (en) * | 2015-07-08 | 2017-01-11 | 陕西天汉生物科技有限公司 | Ethyl maltol crystallization sublimation process capable of reducing energy consumption |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109503536A (en) * | 2018-12-10 | 2019-03-22 | 安徽金禾实业股份有限公司 | A kind of ethylmaltol method of purification and device |
| CN109535113A (en) * | 2018-12-10 | 2019-03-29 | 安徽金禾实业股份有限公司 | A kind of maltol lyophilization method and device |
| CN112742061A (en) * | 2020-12-11 | 2021-05-04 | 安徽金禾实业股份有限公司 | Cooling device and cooling method for maltol sublimation section |
| WO2022122029A1 (en) | 2020-12-11 | 2022-06-16 | 安徽金禾实业股份有限公司 | Cooling device and cooling method for maltol sublimation section |
Also Published As
| Publication number | Publication date |
|---|---|
| CN108355372B (en) | 2020-09-08 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101250113B (en) | Method for refining p-phenylene diamine | |
| CN108355372A (en) | A kind of the distillation method of reseptance and device of maltol | |
| CN105858627B (en) | The recovery method of benzene homologues nitrating wasting acid | |
| CN101913994B (en) | Method for producing nonyl phenol | |
| CN106699808A (en) | Acidolysis and solvent recycling process and device for producing glyphosate by using glycine method | |
| CN109608353B (en) | Continuous production process and device for m-aminoacetanilide | |
| CN106631704A (en) | Preparation method for styrenated phenol | |
| CN112047825A (en) | Production process of dichloro pinacolone | |
| CN108947870B (en) | Preparation method of bromosartanbiphenyl | |
| CN101928214A (en) | Method for synthesizing dexketoprofen trometamol | |
| CN101723842B (en) | Method for preparing ethylene diamine tetraacetic acid (EDTA) disodium salt | |
| CN105777540A (en) | Energy-saving efficient isopropenyl acetate synthesis method | |
| CN103102369B (en) | A kind of production method of diethyl ethylphosphate | |
| CN201978736U (en) | Chlorination reaction device in production of ethyl maltol | |
| CN109485564B (en) | Novel method for preparing bifenthrin | |
| CN112979591A (en) | Oxidation extraction process for recycling dichloromethane in preparation of furan ammonium salt | |
| CN103965094A (en) | N-methyl-4-amino-5-bromo-phthalimide synthesis method | |
| CN111269108B (en) | Continuous hydrolysis device and method for 2,4,6 trimethyl benzoic acid acylation liquid | |
| CN112608359A (en) | Process for the preparation of 17 alpha-hydroxyandrosta-4, 9-diene-3, 20-dione | |
| CN205307822U (en) | Production 2 - acrylic amide -2 - methyl -propanesulfonic acid uses novel evaporimeter | |
| CN104761517A (en) | Continuous refining method of versatate glycidyl | |
| CN219540280U (en) | Crude filtrate recovery washing device of allies oneself with bromine | |
| CN220558573U (en) | Multistage condensing equipment of divinylbenzene | |
| CN219824048U (en) | System for continuously recycling ethanol in carbapilin calcium mother liquor | |
| CN206045466U (en) | A kind of residual crystallisation by cooling system of dimethyl sulfoxide rectifying still |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |