CN105884611A - Circular reaction water phase organic acid esterifying device and organic acid esterifying method thereof - Google Patents
Circular reaction water phase organic acid esterifying device and organic acid esterifying method thereof Download PDFInfo
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- CN105884611A CN105884611A CN201610368028.XA CN201610368028A CN105884611A CN 105884611 A CN105884611 A CN 105884611A CN 201610368028 A CN201610368028 A CN 201610368028A CN 105884611 A CN105884611 A CN 105884611A
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- esterifier
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/08—Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C69/00—Esters of carboxylic acids; Esters of carbonic or haloformic acids
- C07C69/66—Esters of carboxylic acids having esterified carboxylic groups bound to acyclic carbon atoms and having any of the groups OH, O—metal, —CHO, keto, ether, acyloxy, groups, groups, or in the acid moiety
- C07C69/67—Esters of carboxylic acids having esterified carboxylic groups bound to acyclic carbon atoms and having any of the groups OH, O—metal, —CHO, keto, ether, acyloxy, groups, groups, or in the acid moiety of saturated acids
- C07C69/675—Esters of carboxylic acids having esterified carboxylic groups bound to acyclic carbon atoms and having any of the groups OH, O—metal, —CHO, keto, ether, acyloxy, groups, groups, or in the acid moiety of saturated acids of saturated hydroxy-carboxylic acids
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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
- Y02P20/582—Recycling of unreacted starting or intermediate materials
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Abstract
The invention discloses a circular reaction water phase organic acid esterifying device and an organic acid esterifying method thereof. The device comprises an esterifying reactor, an alcohol steam dewaterer and a rectifying tower. The top of the esterifying reactor is connected into the bottom of the alcohol steam dewater through a pipeline which is provided with a condensing unit. The alcohol steam dewaterer is connected into the bottom of the esterifying reactor through a return pipeline. The bottom of the alcohol stream dewaterer is connected with the rectifying tower through a pipeline. A device containing a dewatering agent is arranged on the bottom of the alcohol steam dewaterer. The circular reaction water phase organic acid esterifying device has the advantages of being simple in structure, high in efficiency, low in energy consumption and the like and can achieve direct water phase esterifying of organic acid. The invention further discloses the organic acid esterifying method of the device. The method is simple, the organic acid esterifying yield is high, and the method is suitable for industrial mass production.
Description
Technical field
The invention belongs to chemical field, be specifically related to the aqueous phase organic acid esters gasifying device of circular response, further relate to utilize this device to incite somebody to action
Organic acid esters turns to the method for organic acid esters.
Background technology
The compound that organic acid esters is organic acid to be formed under catalyst action with alcohol, be chemical industry and the staple product of pharmacy or
Middle product.But owing to organic acid is faintly acid, carbonyl activity is low, the reaction of organic acid and alcohol is the slowest, and is esterified anti-
Should be a reversible process, while organic carboxyl acid and alcohol effect generate ester and water, ester and water effect can obtain again alcohol and organic
Acid, the yield causing organic acid esters is low.As: when waiting the organic acid of amount of material and esterification participated in by alcohol, can only obtain reason
The ester of opinion yield 2/3rds.Further, in the large-scale production of bulk chemical, in order to reduce production cost organic acid raw material one
As do not use highly purified organic acid, generally use biofermentation product or industrial by-products as raw material, therefore in raw material except
Outside containing main component organic acid, possibly together with substantial amounts of water.And the existence of water can stop organic acid to enter to organic acid esters direction with alcohol
OK, the yield of organic acid esters is reduced further.
It would therefore be highly desirable to improve organic acid to be converted into the inefficient problem of organic acid esters with alcohol, straight especially for organic acid fermentation liquid
Connect the organic ester yield of esterification.
Summary of the invention
In view of this, an object of the present invention is to provide the aqueous phase organic acid esters gasifying device of circular response；The purpose of the present invention
Two be to provide the method utilizing this device that organic acid esters turns to organic acid esters.
For achieving the above object, the present invention provides following technical scheme:
1, the aqueous phase organic acid esters gasifying device of circular response, including esterifier, alcohol steam dehydrator and rectifying column, described ester
Change that reactor head is provided by condensing unit and be passed through the pipeline bottom alcohol steam dehydrator and be connected with alcohol steam dehydrator；
The reflux line that described alcohol steam dehydrator top is passed through bottom esterifier by setting is connected with esterifier；Described alcohol
It is connected with rectifying column by pipeline bottom steam dehydrator；
Described rectifying column top is provided with alcohol air vent, and rectifier bottoms is provided with organic acid esters outlet.
In the present invention, the dehydrating function of alcohol steam dehydrator is by adding dehydrant bottom alcohol steam dehydrator, such as molecular sieve, silicon
The water in steam removed by glue etc..
Preferably, described esterifier top is provided with organic acid head tank, raw polyol tank I and catalysagen batch can；Described
Alcohol steam dehydrator top is provided with raw polyol tank II.
Preferably, the pipeline at described condensing unit two ends is respectively provided with two-port valve I, described reflux line is provided with two-way
Valve II；Respectively by two-port valve control between described organic acid head tank, raw polyol tank I and catalysagen batch can and esterifier
System.
It is furthermore preferred that be provided with heater I bottom described esterifier；It is provided with heater bottom described alcohol steam dehydrator
Ⅱ。
It is furthermore preferred that described esterifier top is provided with the agitator I stretched into bottom esterifier；Described alcohol steam takes off
Hydrophone top is provided with the agitator II stretched into bottom alcohol steam dehydrator.
It is furthermore preferred that the pipeline being provided by two-port valve bottom described esterifier is connected with described rectifying column；Or esterification is anti-
With described essence after answering the pipeline being connected between the pipeline being provided by two-port valve bottom device with alcohol steam dehydrator and rectifying column to merge
Evaporate tower to connect.
It is provided with reactant liquor delivery pump it is furthermore preferred that be connected on pipeline with described rectifying column.
2, the method utilizing the aqueous phase organic acid esters gasifying device esterification organic acid of described circular response, by organic acid soln and alcohol and acid
In esterifier, carry out esterification, obtain the vapour mixture containing organic acid esters, water and alcohol, then gained steam is mixed
It is passed through after compound is condensed in the alcohol steam dehydrator of interpolation dehydrant and is dehydrated, simultaneously by the alcohol reflux in alcohol steam dehydrator
To esterifier, circular response to chemical reaction reaches balance, finally by alcohol steam dehydrator or/and in esterifier
Reactant liquor is passed through rectifying column and removes alcohol or/and acid obtains organic acid esters.
Heretofore described organic acid can be any one in malic acid, succinic acid, fumaric acid, adipic acid, preferably Herba Marsileae Quadrifoliae
Fruit acid；Malic acid esterification process is as follows: with alcohol and concentrated sulphuric acid, malic acid solution is carried out in esterifier esterification,
To vapour mixture containing malate, water and alcohol, then the alcohol adding dehydrant will be passed through after condensed for gained vapour mixture
Being dehydrated in steam dehydrator, simultaneously by the methanol eddy in alcohol steam dehydrator to esterifier, circular response is to changing
Learn reaction and reach balance, finally by alcohol steam dehydrator or/and the reactant liquor in esterifier is passed through rectifying column removal alcohol and/or sulfur
Acid obtains malate.
Add in 2～10:5～50:0.5～20 (g:ml:ml) ratio it is furthermore preferred that malic acid solution will be contained with methanol and concentrated sulphuric acid
Esterifier is esterification under the conditions of 80～120 DEG C, obtains the vapour mixture containing malate, water and methanol, then will
It is passed through after gained vapour mixture is condensed in the alcohol steam dehydrator of interpolation dehydrant and is dehydrated, simultaneously by alcohol steam dehydrator
In methanol be back in esterifier under the conditions of 50～90 DEG C, circular response 2～10 hours, finally by alcohol steam dehydrator
Or/and the reactant liquor in esterifier is passed through rectifying column removes alcohol or/and sulphuric acid obtains malate.
In the present invention, the concentration of malic acid solution preferably mass fraction is the aqueous solution of malic acid of 30-80%.
The beneficial effects of the present invention is: the invention discloses the aqueous phase organic acid esters gasifying device of circular response, this device has knot
Structure is simple, efficiency is high, low power consumption and other advantages, by arranging the pipe installing condensing unit in esterifier and alcohol steam dehydrator
Road and reflux line, make organic acid and alcohol carry out esterification in esterifier, and reaction is formed containing organic acid esters, alcohol and water
Vapour mixture condensation after import alcohol steam dehydrator, utilize dehydrant by the water in vapour mixture in alcohol steam dehydrator
Absorb in time and reaction is carried out to esterification, alcohol is imported esterifier simultaneously and recycles as reaction substrate, continuously
Circular response is complete to organic acid reaction, reacts having in the organic acid esters in alcohol steam generator and esterifier after terminating
Machine acid esters compound is transported in rectifying column carry out rectification purification, obtains organic acid esters compound.The invention also discloses and utilize this device
The method of esterification organic acid, the method condition is controlled, and organic acid esters yield is high, malate compound in malic acid is esterified
Yield improves more than 30%.
Accompanying drawing explanation
In order to make the purpose of the present invention, technical scheme and beneficial effect clearer, the present invention provides drawings described below:
Fig. 1 is the aqueous phase esterifying organic acid structure drawing of device of circular response.
Detailed description of the invention
Below in conjunction with accompanying drawing, the preferred embodiments of the present invention are described in detail.Unreceipted actual conditions in embodiment
Experimental technique, generally according to normal condition or according to the condition proposed by manufacturer.
Embodiment 1
The aqueous phase organic acid esters gasifying device of circular response, its structure is as shown in Figure 1.As it is shown in figure 1, the aqueous phase of circular response has
The Esterification device of machine includes esterifier 1, alcohol steam dehydrator 2 and rectifying column 3, and wherein esterifier 1 top is by setting
Be equipped with condensing unit 13 and be passed through the pipeline bottom alcohol steam dehydrator 2 and be connected with alcohol steam dehydrator 2；Alcohol steam dehydrator
The reflux line that 2 tops are passed through bottom esterifier 1 by setting is connected with esterifier 1；Alcohol steam dehydrator 2 end
Portion is connected with rectifying column 3 by pipeline.When utilizing this device esterification organic acid, alcohol steam dehydrator adds dehydrant,
Dehydrant can be 3A molecular sieve, silica gel or its mixture；For the organic acid esters after making alcohol get rid of and reclaiming rectification during distillation,
Alcohol air vent is set at rectifying column 3 top, organic acid esters outlet is set bottom rectifying column 3.
For controlling the additional proportion of reaction raw materials and realizing continuous esterification, arrange on esterifier top organic acid starting material tank 4,
Raw polyol tank I 5 and catalysagen batch can 6；Alcohol steam dehydrator 2 top is provided with raw polyol tank II 7；And organic acid is former
On the pipeline that batch can 4, raw polyol tank I 5 and catalysagen batch can 6 are connected with esterifier, raw polyol tank II 7 and alcohol steam
It is respectively provided with two-port valve on the pipeline that dehydrator 2 connects and adds to control raw material, need to open when adding raw material corresponding two-port valve,
Finish, close two-port valve.
For controlling esterification speed, the pipeline at condensing unit two ends is respectively provided with two-port valve I 15, reflux line is arranged
There is two-port valve II 16.
The aqueous phase organic acid esters gasifying device of the circular response of the present invention, the heat needed for reaction can be provided by outside, it is preferred that
And it is respectively provided with heater I 9 and heater II 10 bottom alcohol steam dehydrator 2 bottom esterifier 1.
In order to make reaction more abundant, divide bottom esterifier 1 and alcohol steam dehydrator 2 top base is respectively provided with and stretches into
Bottom esterifier 1 and the agitator I 11 of alcohol steam dehydrator 2 and agitator II 12.
Enter rectifying column 3 to control product, reactant liquor delivery pump 14 is being set on the connection pipeline of rectifying column 3.
Owing to, in esterification reaction process, esterifier 1 also containing a small amount of organic acid esters, in order to improve organic acid esters
Yield, can be connected esterifier 1 with rectifying column 3 by pipeline, and be controlled by two-port valve；Can also be anti-by esterification
Device 1 is answered to be connected with rectifying column 3 after being merged by the connection pipeline between pipeline with alcohol steam dehydrator 2 and rectifying column 3 again.
Embodiment 2
The method of the aqueous phase organic acid esters gasifying device esterification organic acid of circular response, specifically comprises the following steps that organic acid soln and alcohol
In esterifier, carry out esterification with acid, obtain the vapour mixture containing organic acid esters, water and alcohol, then gained is steamed
It is passed through after vapour mixture is condensed in the alcohol steam dehydrator of interpolation dehydrant and is dehydrated, simultaneously by the alcohol in alcohol steam dehydrator
Being back in esterifier, circular response to chemical reaction reaches balance, finally by alcohol steam dehydrator or/and esterifier
In reactant liquor be passed through rectifying column remove alcohol obtain organic acid esters.
Below as a example by aqueous solution of malic acid is esterified as malate in said apparatus:
Method 1: malate is prepared in aqueous solution of malic acid esterification: in esterifier in proportion for 2:2:4 (Kg:L:
L) being separately added into mass fraction is 60% aqueous solution of malic acid, methanol and concentrated sulphuric acid, under the conditions of being then heated to 90 DEG C under stirring
Carry out esterification, and formed containing malate, the vapour mixture of first alcohol and water, then by configured for vapour mixture have cold
Solidifying installing pipes is passed through under the liquid level of the alcohol steam dehydrator containing methanol and 3A molecular sieve dehydration agent, the most under agitation heats
To 50 DEG C, adding under the liquid level that thermogenetic methanol steam passes back into esterifier, alcohol steam was dehydrated after 5 hours by circular response
Product in device is passed through in rectifying column distillation and removes methanol, it is thus achieved that malic acid dimethyl ester product, malic acid diformazan in terms of malic acid
Ester products yield is 85%.
Method 2: malate is prepared in aqueous solution of malic acid esterification: in esterifier in proportion for 6:5:0.5 (Kg:L:
L) being separately added into mass fraction is 50% aqueous solution of malic acid, methanol and concentrated sulphuric acid, under the conditions of being then heated to 90 DEG C under stirring
Carry out esterification, and formed containing malate, the vapour mixture of first alcohol and water, then by configured for vapour mixture have cold
Solidifying installing pipes is passed through under the liquid level of the alcohol steam dehydrator containing methanol and Silicagel dehydration agent, is the most under agitation heated to 70 DEG C,
Add under the liquid level that thermogenetic methanol steam passes back into esterifier, circular response anti-by alcohol steam dehydrator after 4 hours
Answer product to be passed through in rectifying column distillation and remove methanol, it is thus achieved that malic acid dimethyl ester product, malic acid dimethyl ester product is received in terms of malic acid
Rate is 82%.
Method 3: malate is prepared in aqueous solution of malic acid esterification: in esterifier in proportion for 10:50:20 (Kg:
L:L) being separately added into mass fraction is 40% aqueous solution of malic acid, methanol and concentrated sulphuric acid, is then heated to 120 DEG C of bars under stirring
Carry out esterification under part, and formed containing malate, the vapour mixture of first alcohol and water, then that vapour mixture is configured
There is condensing unit pipeline to be passed through under the liquid level of the alcohol steam dehydrator containing 3A molecular sieve dehydration agent, be the most under agitation heated to
90 DEG C, add under the liquid level that thermogenetic methanol steam passes back into esterifier, circular response after 2 hours by alcohol steam dehydrator
In product be passed through in rectifying column distillation remove methanol, it is thus achieved that malic acid dimethyl ester product, malic acid dimethyl ester in terms of malic acid
Product yield is 80%.
Method 4: malate is prepared in aqueous solution of malic acid esterification: in esterifier in proportion for 7.5:20:4 (Kg:L:
L) being separately added into mass fraction is 40% aqueous solution of malic acid, methanol and concentrated sulphuric acid, under the conditions of being then heated to 80 DEG C under stirring
Carry out esterification, and formed containing malate, the vapour mixture of first alcohol and water, then by configured for vapour mixture have cold
Solidifying installing pipes is passed through under the alcohol steam dehydrator liquid level containing methanol and dehydrant (3A molecular sieve: silica gel=1:1)；Then exist
Being heated to 50 DEG C under stirring, add under the liquid level that thermogenetic methanol steam passes back into esterifier, circular response is after 10 hours
Product in esterifier and alcohol steam dehydrator being passed through in rectifying column distillation and removes methanol, neutralize concentrated sulphuric acid, extraction obtains
Obtaining malic acid dimethyl ester product, in terms of malic acid, malic acid dimethyl ester product yield is 84.5%.
In above-described embodiment, aqueous solution of malic acid uses microorganism direct fermentation to produce malic acid, but uses microorganism direct fermentation
Method produces malic acid and there is more heteroacid by-product such as succinic acid, acetic acid etc., is esterified and reaction is generated other by-product esters, needs
Using further rectification to separate, its production cost is higher.For overcoming this problem, preferably apple aqueous acid is by Aureobasidium pullulans
The fermenting and producing fermentation liquid containing polymalic acid salt, is then prepared fermentation liquor acid hydrolysis.Aureobasidium pullulans fermentative Production
Polymalic acid salt, there is sweat and do not produce the advantage of heteroacid by-product, then by the fermentation liquor acid containing polymalic acid salt
Hydrolysis prepares high-purity L MALIC ACID (application number 201210200500.0) aqueous solution, and prepared L MALIC ACID aqueous solution is used
The circulation way of distillation carries out esterification and prepares malate.
Wherein the preparation method of L MALIC ACID aqueous solution is as follows:
(1) seed liquor of activation is inoculated in the fermentation tank containing fermentation medium, controls remaining sugar concentration at more than 20g/L,
Temperature is 23～30 DEG C, ventilation ratio is that 1:0.8～1:1.6 (v/v) ferments 96～200 hours, and in sweat, stream adds CaCO3Control
PH processed is 5.0～6.5, adds glucose when remaining sugar concentration is less than 20g/L；Described fermentative medium formula is carbon source
50～200g/L, nitrogen source 1～5g, KH2PO40.005～0.3g/L, ZnSO40.005～0.3g/L and MgSO40.005～0.3g/L；
Described carbon source is one or more in glucose, sucrose, xylose, molasses, lactose and fructose；Described nitrogen source be ammonium sulfate,
One or more in ammonium chloride, potassium nitrate or ammonium nitrate.
(2) fermentation liquid is removed thalline, must ferment the stillness of night, add sulphuric acid or hydrochloric acid after then fermentation clear liquid being concentrated to final concentration
It is 0.5～2M, then acid hydrolysis 4～10 hours under the conditions of 70～95 DEG C, it is thus achieved that aqueous solution of malic acid, wherein said removal thalline
Method be by the ultrafiltration membrance filter of fermentation liquid molecular weight 10KDa；Described concentration is by fermentation clear liquid molecular weight 200Da
NF membrane concentrate.
Said method is also applied for the carboxylate synthesis of the organic carboxyl acids such as succinic acid, fumaric acid, adipic acid.
Finally illustrating, preferred embodiment above is only in order to illustrate technical scheme and unrestricted, although by above-mentioned
The present invention is described in detail by preferred embodiment, it is to be understood by those skilled in the art that can in form and
In details, it is made various change, without departing from claims of the present invention limited range.
Claims (10)
1. the aqueous phase organic acid esters gasifying device of circular response, it is characterised in that: include esterifier, alcohol steam dehydrator and rectification
Tower is that described esterifier top is provided by condensing unit and be passed through the pipeline bottom alcohol steam dehydrator and take off with alcohol steam
Hydrophone connects；Described alcohol steam dehydrator top is passed through the reflux line bottom esterifier with esterifier even by setting
Connect；It is connected with rectifying column by pipeline bottom described alcohol steam dehydrator；
Described rectifying column top is provided with alcohol air vent, and rectifier bottoms is provided with organic acid esters outlet.
The aqueous phase organic acid esters gasifying device of circular response the most according to claim 1, it is characterised in that: on described esterifier
Portion is provided with organic acid head tank, raw polyol tank I and catalysagen batch can；Described alcohol steam dehydrator top is provided with raw polyol
Tank II.
The aqueous phase organic acid esters gasifying device of circular response the most according to claim 1 or claim 2, it is characterised in that: described condensing unit
It is respectively provided with two-port valve I on the pipeline at two ends, described reflux line is provided with two-port valve II；Described organic acid head tank, alcohol
Controlled by two-port valve respectively between head tank I and catalysagen batch can and esterifier.
The aqueous phase organic acid esters gasifying device of circular response the most according to claim 1, it is characterised in that: at the bottom of described esterifier
It is respectively provided with having heaters I and heater II bottom portion and described alcohol steam dehydrator.
The aqueous phase organic acid esters gasifying device of circular response the most according to claim 1, it is characterised in that: described esterifier top
Portion is provided with the agitator I stretched into bottom esterifier；Described alcohol steam dehydrator top is provided with stretches into alcohol steam dehydrator
The agitator II of bottom.
The aqueous phase organic acid esters gasifying device of circular response the most according to claim 1, it is characterised in that: at the bottom of described esterifier
Portion is provided by the pipeline of two-port valve and is connected with described rectifying column；Or bottom esterifier, it is provided by the pipeline of two-port valve
The pipeline being connected with between alcohol steam dehydrator and rectifying column is connected with described rectifying column after merging.
The aqueous phase organic acid esters gasifying device of circular response the most according to claim 1, it is characterised in that: with described rectifying column connecting tube
Reactant liquor delivery pump it is provided with on road.
8. the method utilizing the aqueous phase organic acid esters gasifying device esterification organic acid of circular response described in any one of claim 1～7, its feature
It is: organic acid soln is carried out esterification with alcohol and acid in esterifier, obtains the steaming containing organic acid esters, water and alcohol
Vapour mixture, is then dehydrated being passed through after condensed for gained vapour mixture in the alcohol steam dehydrator adding dehydrant, with
Time by the alcohol reflux in alcohol steam dehydrator to esterifier, circular response to chemical reaction reaches balance, is finally steamed by alcohol
Vapour dehydrator is or/and the reactant liquor in esterifier is passed through rectifying column removal alcohol or/and acid obtains organic acid esters.
Method the most according to claim 8, it is characterised in that: malic acid solution is entered in esterifier with alcohol and concentrated sulphuric acid
Row esterification, obtains the vapour mixture containing malate, water and alcohol, is then passed through after condensed for gained vapour mixture
Add in the alcohol steam dehydrator of dehydrant and be dehydrated, simultaneously by the methanol eddy in alcohol steam dehydrator to esterifier,
Circular response to chemical reaction reaches balance, finally by alcohol steam dehydrator or/and the reactant liquor in esterifier is passed through rectifying column
Remove alcohol and/or sulphuric acid obtains malate.
Method the most according to claim 9, it is characterised in that: will contain malic acid solution and methanol and concentrated sulphuric acid by
2～10:5～50:0.5～20 (g:ml:ml) ratio adds esterifier esterification under the conditions of 80～120 DEG C, obtains containing Herba Marsileae Quadrifoliae
The vapour mixture of fruit acid ester, water and methanol, then will be passed through the alcohol steam adding dehydrant after condensed for gained vapour mixture
Dehydrator is dehydrated, the methanol in alcohol steam dehydrator is back in esterifier under the conditions of 50～90 DEG C simultaneously,
Circular response 2～10 hours, finally by alcohol steam dehydrator or/and reactant liquor in esterifier be passed through rectifying column remove alcohol or/
Malate is obtained with sulphuric acid.
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| CN201610368028.XA CN105884611B (en) | 2016-05-26 | 2016-05-26 | The water phase esterifying organic acid device of circular response and its method for being esterified organic acid |
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| CN201610368028.XA CN105884611B (en) | 2016-05-26 | 2016-05-26 | The water phase esterifying organic acid device of circular response and its method for being esterified organic acid |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1225919A (en) * | 1998-12-02 | 1999-08-18 | 巴陵石化岳阳石油化工总厂 | Synthesizing method for dimethyl ester of mixed acid of butane diacid, glutaric acid and hexane diacid |
| CN101018758A (en) * | 2004-07-19 | 2007-08-15 | 密执安州大学 | Improved process for production of organic acid esters |
| CN202717761U (en) * | 2012-05-31 | 2013-02-06 | 源华能源科技（福建）有限公司 | Continuous esterification dehydration reaction device of biodiesel |
-
2016
- 2016-05-26 CN CN201610368028.XA patent/CN105884611B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1225919A (en) * | 1998-12-02 | 1999-08-18 | 巴陵石化岳阳石油化工总厂 | Synthesizing method for dimethyl ester of mixed acid of butane diacid, glutaric acid and hexane diacid |
| CN101018758A (en) * | 2004-07-19 | 2007-08-15 | 密执安州大学 | Improved process for production of organic acid esters |
| CN202717761U (en) * | 2012-05-31 | 2013-02-06 | 源华能源科技（福建）有限公司 | Continuous esterification dehydration reaction device of biodiesel |
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