CN205893125U - Device of preparation fumaric acid monoester - Google Patents
Device of preparation fumaric acid monoester Download PDFInfo
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- CN205893125U CN205893125U CN201620528936.6U CN201620528936U CN205893125U CN 205893125 U CN205893125 U CN 205893125U CN 201620528936 U CN201620528936 U CN 201620528936U CN 205893125 U CN205893125 U CN 205893125U
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- cold well
- reactor
- pipeline
- mercury lamp
- fumaric monoalkylester
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Abstract
The utility model relates to a device of preparation fumaric acid monoester, including the seal reaction ware, the cryogenic cooling pump, the photoreaction appearance, cold well, the bottom of seal reaction ware is equipped with a magnetic stirrers, the lower extreme of cold well be located the seal reaction ware, be equipped with a mercury lamp in the cold well, the mercury lamp with photoreaction appearance electricity connect, the cryogenic cooling pump passes through the pipeline intercommunication with cold well, still be equipped with a thermometer that is used for detecting the interior temperature of seal reaction ware in the seal reaction ware, the seal reaction ware still is connected with a female fluid recovery unit through the pipeline, and simplification equipment reduces the energy consumption, product productivity purity is more ideal, one step synthesis of, and the side reaction is few, and synthetic product purity is high, the reaction is not used to have corrosive hydrochloric acid and is catalyst, not etch apparatus, the washing of product with retrieve the mother liquor and does not use noxious material such as benzene, toluene, do not cause the pollution to the environment, low in production cost is favorable to the industrialization.
Description
Technical field
This utility model relates to chemical industrial field, specifically a kind of device preparing fumaric monoalkylester.
Background technology
The antifungus agent being usually used in the industries such as food, feedstuff in the market is mainly organic acid and its esters；As benzoic acid
And its esters, sorbic acid and its esters, propanoic acid and its esters etc..But these products are both needed under suitable ph value environment, (ph
Value is less than 5) just there are bacteriostasis.Organic acid ester antifungus agent, its toxicity is very low, and bacteriostasis be far longer than organic acid and its
Salt, and the ph value wider range being suitable for, ph value all has good bacteriostasis between 3-8.As the rich horse in recent years developed
Esters of gallic acid antifungus agent has dimethyl fumarate (dwf), DEF (def), fumaric acid dipropyl (dpf), fumaric acid two
Butyl ester, monomethyl fumarate (mmf), monomethyl ester (mef), fumaric acid list propyl ester (mpf) and monobutyl fumarate (mbf)
Deng.The equal low toxicity of these products, has efficient Antibacteria effect.Wherein most representative be dimethyl fumarate, but it produce and
Skin and some stimulations of mucosa to people in application, have gradually limited its use in developed countries such as America and Europes.And richness horse
The fumaric monoalkylester class compound such as sour mono-methyl, monomethyl ester is due to having low irritant and efficient corrosion resisting, the spy such as mould proof
Point is day by day had wide market prospect by people are of interest.
The preparation of fumaric monoalkylester class compound, the generally maleic anhydride of the amount of material and the corresponding unitary such as employing
Alcohol is raw material.First carry out alcoholysis reaction, generate corresponding maleic anhydride monoesters, then carry out isomerization reaction generating accordingly
Fumaric monoalkylester.
Reaction equation:
Br dilute anhydride monohydric alcohol br dilute anhydride monoesters fumaric monoalkylester
The shortcoming that above-mentioned technique exists has
(1) response time length, reactions steps are loaded down with trivial details.Two steps are needed to carry out.Carry out alcoholysis with monohydric alcohol first, then make again
Prepare monomethyl fumarate with catalyst (hydrochloric acid, aluminum chloride etc.) isomerization.
(2) yield and purity are undesirable.Because current technique is all to be carried out using two-step method, occur in preparation process
By-product is more, and yield is not high by only 70% about.
(3) catalyst using is corrosive, unfriendly to environment.The catalyst using both at home and abroad be mostly with hydrochloric acid,
Aluminum chloride and acyl chlorides, these severe corrosion equipments.
(4) product, due to needing to be washed using the poisonous solvent such as substantial amounts of benzene, toluene containing hydrochloric acid, is made to environment
Become pollution, production cost high, be unfavorable for industrialized production.
Utility model content
In order to overcome the shortcoming of above-mentioned prior art, the purpose of this utility model is to provide a kind of solution in existing process instead
Long between seasonable, reactions steps are loaded down with trivial details, product yield and purity are undesirable, are unfavorable for work to environment, production cost height
The device used by process preparing fumaric monoalkylester of industry.
For reaching above-mentioned purpose, this utility model employs the following technical solutions, a kind of device preparing fumaric monoalkylester, bag
Include sealing reactor, sub-cooled pump, photoreaction instrument, cold well, the bottom of described sealing reactor is provided with magnetic stirring apparatuss,
The lower end of described cold well is located in sealing reactor, is provided with a mercury lamp, described mercury lamp and described light in described cold well
Reaction instrument electrical connection, described sub-cooled pump is connected by pipeline with cold well；It is additionally provided with a use in described sealing reactor
In the thermometer of detection sealing reactor temperature, described sealing reactor is also associated with a disposing mother liquor dress by pipeline
Put.
Described mother liquor recovering device includes vacuum pump, round-bottomed flask and the coil condenser being located above round-bottomed flask,
The lower end of described coil condenser is located in round-bottomed flask, and described vacuum pump is connected by pipeline with round-bottomed flask, described
The upper end of coil condenser with sealing reactor be connected by pipeline.
The ultraviolet that described ultraviolet source sends irradiates optical wavelength 260nm～400nm.
Described ultraviolet source is mercury lamp.
The power of described mercury lamp is 500～1500w.
The power of described mercury lamp is 1000w.
This utility model adopts above technical scheme, have advantages below, 1) structure is simple, is provided using this utility model
Reaction unit use the reaction time short, process is simple, a step can with sinteticses, simplify equipment, reducing energy consumption.
(2) product yield purity is more satisfactory, one-step synthesis, and side reaction is few, and sinteticses purity is high.
(3) reaction does not use and has corrosive hydrochloric acid and make catalyst, not etching apparatus.
(4) washing of product and recovery mother solution do not use the noxious substances such as benzene, toluene, environment is not polluted, produces
Low cost, is conducive to industrialization.
Brief description
Fig. 1 is structural representation of the present utility model；
In figure: 1. vacuum pump；2. coil condenser；3. round-bottomed flask；4. cold well；5. ultraviolet source；6. thermometer；7.
Photoreaction instrument；8. sub-cooled pump；9. the magnetic stirring apparatuss with heating；10. seal reactor.
Specific embodiment
With reference to the accompanying drawings and examples this utility model is described in detail.
A kind of process preparing fumaric monoalkylester, adds monohydric alcohol and maleic anhydride in light reaction device,
And a step is obtained by ultraviolet illumination obtain fumaric monoalkylester.
With maleic anhydride for raw material and monohydric alcohol under ultraviolet light, first carry out esterification, then carry out isomery
Change reaction one step and fumaric monoalkylester is obtained.
Reactional equation (1)
Br dilute anhydride monohydric alcohol br dilute anhydride monoesters fumaric monoalkylester
The difference that this process is had with current process be can be seen that by the description above and reactional equation
Be, this method during reaction it is only necessary to illumination it is achieved that and a step realize, without multistep, in preparation
During also without catalyst, the catalyst adopting in current process is substantially corrosive hydrochloric acid, and environment is made
Become pollution, and production cost is high, is conducive to industrialization, simultaneously because having the presence of catalyst, the purity ratio of product is relatively low, and
This method only needs to just to realize the generation of fumaric monoalkylester, process is simple by illumination one step, will not cause dirt to environment
Dye, the purity of product and yield are high simultaneously.Low production cost, is conducive to industrialization.
Particularly carry out in accordance with the following methods:
The mass ratio pressing 5～20:1 in light reaction device adds monohydric alcohol and maleic anhydride；Controlling reaction temperature
At -5～30 DEG C, react 1～3 hour, after the completion of reaction in the case of irradiating the ultraviolet source of optical wavelength 260nm～400nm
By reacted reactant liquor vacuum distillation, washing, sucking filtration, it is dried to obtain fumaric monoalkylester.
Embodiment 1
As shown in Figure 1, a kind of device preparing fumaric monoalkylester includes sealing reactor 10, sub-cooled pump 8, and light is anti-
Answer instrument 7, cold well 4, the bottom of described sealing reactor 10 is provided with magnetic stirring apparatuss 9, and the lower end of described cold well 4 is located at close
In envelope reactor 10, in described cold well 4, it is provided with a ultraviolet source 5, described ultraviolet source 5 and described photoreaction instrument 7 electricity
Connect, described sub-cooled pump 8 is connected by pipeline with cold well 4；It is additionally provided with one in described sealing reactor 10 to be used for examining
Survey the thermometer 6 of temperature in sealing reactor 10, described sealing reactor 10 is also associated with a disposing mother liquor dress by pipeline
Put.Sealing reactor 10 is used for holding reactant liquor, and magnetic stirring apparatuss 9 are used for the reactant liquor in stirring sealing reactor 10, and energy
Enough heated, ultraviolet source 5 provides ultraviolet lighting for reactant liquor, cold well 4 is lowered the temperature to ultraviolet source 5, it is to avoid temperature mistake
Height, sub-cooled pump 8 is lowered the temperature to ultraviolet source with cold well 4, and photoreaction instrument 7 controls the ultraviolet lighting of ultraviolet source.Anti-
Later substantial amounts of mother solution can should be remained, in order to recycle to disposing mother liquor, using mother liquor recovering device specifically this disposing mother liquor
Device includes vacuum pump 1, round-bottomed flask 3 and the coil condenser 2 being located at round-bottomed flask 3 top, described coil condenser 2
Lower end is located in round-bottomed flask 3, and described vacuum pump 1 is connected by pipeline with round-bottomed flask 3, described coil condenser 2
Upper end is connected by pipeline with sealing reactor 10；Particularly maleic anhydride and excessive monohydric alcohol add logical nitrogen to protect
In the sealing reactor 10 of shield, under ultraviolet light, (under mercury lamp or other LED lamp irradiation) is reacted, and opens magnetic agitation
Device 9(does not now leave and reacts under heating room temperature), so that reactant liquor is slowly stirred, in 1～3 hour response time, open low in reaction
Warm vacuum pump 8, (mainly lowers the temperature to mercury lamp, cryogenic vacuum pumps 8 are ined succession cold well 4, and cold well 4 purpose is to hydrargyrum to reactor cooling
Lamp is lowered the temperature) after the completion of reaction, need after the reaction to carry out vacuum distillation to the reactant liquor in reaction vessel (now to need out bottom
The heating function of magnetic stirring apparatuss 9) steam that obtains is exactly unreacted unitary by the condensed liquid of coil condenser 2
Alcohol, the solid product fumaric monoalkylester obtaining in sealing reactor 10.
Embodiment 2
10g maleic anhydride is dissolved completely in 100g methanol solvate the Photoreactor having nitrogen protection, control
Reaction temperature processed is 15 DEG C, ultraviolet light (wavelength 365nm, Output optical power 500w) reactant liquor, after reacting 2 hours, will be anti-
Liquid is answered to obtain monomethyl fumarate product 9.8g through vacuum distillation, washing, sucking filtration and after being dried.Product purity 96.8%, produces
Rate 97.8%.
Embodiment 3
10g maleic anhydride is dissolved completely in 50g alcohol solvent the Photoreactor having nitrogen protection, controls
Reaction temperature is -5 DEG C, ultraviolet light (wavelength 260nm, Output optical power 1000w) reactant liquor, after reacting 1 hour, will react
Liquid obtains monomethyl ester through vacuum distillation, washing, sucking filtration and after being dried and produces 9.1g.Product purity 96.2%, yield 89.5%.
Embodiment 4
10g maleic anhydride is dissolved completely in 200g propanol solvent the Photoreactor having nitrogen protection, control
Reaction temperature processed is 30 DEG C, ultraviolet light (wavelength 400nm, Output optical power 750w) reactant liquor, after reacting 3 hours, will be anti-
Liquid is answered to obtain fumaric acid list propyl ester product 9.7g after vacuum distillation, washing, sucking filtration, drying.Product purity 95.7%, yield
96.5%.
Embodiment 5
10g maleic anhydride is dissolved completely in 65g methanol solvate the Photoreactor having nitrogen protection, controls
Reaction temperature is 25 DEG C, ultraviolet light (wavelength 400nm, Output optical power 750w) reactant liquor, after reacting 2.5 hours, will be anti-
Liquid is answered to obtain monomethyl fumarate product 9.85g after vacuum distillation, washing, sucking filtration, drying.Product purity 97.7%, yield
98.5%.
Comparative example
The present embodiment carries out Experimental Comparison to current monomethyl fumarate technique processed, by 49g maleic anhydride and 12.7g
Absolute methanol puts in reactor, stirs under room temperature, and temperature rises to 33～35 DEG C automatically, reaction 35min about, maleic two
Anhydride all dissolves, and after adding 6.3g absolute methanol, heating in water bath is further continued for reacting after 30 minutes to after 50 DEG C, adjusts water-bath temperature
After degree rises to 80 DEG C, 3.1g good fortune horse acyl chlorides is added to carry out isomerization reaction in reactor, reaction 5min about, in reactant liquor
Crystal is had to separate out.Under thermal environment, temperature of reaction system is drastically increased to 120 DEG C, after insulation 10min, under temperature of reaction system
Fall, maintains reaction 125min at 80 DEG C of bath temperature.Finally, produced through dissolving, cooling, centrifugation, vacuum drying
Thing 53g, purity 68%, yield is 84.6%.
By current in the purity of the fumaric monoalkylester obtained by embodiment 2,3,4,5 and productivity ratio and comparative example
Process ration can be seen that this utility model offer embodiment 2,3,4,5 in any embodiment in system fumaric monoalkylester
Purity and productivity ratio be all significantly larger than in comparative example the purity of fumaric monoalkylester and the productivity ratio of system, this practicality simultaneously is newly
The embodiment that type provides does not use to be had corrosive hydrochloric acid and makees catalyst, not etching apparatus；The washing of product and recovery mother solution
Do not use the noxious substances such as benzene, toluene, environment is not polluted, low production cost, be conducive to industrialization.Pass through to implement simultaneously
Example 2,3,4,5 is as can be seen that embodiment 5 is preferred version, the product purity of preparation and yield highest.
Exemplified as above is only to illustration of the present utility model, does not constitute to protection domain of the present utility model
Limit, the every and same or analogous design of this utility model belongs within protection domain of the present utility model.
Claims (6)
1. a kind of device preparing fumaric monoalkylester is it is characterised in that include sealing reactor (10), sub-cooled pump (8), light
Reaction instrument (7), cold well (4), the bottom of described sealing reactor (10) is provided with magnetic stirring apparatuss (9), described cold well (4)
Lower end be located in sealing reactor (10), be provided with a ultraviolet source (5) in described cold well (4), described ultraviolet source (5)
Electrically connect with described photoreaction instrument (7), described sub-cooled pump (8) is connected by pipeline with cold well (4)；Described sealing
Be additionally provided with reactor (10) one for detection seal the thermometer (6) of reactor (10) interior temperature, described sealing reactor
(10) mother liquor recovering device is also associated with by pipeline.
2. a kind of device preparing fumaric monoalkylester according to claim 1 is it is characterised in that described disposing mother liquor fills
Put including vacuum pump (1), round-bottomed flask (3) and be located at coil condenser (2) above round-bottomed flask (3), described is snakelike cold
The lower end of condenser (2) is located in round-bottomed flask (3), and described vacuum pump (1) is connected by pipeline with round-bottomed flask (3), described
The upper end of coil condenser (2) with sealing reactor (10) be connected by pipeline.
3. a kind of device preparing fumaric monoalkylester according to claim 1 is it is characterised in that described ultraviolet source
(5) ultraviolet sending irradiates optical wavelength 260nm～400nm.
4. a kind of device preparing fumaric monoalkylester according to claim 1 is it is characterised in that described ultraviolet source
(5) it is mercury lamp.
5. a kind of device preparing fumaric monoalkylester according to claim 4 is it is characterised in that the power of described mercury lamp
For 500～1500w.
6. a kind of device preparing fumaric monoalkylester according to claim 5 is it is characterised in that the power of described mercury lamp is
1000w.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201620528936.6U CN205893125U (en) | 2016-06-03 | 2016-06-03 | Device of preparation fumaric acid monoester |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201620528936.6U CN205893125U (en) | 2016-06-03 | 2016-06-03 | Device of preparation fumaric acid monoester |
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| Publication Number | Publication Date |
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| CN205893125U true CN205893125U (en) | 2017-01-18 |
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ID=57766745
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| CN201620528936.6U Active CN205893125U (en) | 2016-06-03 | 2016-06-03 | Device of preparation fumaric acid monoester |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107141216A (en) * | 2017-03-06 | 2017-09-08 | 四川金江建材科技有限公司 | Concrete slump retaining agent intermediate synthetic method |
-
2016
- 2016-06-03 CN CN201620528936.6U patent/CN205893125U/en active Active
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107141216A (en) * | 2017-03-06 | 2017-09-08 | 四川金江建材科技有限公司 | Concrete slump retaining agent intermediate synthetic method |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C41 | Transfer of patent application or patent right or utility model | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20170119 Address after: 712000 Xianyang province Shaanxi City Weicheng Lin Road Patentee after: Shaanxi Energy Institute Patentee after: Ling Jie Address before: 712000 Xianyang City, Shaanxi Province Lin Weicheng district middle road Shaanxi Energy Institute Patentee before: Shaanxi Energy Institute |
|
| TR01 | Transfer of patent right |
Effective date of registration: 20210416 Address after: 713400 energy and chemical building materials Industrial Park, Jianjun Town, Yongshou County, Xianyang City, Shaanxi Province Patentee after: SHAANXI HUAHAOXUAN NEW ENERGY TECHNOLOGY DEVELOPMENT Co.,Ltd. Address before: 712000 Xianyang province Shaanxi City Weicheng Lin Road Patentee before: SHAANXI ENERGY INSTITUTE Patentee before: Ling Jie |
|
| TR01 | Transfer of patent right |