CN204170712U - A kind of for the epoxidised tubular reaction device of unsaturated fatty acid ester - Google Patents
A kind of for the epoxidised tubular reaction device of unsaturated fatty acid ester Download PDFInfo
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- CN204170712U CN204170712U CN201420450044.XU CN201420450044U CN204170712U CN 204170712 U CN204170712 U CN 204170712U CN 201420450044 U CN201420450044 U CN 201420450044U CN 204170712 U CN204170712 U CN 204170712U
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Abstract
The utility model discloses a kind of for the epoxidised tubular reaction device of unsaturated fatty acid ester.This device is made up of shell-and-tube reactor, medium condenser, mediation cycle pump, feedstock circulation pump and material heater.The tube side of shell-and-tube reactor walks unsaturated fatty acid ester raw material, and shell side adopts boiling point and the close solvent of epoxidation reaction optimum temperature to move thermal medium.The tube side of the medium condenser of tubular structure is walked to move thermal medium, and shell side adopts circulating water.The top of shell-and-tube reactor is connected with the tube side of medium condenser.The outlet of medium condenser tube side is connected with mediation cycle pump.Mediation cycle delivery side of pump enters the shell side of shell-and-tube reactor.When this reaction unit is used for epoxidation process, reaction liberated heat is taken away by the gasification of medium, ensure that reaction system is carried out under being in comparatively suitable temperature, significantly improves the selective of reaction, i.e. product epoxide number.Meanwhile, the circulating hot water that medium condenser obtains can be used for heating raw, and capacity usage ratio is high.
Description
Technical field
The utility model relates to chemical production equipment field, is specially a kind of for the epoxidised tubular reaction device of unsaturated fatty acid ester.
Background technology
The epoxide number of the epoxy aliphatic acid methyl ester product that existing peroxyformic acid method obtains is generally about 3.5%, and high-quality product can reach 4.0%, but need working concentration up to 50% H
2o
2.The low main cause of unsaturated fatty acid methyl ester epoxide number is caused to be the hydrolysis of epoxide ring.Epoxidized soybean oil is the green non-poisonous secondary plasticizer(-iser) of one and stabilizing agent that use in PVC processing.Because it is non-toxic and the feature of environmental protection, apply increasingly extensive.The synthesis of epoxidized soybean oil, key reaction principle is that double bond in soybean oil and peroxy acid react, and generates epoxide group.Common soybeans oil iodine number is generally at 125 (gI
2/ 100g) left and right, if wherein unsaturated double-bond and peroxy acid fully react, its theoretical epoxy value should about 8.5%, and the epoxidized soybean oil obtained is synthesized in domestic production, and its epoxide number is generally about 5.9% ~ 6.0%.Adopt the means such as high-strength hydrogen peroxide, appropriate catalysts, interpolation auxiliary agent and acidity regulator can improve reaction environment to suppress hydrolysis, appropriateness improves product epoxide number.
The epoxidation process of unsaturated fatty acid ester is the exothermic reaction of a moderate strength.Temperature controls to be the key problem in technology improving product epoxide number, and the main tank reactor that adopts moves thermal control temperature by cooling water circulation at present.The factors such as by the impact in consersion unit space, the area of heat exchanger tube can not be too large, and stir speed (S.S.) is slower in addition, seriously constrain and move hot speed.This just causes reaction mass extremely uneven in the Temperature Distribution of diverse location, and product epoxide number is difficult to maintain higher level.Can find out, the selection of optimization of the structure of reactor and heat-removing way is the effective measures improving epoxidation plants efficiency and product quality.
Summary of the invention
The utility model is comparatively large for solving thermal discharge in formic acid method epoxidation process, the difficult control of temperature of reaction mass, and provides a kind of for the epoxidised tubular reaction device of unsaturated fatty acid ester.It can solve the product epoxide number that exists in conventional production equipment problem on the low side.The tubular reaction device of the present invention's design is made up of shell-and-tube reactor, feedstock circulation pump, medium condenser, mediation cycle pump and material heater.Shell-and-tube reactor tube side walks reaction raw materials, and shell side is walked to move thermal medium.Medium after gasification enters the shell side that medium condenser condenses Posterior circle is back to shell-and-tube reactor.Epoxidation process liberated heat is taken away by the gasification of medium, ensure that reaction system is carried out under being in more uniform temperature, and the method significantly improves the selective of epoxidation process and product epoxide number.
The utility model is achieved by the following technical solutions.
A kind of for the epoxidised tubular reaction device of unrighted acid, it comprises shell-and-tube reactor, medium condenser, mediation cycle pump, feedstock circulation pump and material heater.The tube side of described shell-and-tube reactor walks unsaturated fatty acid ester raw material, and shell side adopts boiling point and the close solvent of epoxidation reaction optimum temperature to move thermal medium.Described medium condenser is also tubular structure, and tube side walks medium, and shell side adopts circulating water.Described mediation cycle pump and feedstock circulation pump are centrifugal structure.The top of described shell-and-tube reactor is connected with the tube side of medium condenser.The outlet of medium condenser tube side is connected with mediation cycle pump.Mediation cycle delivery side of pump enters the shell side of shell-and-tube reactor.Shell-and-tube reactor, medium condenser, mediation cycle pump, feedstock circulation pump with all adopt pipeline between material heater and be connected.The connecting pipe of described shell-and-tube reactor and medium condenser is provided with mediation cycle pump, and nearly shell-and-tube reactor end is provided with material heater on pipeline.The pipeline of described shell-and-tube reactor outlet and entrance is provided with feedstock circulation pump.Described unsaturated fatty acid ester raw material comprises soybean oil, cottonseed oil, rapeseed oil, fatty acid methyl ester and fatty-acid ethyl ester.The mixed solvent that described epoxidation process temperature control medium used comprises n-hexane, cyclohexane and two or three can form azeotropic mixture.
The utility model beneficial effect is compared with prior art that apparatus structure is simple, preparation process gentle coherent, reaction time epoxide number that is short, product is high, and reaction heat can utilize further, production cost is low, efficiency is high, energy-saving benefit is remarkable.
Accompanying drawing explanation
now by reference to the accompanying drawings the utility model is described further.
fig. 1 is structural representation of the present utility model.In figure1, material heater; 2, shell-and-tube reactor; 3, medium condenser; 4, mediation cycle pump; 5, feedstock circulation pump.
Detailed description of the invention
As shown in Figure 1, the utility model is a kind of for the epoxidised tubular reaction device of unsaturated fatty acid ester, and it comprises shell-and-tube reactor (2), medium condenser (3), mediation cycle pump (4), Matter Transfer pump (5) and material heater (1).The tube side of shell-and-tube reactor (2) walks unsaturated fatty acid ester raw material, and shell side adopts boiling point and the close solvent of epoxidation reaction optimum temperature to move thermal medium.Medium condenser (3) is also tubular structure, and tube side walks medium, and shell side adopts circulating water.The top of shell-and-tube reactor (2) is connected with the tube side of medium condenser (3).The outlet of medium condenser (3) tube side is connected with mediation cycle pump (4).The outlet of mediation cycle pump (4) enters the shell side of shell-and-tube reactor (2).
Further, described unsaturated fatty acid ester raw material comprises soybean oil, cottonseed oil, rapeseed oil, fatty acid methyl ester and fatty-acid ethyl ester.
Further, described epoxidation process temperature control thermal medium of moving used comprises the mixed solvent that n-hexane, cyclohexane and ethyl acetate and ethanol etc. two or three can form azeotropic mixture.
Embodiment one
As shown in Figure 1, be 110 (gI by flow 1500 kgs/hour of iodine numbers respectively
2/ 100g) fatty acid methyl ester, a certain amount of industrial formic acid and 30% hydrogen peroxide in proportion pump to the charge door of the front unsaturated fatty acid ester of material heater (1) and hydrogen peroxide.Shell-and-tube reactor number of tubes 30, length 3 meters, pipe sizing is 42*6, material stainless steel.To thermal medium n-hexane be moved from tank pump to the shell side of shell-and-tube reactor, open medium condenser cooling water valve.Open material heater, mediation cycle pump and feedstock circulation pump, control reaction temperature at 70 DEG C, after continuous circulation operates 20 minutes.Opened by reactor dispensing valve, reactant mixture enters the standing tank layering in downstream.Upper strata is epoxy aliphatic acid methyl ester phase, and lower floor is aqueous phase.Upper strata is after washing and alkali cleaning remove formic acid, and the further vacuum dehydration of epoxy aliphatic acid methyl ester obtains finished product.The quality index of gained epoxy aliphatic acid methyl ester product: color and luster (Fe-Co colorimetric) <150, epoxide number (%) >4.2, iodine number (gI
2/ 100g) <5.0, acid number (mgKOH/g) <0.32, heating loss (125 DEG C of 2 h) %<0.25, heat endurance (epoxy retention rate 177 DEG C 3 h) %>95, moisture <0.15%, flash-point >185 DEG C.Wherein, epoxide number 4.2% is significantly higher than the epoxide number obtaining epoxy aliphatic acid methyl ester product in tank reactor from the raw material of identical iodine number under similar conditions.
Embodiment two
The utility model is also adapted to the preparation of epoxidized soybean oil.As shown in Figure 1, be 125 (gI by flow 1600 kgs/hour of iodine numbers respectively
2/ 100g) soybean oil, a certain amount of industrial formic acid and 30% the unsaturated fatty acid ester of hydrogen peroxide in proportion before pump to material heater and the charge door of hydrogen peroxide.Shell-and-tube reactor number of tubes 36, length 3.5 meters, pipe sizing is 42*6, material stainless steel.By moving thermal medium ethanol and ethyl acetate mixture from tank pump to the shell side of shell-and-tube reactor, open medium condenser cooling water valve.Open material heater, mediation cycle pump and feedstock circulation pump, control reaction temperature at 75 DEG C, after continuous circulation operates 25 minutes.Opened by reactor dispensing valve, reactant mixture enters the standing tank layering in downstream.Upper strata is epoxy soybean oil phase, and lower floor is aqueous phase.Upper strata is after washing conjunction alkali cleaning removes formic acid, and the further vacuum dehydration of epoxidized soybean oil obtains finished product.The quality index of gained epoxy soybean oil product: color and luster (Fe-Co colorimetric) <210, epoxide number (%) >6.2, iodine number (gI
2/ 100g) <5.5, acid number (mgKOH/g) <0.3, heating loss (125 DEG C of 2 h) %<0.25, heat endurance (epoxy retention rate 177 DEG C 3 h) %>96, moisture <0.15%, heavy metal (in Pb) mg/kg<9, arsenic (As) mg/kg<11, flash-point >275 DEG C.Wherein, epoxide number 6.3% is significantly higher than the epoxide number obtaining epoxy soybean oil product in tank reactor from the raw material of identical iodine number under similar conditions.
Claims (4)
1. for the epoxidised tubular reaction device of unsaturated fatty acid ester, it is characterized in that, it comprises shell-and-tube reactor (2), medium condenser (3), mediation cycle pump (4), feedstock circulation pump (5) and material heater (1); The tube side of described shell-and-tube reactor (2) walks unsaturated fatty acid ester raw material, and shell side adopts boiling point and the close solvent of epoxidation reaction optimum temperature to move thermal medium; Described medium condenser (3) is also tubular structure, and tube side walks medium, and shell side adopts cooling water to move thermal medium; Described mediation cycle pump (4) and feedstock circulation pump (5) are centrifugal structure; The top of described shell-and-tube reactor (2) is connected with the tube side of medium condenser (3); The outlet of medium condenser (3) tube side is connected with mediation cycle pump (4); The outlet of mediation cycle pump (4) enters the shell side of shell-and-tube reactor (2).
2. as claimed in claim 1 a kind of for the epoxidised tubular reaction device of unsaturated fatty acid ester, it is characterized in that shell-and-tube reactor (2), medium condenser (3), mediation cycle pump (4), between feedstock circulation pump (5) with material heater (1), all adopt pipeline to be connected; Described shell-and-tube reactor (2) is provided with mediation cycle pump (4) with the connecting pipe of medium condenser (3), and nearly shell-and-tube reactor (2) end is provided with material heater (1) on pipeline; The pipeline of described shell-and-tube reactor (2) outlet and entrance is provided with feedstock circulation pump (5).
3. as claimed in claim 1 a kind of for the epoxidised tubular reaction device of unsaturated fatty acid ester, it is characterized in that described unsaturated fatty acid ester raw material comprises soybean oil, cottonseed oil, rapeseed oil, fatty acid methyl ester and fatty-acid ethyl ester.
4. as claimed in claim 1 a kind of for the epoxidised tubular reaction device of unsaturated fatty acid ester, it is characterized in that the mixed solvent that described epoxidation process temperature control medium used comprises n-hexane, cyclohexane and two or three can form azeotropic mixture.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201420450044.XU CN204170712U (en) | 2014-08-12 | 2014-08-12 | A kind of for the epoxidised tubular reaction device of unsaturated fatty acid ester |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201420450044.XU CN204170712U (en) | 2014-08-12 | 2014-08-12 | A kind of for the epoxidised tubular reaction device of unsaturated fatty acid ester |
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| CN204170712U true CN204170712U (en) | 2015-02-25 |
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| CN201420450044.XU Expired - Fee Related CN204170712U (en) | 2014-08-12 | 2014-08-12 | A kind of for the epoxidised tubular reaction device of unsaturated fatty acid ester |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105561893A (en) * | 2016-01-26 | 2016-05-11 | 浙江工业大学 | Grease epoxidation reaction device |
-
2014
- 2014-08-12 CN CN201420450044.XU patent/CN204170712U/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105561893A (en) * | 2016-01-26 | 2016-05-11 | 浙江工业大学 | Grease epoxidation reaction device |
| CN105561893B (en) * | 2016-01-26 | 2018-05-29 | 浙江工业大学 | A kind of grease collar oxidation reaction apparatus |
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| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20150225 Termination date: 20150812 |
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| EXPY | Termination of patent right or utility model |