CN205170714U - Device of industrialization continuous production tetrahydrofurfuryl alcohol ether - Google Patents
Device of industrialization continuous production tetrahydrofurfuryl alcohol ether Download PDFInfo
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- CN205170714U CN205170714U CN201520759223.6U CN201520759223U CN205170714U CN 205170714 U CN205170714 U CN 205170714U CN 201520759223 U CN201520759223 U CN 201520759223U CN 205170714 U CN205170714 U CN 205170714U
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- Prior art keywords
- tetrahydrofurfuryl alcohol
- tubular reactor
- ethanol
- pump
- alcohol ether
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Abstract
The utility model relates to a device of industrialization continuous production tetrahydrofurfuryl alcohol ether, the device is including raw materials deposit - the measurement conveying system, tubular reactor system, dehydration system, rectification system and the product jar that link to each other in proper order. The device provided by the utility model be applicable to industrialization continuous production, used the tubular reactor who is equipped with strong acid solid catalyst, saved the step of adding strong acid solution, eliminated the hazards of production technology, reduced pollutant discharge in the production process to the effectual manufacturing cost that has reduced, the device operation is stable, and product nature is excellent, can be suitable for the production process of organic chemical industry ethers compound.
Description
Technical field
The utility model relates to the production technique of organic chemical industry's ether compound, particularly the device of industrialization continuous seepage tetrahydrofurfuryl alcohol ether.
Background technology
Tetrahydrofurfuryl alcohol ether, also known as ethyl tetrahydrofurfuryl ether, ethyl tetrahydrochysene furfuryl ether, 2-(ethoxymethyl) tetrahydrofuran (THF) etc., molecular formula is C
7h
14o
2.In existing ethyl tetrahydrochysene furfuryl ether synthesis technique, be raw material mainly with tetrahydrofurfuryl alcohol, halohydrocarbon, use sodium alkoxide, alkali or basic salt to carry out reaction and prepare ethyl tetrahydrochysene furfuryl ether.Because sodium Metal 99.5 reagent cost is high, alkali or basic salt have certain corrodibility, there is certain risk in production operation, and if in reaction process unreacted completely alkali do not carry out further processing treatment and can cause certain pollution to environment.Further, synthetic method disclosed in prior art mostly is laboratory synthetic method, does not generally relate to the treatment process of centre or process product, and after being applied to scale operation productive rate and product purity lower, not there is the basis of suitability for industrialized production.
Utility model content
The purpose of this utility model is the defect overcoming prior art, provides a kind of device of industrialization continuous seepage tetrahydrofurfuryl alcohol ether.
Described device comprises raw material savings-transmission measurement system, tubular reactor system, dehydration drying system, distillation system and the products pot that order is successively connected.
Described raw material savings-transmission measurement system is saved-is measured supply unit and ethanol by tetrahydrofurfuryl alcohol arranged side by side and saves-measure supply unit and form.Wherein, tetrahydrofurfuryl alcohol is saved-is measured supply unit and is made up of the tetrahydrofurfuryl alcohol storage tank be connected successively and tetrahydrofurfuryl alcohol metering conveying pump, and ethanol is saved-measured supply unit and is made up of the ethanol storage tank be connected successively and ethanol metering conveying pump; Described tetrahydrofurfuryl alcohol metering conveying pump is connected with tubular reactor respectively with ethanol metering conveying pump.
Described tubular reactor system comprises the tubular reactor of filling solid acid catalyst.Described tubular reactor is preferably made up of the refrigerant tubular reactor be sequentially connected and heating agent tubular reactor.Described solid acid catalyst is preferably filled in refrigerant tubular reactor, without filling in heating agent tubular reactor.Described tubular reactor system can also comprise the product tundish between described tubular reactor and dehydration drying system.
Described dehydration drying system comprises tetrahydrofurfuryl alcohol ether dehydration pump, water trap, the moisture eliminator that order is successively connected; The thick tetrahydrofurfuryl alcohol ether storage tank be connected with described moisture eliminator can also be comprised.
Described distillation system comprises rectifying tower fresh feed pump, tower reactor well heater, the rectifying tower that order is successively connected.The top of described rectifying tower can also be provided with overhead condenser, return tank of top of the tower and rectifier column reflux pump, to realize reflowing result.
Described device can adopt following consecutive steps to carry out the production of tetrahydrofurfuryl alcohol ether:
(1) by the mixture that tetrahydrofurfuryl alcohol and ethanol form with mol ratio 1:1 ~ 3, input is filled in the tubular reactor of solid acid catalyst, fully after reaction, and output-response thing;
(2) described reactant is passed into dehydration drying system, dehydrates, obtain water content be 0.05 ~ 0.08% dehydrate product;
(3) the described product that dehydrates is passed into distillation system, carry out rectifying, collect the cut of 135 ~ 165 DEG C, obtain end product.
The method that the utility model provides avoids the raw material that corrodibility, contaminative and the danger such as halohydrocarbon, alkali or the basic salt adopted in use prior art are stronger, with tetrahydrofurfuryl alcohol and ethanol for reaction raw materials, solid acid catalyst is adopted to produce tetrahydrofurfuryl alcohol ether, whole reaction process safety, efficient, environmental protection.
The solid acid catalyst that the utility model uses is preferably H-ZSM-5, SiO
2-Al
2o
3or B
2o
3-Al
2o
3.Solid catalyst acid capacity>=3.2mmol/mg selected by the utility model, granularity is 16-50 order, and tap density is 0.55-0.65g/ml, specific surface area>=20m
2/ g, aperture>=15nm, pore volume>=0.2cc, intensity>=95%, maximum operation (service) temperature≤180 DEG C.
In actual production, the process air speed of described solid acid catalyst is 2 ~ 4h
-1.Air speed described in the utility model refers to the gas volume of unit time per volume of catalyst process.The unit of described air speed is m
3/ (m
3h), the utility model is reduced to h
-1.
In tubular reactor, the main reaction occurred is:
C
5H
10O
2+C
2H
6O→C
7H
14O
2+H
2O
The principal reaction mechanism of above-mentioned reaction is: alcohol is under the katalysis at solid acid catalyst, and dehydration reaction generates ether.
The utility model is found by a large amount of Industrialized Production Practice, and described reaction is first carried out low-temp reaction and carried out the generation that pyroreaction can improve reaction efficiency, minimizing side reaction product again.
In actual production process, the temperature in refrigerant tubular reactor is-20 ~ 10 DEG C, is preferably-15 ~ 0 DEG C, more preferably-12 ~-8 DEG C.The utility model is by a large amount of practice, in conjunction with the catalysis feature of solid acid catalyst, carry out preferably to the temperature in refrigerant reactor, under above-mentioned temperature of reaction, the gasification of feed ethanol can be reduced, make reactant concn maintain a higher level, react fully and carry out, prevent the azeotrope of second alcohol and water from producing, make reaction system more stable, and the generation of by product ether can be reduced.
Reaction pressure in refrigerant tubular reactor is 0.01 ~ 0.5MPa, is preferably 0.1 ~ 0.2MPa.
The flow velocity that material enters refrigerant tubular reactor is 20 ~ 45kg/h, is preferably 20 ~ 25kg/h.
In actual production process, the temperature in described heating agent tubular reactor is 15 ~ 80 DEG C, is preferably 50 ~ 80 DEG C, more preferably 70 ~ 75 DEG C.The utility model is carrying out on preferred basis to the temperature in refrigerant reactor, further the temperature in refrigerant reactor is adjusted accordingly, after material carries out low-temp reaction in refrigerant tubular reactor, pyroreaction is carried out again under above-mentioned temperature of reaction, can transformation efficiency be increased substantially, and reduce costs.
Reaction pressure in heating agent tubular reactor is 0.01 ~ 0.5MPa, is preferably 0.1 ~ 0.2MPa.
The flow velocity that material enters heating agent tubular reactor is 15 ~ 30kg/h, is preferably 15 ~ 25kg/h.
In order to realize the best catalytic efficiency of catalyzer, described solid acid catalyst is preferably only filled in described refrigerant tubular reactor.And solid acid catalyst is applied in low-temp reaction environment, the work-ing life of catalyzer can be increased.
Dehydrate described in the utility model step (2) and preferably carry out in the dehydration drying system be made up of dehydration pump, water trap and moisture eliminator.Described dehydration drying system internal pressure is preferably 0.2 ~ 2MPa.Material preferably enters this system with flow velocity 20 ~ 200kg/h.
Step (3) described distillation system preferably carries out in the distillation system comprising rectifying tower.Distillation system internal pressure is preferably 0.2 ~ 2MPa.Material preferably enters this system with flow velocity 20 ~ 200kg/h.In actual rectifying, should first control at 140 ~ 175 DEG C by rectifying bottom temperature, rectifying tower top temperature controls, at 135 ~ 165 DEG C, inlet amount to be controlled at 20 ~ 200kg/h, when rectifying tower top temperature-stable is at 135 ~ 165 DEG C, carry out extraction, this section of component is product tetrahydrofurfuryl alcohol ether.
The device that the utility model is supplied to can be applicable to industrialization continuous seepage ether compound.
The device environmental protection that the utility model provides, safety, can be applied to industrialization continuous seepage.The utility model is added up by serialization suitability for industrialized production, and the object product comprehensive yield obtained is 86 ~ 91%, and gained object product purity can reach 98.5 ~ 99.2%, the yield that can reach higher than existing method tetrahydrobiopterin synthesis furfuryl alcohol ether far away and purity.
Accompanying drawing explanation
Fig. 1 is the schematic diagram of device described in embodiment 1; Wherein, 0, tetrahydrofurfuryl alcohol storage tank, 1, ethanol storage tank, 2, tetrahydrofurfuryl alcohol metering conveying pump, 3, ethanol metering conveying pump, 4, refrigerant tubular reactor, 5, heating agent tubular reactor, 6, product tundish, 7, tetrahydrofurfuryl alcohol ether dehydration pump, 8, water trap, 9, moisture eliminator, 10, thick tetrahydrofurfuryl alcohol ether storage tank, 11, rectifying tower fresh feed pump, 12, tower reactor well heater, 13, rectifying tower, 14, overhead condenser, 15, return tank of top of the tower, 16, rectifier column reflux pump, 17, products pot.
Fig. 2 is end product described in embodiment 3
1h-NMR resonance peak ownership figure.
Fig. 3 is the infrared spectrum of end product described in embodiment 3.
Embodiment
Following examples for illustration of the utility model, but are not used for limiting scope of the present utility model.
Embodiment 1
Present embodiments provide a kind of device (as shown in Figure 1) of industrialization continuous seepage tetrahydrofurfuryl alcohol ether, described device comprises raw material savings-transmission measurement system sequentially connected successively, refrigerant tubular reactor 4, heating agent tubular reactor 5, product tundish 6, tetrahydrofurfuryl alcohol ether dehydration pump 7, water trap 8, moisture eliminator 9, thick tetrahydrofurfuryl alcohol ether storage tank 10, rectifying tower fresh feed pump 11, tower reactor well heater 12, rectifying tower 13 and products pot 17;
Described raw material savings-transmission measurement system is made up of tetrahydrofurfuryl alcohol savings-transmission measurement system arranged side by side and ethanol savings-transmission measurement system;
Wherein, tetrahydrofurfuryl alcohol savings-transmission measurement system is made up of the tetrahydrofurfuryl alcohol storage tank 0 be connected successively and tetrahydrofurfuryl alcohol metering conveying pump 2, and ethanol savings-transmission measurement system is made up of the ethanol storage tank 1 be connected successively and ethanol metering conveying pump 3; Described tetrahydrofurfuryl alcohol metering conveying pump 2 is connected with refrigerant tubular reactor 4 respectively with ethanol metering conveying pump 3;
The top of described rectifying tower 13 is also provided with overhead condenser 14, return tank of top of the tower 15 and rectifier column reflux pump 16.
Embodiment 2
Present embodiments provide the concrete operation step of device described in embodiment 1, comprising: outsourcing tetrahydrofurfuryl alcohol and ethanol are added storage tank 0,1 respectively, the heating agent of the refrigerant import and export and heating agent tubular reactor 5 of opening refrigerant tubular reactor 4 is imported and exported; Respectively pre-cold-peace preheating is carried out to refrigerant tubular reactor 4 and heating agent tubular reactor 5, respectively temperature of reaction is controlled at-20 ~ 10 DEG C and 15 ~ 80 DEG C in reaction process; Start tetrahydrofurfuryl alcohol charging pump 2 and ethanol charging pump 3 respectively, by tetrahydrofurfuryl alcohol and ethanol continus convergence, and regulate tetrahydrofurfuryl alcohol and ethanol charging pump flow, the add-on of tetrahydrofurfuryl alcohol and ethanol is exported according to the ratio of mol ratio 1:1 ~ 3; Open the import of tetrahydrofurfuryl alcohol ether tundish 6, collect reaction solution, when tank level reaches 60 ~ 80%, open water trap 8 and moisture eliminator 9 terminal valve and thick tetrahydrofurfuryl alcohol ether storage tank 10 valve; Open reaction solution dehydration pump 7, regulate rate of discharge, flow control, at 20 ~ 200kg/h, makes reaction solution be dewatered by water trap 8 and moisture eliminator 9 successively, the thick tetrahydrofurfuryl alcohol ether of the product introduction after dehydration storage tank 10; When thick tetrahydrofurfuryl alcohol ether storage tank 10 liquid level reaches 60 ~ 80%, come into operation tower bottom of rectifying tower 12 well heater and overhead condenser 14, controlled by bottom temperature at 140 ~ 175 DEG C in rectifying, and tower top temperature controls at 135 ~ 165 DEG C; Start rectifying tower fresh feed pump 11, and inlet amount is controlled at 20 ~ 200kg/h; When tower top temperature is stabilized in 135 ~ 165 DEG C, carry out extraction, this section of component is product tetrahydrofurfuryl alcohol ether, opens tetrahydrofurfuryl alcohol ether products pot, extraction product is carried out collection and stores.
Embodiment 3
Adopt embodiment 1 generator, produce tetrahydrofurfuryl alcohol ether according to following steps:
(1) by the mixture that 1000kg tetrahydrofurfuryl alcohol and 1100kg ethanol form, input the refrigerant tubular reactor of filling solid catalyst H-ZSM-5 with flow velocity 20kg/h, the process air speed of described solid catalyst is 2h
-1,-10 DEG C, under the condition of 0.1Mpa fully after reaction, then input packless heating agent tubular reactor with flow velocity 15kg/h, 72 DEG C, under the condition of 0.1Mpa fully after reaction, output-response thing;
(2) described reactant is inputted dehydration drying system with flow velocity 20kg/h, successively through dehydration pump dehydration, after drying bed drying, obtain water content be 0.05% dehydrate product;
(3) the described product that dehydrates is inputted distillation system with flow velocity 20kg/h, collect the cut of 135 ~ 165 DEG C, obtain 934.5kg end product.
The present embodiment detects gained end product further.Described detection is specially:
(1) adopt SPEC-PMR-CHM500MHz nuclear magnetic resonance spectrometer to measure end product, solvent is deuterochloroform; Its tetrahydrofurfuryl alcohol ether
1as shown in Figure 2, result is as shown in table 1 for H-NMR resonance peak ownership figure.
Table 1: end product
1h-NMR detected result
| Numbering | Proton quantity | Chemical shift δ (ppm) |
| a | 3 | 1.1～1.3 |
| b | 2 | 3.5～3.6 |
| c | 1 | 3.4～3.5 |
| d | 1 | 3.7～3.8 |
| e | 1 | 1.5～1.7 |
| f | 1 | 1.9～2.0 |
| g | 1 | 1.8～1.9 |
| h | 1 | 1.9 |
| i | 1 | 3.8～3.9 |
| j | 1 | 3.9～4.0 |
| k | 1 | 4.0～4.1 |
(2) structure of FTIR-7600 type Fourier transform infrared chromatographic instrument to end product is adopted to analyze; The infrared spectrum of end product as shown in Figure 3, so its molecular structure is:
From the detected result of above-mentioned (1) and (2), end product is tetrahydrofurfuryl alcohol ether.
(3) benevolence China GC-9890A type gas chromatograph is adopted to analyze the composition of end product and purity; Design parameter comprises: chromatographic column: 20mm*0.25mm, PEG-20M capillary column; Column temperature: 45 DEG C/4 points to 100 DEG C/8 points; Temperature rise rate: 20 DEG C/minute; Temperature of vaporization chamber: 265 DEG C; Splitting ratio: 5:1.
Analytical results is: in end product, tetrahydrofurfuryl alcohol ether purity is 98.8%; In tetrahydrofurfuryl alcohol tetrahydrofurfuryl alcohol ether yield for 86.4%.
Embodiment 4
Adopt embodiment 1 generator, produce tetrahydrofurfuryl alcohol ether according to following steps:
(1) by the mixture that 1200kg tetrahydrofurfuryl alcohol and 1500kg ethanol form, input with flow velocity 25kg/h and fill solid catalyst SiO
2-Al
2o
3refrigerant tubular reactor, the process air speed of described solid catalyst is 4h
-1,-8 DEG C, under the condition of 0.2Mpa fully after reaction, then input packless heating agent tubular reactor with flow velocity 25kg/h, 70 DEG C, under the condition of 0.2Mpa fully after reaction, output-response thing;
(2) described reactant is inputted dehydration drying system with flow velocity 200kg/h, successively through dehydration pump dehydration, after drying bed drying, obtain water content be 0.08% dehydrate product;
(3) the described product that dehydrates is inputted distillation system with flow velocity 200kg/h, collect the cut of 135 ~ 165 DEG C, obtain 1056kg end product.
Detection method described in embodiment 1 is adopted to detect end product.From detected result, end product is tetrahydrofurfuryl alcohol ether, and purity is 99%, in tetrahydrofurfuryl alcohol tetrahydrofurfuryl alcohol ether yield for 88%.
Embodiment 5
Adopt embodiment 1 generator, produce tetrahydrofurfuryl alcohol ether according to following steps:
(1) by the mixture that 1200kg tetrahydrofurfuryl alcohol and 1620kg ethanol form, input with flow velocity 23kg/h and fill solid catalyst B
2o
3-Al
2o
3refrigerant tubular reactor, the process air speed of described solid catalyst is 3h
-1,-12 DEG C, under the condition of 0.15Mpa fully after reaction, then input packless heating agent tubular reactor with flow velocity 20kg/h, 75 DEG C, under the condition of 0.15Mpa fully after reaction, output-response thing;
(2) described reactant is inputted dehydration drying system with flow velocity 100kg/h, successively through dehydration pump dehydration, after drying bed drying, obtain water content be 0.06% dehydrate product;
(3) the described product that dehydrates is inputted distillation system with flow velocity 100kg/h, collect the cut of 135 ~ 165 DEG C, obtain 1064kg end product.
Detection method described in embodiment 1 is adopted to detect end product.From detected result, end product is tetrahydrofurfuryl alcohol ether, and purity is 99.2%, in tetrahydrofurfuryl alcohol tetrahydrofurfuryl alcohol ether yield for 91%.
Under reaction conditions described in the present embodiment, replace described solid acid catalyst with the vitriol oil; After testing, product purity is 92%, and yield is 83.5%.
Although above with general explanation, embodiment and test, done detailed description to the utility model, on the utility model basis, can make some modifications or improvements it, this will be apparent to those skilled in the art.Therefore, these modifications or improvements on the basis of not departing from the utility model spirit, all belong to the scope that the utility model is claimed.
Claims (10)
1. a device for industrialization continuous seepage tetrahydrofurfuryl alcohol ether, is characterized in that, comprises raw material savings-transmission measurement system, tubular reactor system, dehydration drying system, distillation system and products pot that order is successively connected;
Described raw material savings-transmission measurement system is saved-is measured supply unit and ethanol by tetrahydrofurfuryl alcohol arranged side by side and saves-measure supply unit and form;
Described tubular reactor system comprises the tubular reactor of filling solid acid catalyst.
2. device according to claim 1, is characterized in that, described tetrahydrofurfuryl alcohol is saved-measured supply unit and is made up of the tetrahydrofurfuryl alcohol storage tank be connected successively and tetrahydrofurfuryl alcohol metering conveying pump;
Send ethanol to save-measure supply unit to be made up of the ethanol storage tank be connected successively and ethanol metering conveying pump;
Described tetrahydrofurfuryl alcohol metering conveying pump is connected with tubular reactor respectively with ethanol metering conveying pump.
3. device according to claim 1 and 2, is characterized in that, described tubular reactor is made up of the refrigerant tubular reactor be sequentially connected and heating agent tubular reactor.
4. device according to claim 3, is characterized in that, described solid acid catalyst is only filled in refrigerant tubular reactor.
5. device according to claim 1, is characterized in that, described tubular reactor system also comprises product tundish; Described product tundish are connected with dehydration drying system with tubular reactor respectively.
6. device according to claim 1 or 5, is characterized in that, described dehydration drying system comprises tetrahydrofurfuryl alcohol ether dehydration pump, water trap, the moisture eliminator that order is successively connected.
7. device according to claim 6, is characterized in that, described dehydration drying system also comprises thick tetrahydrofurfuryl alcohol ether storage tank; Described thick tetrahydrofurfuryl alcohol ether storage tank is connected with distillation system with moisture eliminator respectively.
8. the device according to claim 1 or 7, is characterized in that, described distillation system comprises rectifying tower fresh feed pump, tower reactor well heater, the rectifying tower that order is successively connected.
9. device according to claim 8, is characterized in that, the top of described rectifying tower is provided with overhead condenser, return tank of top of the tower and rectifier column reflux pump.
10. device according to claim 1, it is characterized in that, comprise raw material savings-transmission measurement system sequentially connected successively, refrigerant tubular reactor, heating agent tubular reactor, product tundish, tetrahydrofurfuryl alcohol ether dehydration pump, water trap, moisture eliminator, thick tetrahydrofurfuryl alcohol ether storage tank, rectifying tower fresh feed pump, tower reactor well heater, rectifying tower and products pot;
Described tetrahydrofurfuryl alcohol savings-transmission measurement system is made up of the tetrahydrofurfuryl alcohol storage tank be connected successively and tetrahydrofurfuryl alcohol metering conveying pump, and ethanol savings-transmission measurement system is made up of the ethanol storage tank be connected successively and ethanol metering conveying pump; Described tetrahydrofurfuryl alcohol metering conveying pump is connected with refrigerant tubular reactor respectively with ethanol metering conveying pump;
The top of described rectifying tower is also provided with overhead condenser, return tank of top of the tower and rectifier column reflux pump.
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|---|---|---|---|
| CN201520759223.6U CN205170714U (en) | 2015-09-28 | 2015-09-28 | Device of industrialization continuous production tetrahydrofurfuryl alcohol ether |
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|---|---|---|---|
| CN201520759223.6U CN205170714U (en) | 2015-09-28 | 2015-09-28 | Device of industrialization continuous production tetrahydrofurfuryl alcohol ether |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105348228A (en) * | 2015-09-28 | 2016-02-24 | 李沛轩 | Industrial continuous production method and apparatus for tetrahydrofurfuryl alcohol diethyl ether |
-
2015
- 2015-09-28 CN CN201520759223.6U patent/CN205170714U/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105348228A (en) * | 2015-09-28 | 2016-02-24 | 李沛轩 | Industrial continuous production method and apparatus for tetrahydrofurfuryl alcohol diethyl ether |
| CN105348228B (en) * | 2015-09-28 | 2024-04-16 | 尤学民 | Method and device for industrially and continuously producing tetrahydrofurfuryl alcohol diethyl ether |
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|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C41 | Transfer of patent application or patent right or utility model | ||
| CB03 | Change of inventor or designer information |
Inventor after: You Xuemin Inventor after: Zhao Yu Inventor before: Li Peixuan Inventor before: Lu Yian Inventor before: Liu Baixi |
|
| COR | Change of bibliographic data | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20160922 Address after: 833699 No. 8, Taoyuan 4, Dushanzi District, the Xinjiang Uygur Autonomous Region, Karamay Patentee after: You Xuemin Patentee after: Zhao Yu Address before: 211899, No. 30 Zhujiang South Road, Jiangpu street, Pukou District, Jiangsu, Nanjing Patentee before: Li Peixuan Patentee before: Lu Yian Patentee before: Liu Baixi |
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| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20160420 Termination date: 20210928 |