CN201880521U - Device for continuously preparing medium-high carbon fatty acid ester - Google Patents
Device for continuously preparing medium-high carbon fatty acid ester Download PDFInfo
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- CN201880521U CN201880521U CN2010205613428U CN201020561342U CN201880521U CN 201880521 U CN201880521 U CN 201880521U CN 2010205613428 U CN2010205613428 U CN 2010205613428U CN 201020561342 U CN201020561342 U CN 201020561342U CN 201880521 U CN201880521 U CN 201880521U
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Abstract
The utility model discloses a device for continuously preparing medium-high carbon fatty acid ester, which comprises a gas-film type reaction device, wherein the gas-film type reaction device is a tower type reactor. The tower type reactor comprises a tower main body, an ester discharging opening, an alcohol-steam inlet, a liquid-material inlet and a steam outlet, wherein the tower main body is in the shape of a cylindrical shell, and the ester discharging opening, the alcohol-steam inlet, the liquid-material inlet and the steam outlet are respectively arranged on the tower main body from bottom to top. The ester discharging opening is positioned at the bottom of the tower main body, the alcohol-steam inlet is positioned at the lower part of the lateral part of the tower main body, the liquid-material inlet is positioned at the upper part of the lateral part of the tower main body, the steam outlet is positioned at the top of the tower main body, and the bottom of the tower main body is a liquid storing part. The tower type reactor also comprises five to twenty-one layers of grids which are fixed in the tower main body and sequentially arranged according to a sequence from top to bottom; and the grids are arranged between the alcohol-steam inlet and the liquid-material inlet. The time for preparing the medium-high carbon fatty acid ester by adopting the device disclosed by the utility model is short, the conversion rate is high, and the energy consumption is low.
Description
Technical field
The utility model relates to a kind of device for preparing the medium high carbon fatty acid ester.
Background technology
The alleged medium high carbon fatty acid ester of the utility model is meant that the carbon number on the carbochain is 6 to 18 a fatty acid ester, and the medium high carbon fatty acid ester generally can and make by medium high carbon aliphatic acid and alcohol generation esterification.At present, the typical method of the esterification of medium high carbon aliphatic acid is the preparation method of discontinuous, and the used equipment of this method is seen Fig. 1.Reactor a among Fig. 1 has agitator b, and reflux condenser c is equipped with on the top of this reactor a.During preparation medium high carbon fatty acid ester, medium high carbon aliphatic acid and alcohol are accurately dropped among the reactor a after the proportioning, in the chuck d of reactor a, feed steam and make the material system reflux at a certain temperature and generate the reaction of medium high carbon fatty acid ester, must stir on backflow limit, limit in the course of reaction, make a large amount of excessive alcohol constantly be back among the reactor a by reflux condenser c.The shortcoming of this method is: (1) is owing to the boiling point lower (methyl alcohol is 64.5 ℃, and ethanol is 78.4 ℃) of alcohol, so the back flow reaction temperature is lower, causes the reaction time longer, generally needs 6h～8h just can react completely.(2) reaction conversion ratio is not high, between 90%～95%.(3) need guarantee that with a large amount of alcohol esterification is complete, and a large amount of alcohol that refluxes constantly flows into the temperature that can reduce among the reactor a among the reactor a, thereby constantly heating keeps reaction temperature, energy consumption is higher.(4) shipwreck that generates in the course of reaction is to remove.
Summary of the invention
The purpose of this utility model is to overcome the problems referred to above, and the device that provides a kind of continous way to prepare the medium high carbon fatty acid ester is short with this device preparation medium high carbon fatty acid ester time, conversion ratio is high, energy consumption is low.
A kind of technical scheme that realizes the utility model purpose is: a kind of continous way prepares the device of medium high carbon fatty acid ester, comprises the air film type reaction unit; The air film type reaction unit is a tower reactor; This tower reactor comprises the tower main body of cylinder shelly and is separately positioned on the ester floss hole on the tower main body, pure steam inlet, liquid material inlet and steam (vapor) outlet from bottom to top; The ester floss hole is positioned at the bottom of tower main body, and pure steam inlet is positioned at tower main body side subordinate side, and liquid material inlet is positioned at tower main body sidepiece top, and steam (vapor) outlet is positioned at the top of tower main body; The bottom of tower main body is a liquid storage portion; Tower reactor also comprises 5 to 21 layers of grid that are fixed in the tower main body and set gradually according to order up and down; Described grid is arranged between pure steam inlet and the liquid material inlet; Intensive filler or the pellet type catalyst banked up on each layer grid, the filler of banking up on grid then forms packing layer, and the catalyst of banking up on grid then forms catalyst layer, and packing layer and catalyst layer are according to the interlace mode setting; Described pellet type catalyst is the graininess acidic catalyst; Tower reactor also comprises the dish type atomizing distributor that is fixed in the tower main body and is positioned at tower main body top; The airtight connection that enters the mouth of the charging aperture of dish type atomizing distributor and the liquid material of tower reactor, dish type atomizing distributor is for having the coil pipe of conventional quantity and big or small atomizing spray orifice on tube wall.
Filler is the ceramic Pall ring or the cylindrical shape net of being reeled and to be formed by stainless steel cloth.
Described graininess acidic catalyst is that particle diameter is the solid acid catalyst of 3～10mm.
Described solid acid catalyst is SO
4 2-/ M
xO
yThe solid super acid catalyst of type; Described SO
4 2-/ M
xO
yThe solid super acid catalyst of type is SO
4 2-/ ZrO
2, SO
4 2-/ Fe
2O
3, SO
4 2-/ Al
2O
3, SO
4 2-/ ZrO
2-Al
2O
3, or SO
4 2-/ TiO
2-SnO
2-Al
2O
3
The height of described cylindric tower reactor is 15～30m, and diameter is 0.5～3m; Described liquid material inlet to the distance at the tower main body top of cylindric tower reactor is 0.5～1.5m; Described pure steam inlet to the distance of the tower bottom part body of cylindric tower reactor is 5～10m; Basecoat in the described grid is positioned at described pure steam inlet top 0.5～1m; The nozzle diameter of described steam (vapor) outlet is 0.1～0.5m; The loading height of described catalyst layer is 5～20cm; The loading height of packing layer is 1～5m; Distance between the upper end of the material on the lower end of last layer grid and the following one deck grid is 20～35cm.
Total number of plies of described grid is an odd number, and odd number layer wherein is packing layer, and the even numbers layer is catalyst layer.
The another kind of technical scheme that realizes the utility model purpose is: a kind of continous way prepares the device of medium high carbon fatty acid ester, comprises the air film type reaction unit; The air film type reaction unit is a tower reactor; This tower reactor comprises the tower main body of cylinder shelly and is separately positioned on the ester floss hole on the tower main body, pure inlet, aliphatic acid inlet and steam (vapor) outlet from bottom to top; The ester floss hole is positioned at the bottom of tower main body, and the alcohol inlet is positioned at tower main body side subordinate side, and the aliphatic acid inlet is positioned at tower main body sidepiece top, and steam (vapor) outlet is positioned at the top of tower main body; The bottom of tower main body is a liquid storage portion; Tower reactor also comprises the grid that is fixed in the tower main body; Described grid is arranged between alcohol inlet and the aliphatic acid inlet; Grid is provided with the formed packing layer of the intensive filler of banking up; Tower reactor also comprises dish type atomizing distributor and the spiral heater that is fixed in the tower main body; Spiral heater is positioned at the alcohol inlet below of tower main body; Dish type atomizing distributor is for having the coil pipe of the conventional quantity and the atomizing spray orifice of size on tube wall; Dish type atomizing distributor is positioned at the top of tower main body, and its charging aperture enters the mouth airtight linking to each other with the aliphatic acid of tower reactor.
Filler is the ceramic Pall ring or the cylindrical shape net of being reeled and to be formed by stainless steel cloth.
Grid has 3 to 10 layers, is equipped with the formed packing layer of the intensive filler of banking up on every layer of grid.
The height of described cylindric tower reactor is 15～30m, and diameter is 0.5～3m; Described aliphatic acid inlet to the distance at the tower main body top of cylindric tower reactor is 0.5～1.5m; Described alcohol inlet to the distance of the tower bottom part body of cylindric tower reactor is 5～10m; Basecoat in the described grid is positioned at described alcohol inlet top 0.5～1m; The nozzle diameter of described steam (vapor) outlet is 0.1～0.5m; The loading height of described packing layer is 1～5m; Distance between the upper end of the material on the lower end of last layer grid and the following one deck grid is 20～35cm.
The utlity model has positive effect: (1) a kind of device of the present utility model can be gas with methyl alcohol or ethanol evaporation and mainly carry out esterification at catalyst surface and filling surface with the aliphatic acid of liquid state under the catalytic action of solid acid in convection current, increased the contact area between the reactant so on the one hand greatly, on the other hand owing to thereby higher feasible being reflected under the higher temperature of temperature of pure steam carried out, can provide reaction needed heat fast, not only can be the fast a large amount of needed heats of postreaction, and accelerated reaction speed greatly, thereby shortened the reaction time, 6 to 8 hours original reaction time of esterification has been shortened within 10 fens kinds.This device makes the moisture that produces in the course of reaction not rest on filler or catalyst surface along with pure steam outflow reactor at any time, the fatty acid ester that reaction is produced then falls to the tower main body under the gravity effect bottom does not rest on filler or catalyst surface yet, thereby improved conversion ratio greatly, conversion ratio can reach more than 98%.(2) another kind of device of the present utility model can the base metal catalysts in being dissolved in liquid alcohol join excessive liquid methanol or ethanol in the air film type reaction unit, liquid alcohol is vaporizated into pure steam and mainly carries out the catalyzed alcoholysis reaction at filling surface with liquid fat in convection current, increased the contact area between the reactant so on the one hand greatly, on the other hand owing to thereby higher feasible being reflected under the higher temperature of temperature of pure steam carried out, not only can be the fast a large amount of needed heats of postreaction, and accelerated reaction speed greatly, thereby shortened the reaction time, 6 to the 8 hours original alcoholysis reaction time has been shortened within 10 fens kinds.This device makes the fatty acid ester and the glycerine that produce in the course of reaction then fall to the bottom of tower main body under the gravity effect and not rest on filler or catalyst surface, thereby has improved conversion ratio greatly, and conversion ratio can reach more than 98%.(3) adopt plant energy consumption of the present utility model low, have only 1/10～1/20 of traditional handicraft.(4) device of the present utility model can be realized the production of serialization, and output can reach tens of times even hundreds of times of traditional handicraft, is applicable to large-scale production.(5) adopt the purity of the fatty acid ester of device preparation of the present utility model to reach more than 99.5%.
Description of drawings
Fig. 1 prepares the device that fatty acid ester adopts for traditional handicraft.
Fig. 2 is the device that embodiment 1 adopts.
Fig. 3 prepares the schematic diagram of medium high carbon fatty acid ester for the device of Fig. 2.
Fig. 4 is the device that embodiment 2 adopts.
Fig. 5 prepares the schematic diagram of medium high carbon fatty acid ester for the device of Fig. 4.
Label in the above-mentioned accompanying drawing is as follows:
Reactor a, agitator b, reflux condenser c, chuck d,
Tower reactor 1(air film type reaction unit), tower main body 10, ester floss hole 11, pure steam inlet 12, alcohol inlet 12 ' liquid material inlet 13, aliphatic acid inlet 13 ', steam (vapor) outlet 14, liquid storage portion 15, grid 16, dish type atomizing distributor 17, spiral heater 18
Liquid alcohol storage tank 31, the first measuring pumps 33, vaporizer 34,
Heat insulated tank 41, the second measuring pumps 42, heat exchanger 43,
Mixed vapour treatment system 6, pure steam treatment system 6 ' second heat exchanger, 61, the first reservoirs, 62, the three measuring pumps 63, vertical pipe type destilling tower 64, the three heat exchangers 65, molecular sieve adsorption jar 66, the second product pumps 67, liquid alcohol buffering recycling can 68.
The specific embodiment
(embodiment 1)
See Fig. 2, the device that the continous way that present embodiment adopts prepares the medium high carbon fatty acid ester comprises air film type reaction unit 1, and this air film type reaction unit 1 is a tower reactor, and it highly is 27m, and diameter is 3m, and its material is the 316L stainless steel.This tower reactor 1 comprises the tower main body 10 of cylinder shelly and is separately positioned on ester floss hole 11 on the tower main body 10, pure steam inlet 12, liquid material inlet 13 and steam (vapor) outlet 14 from bottom to top.Be respectively equipped with by-pass valve control on ester floss hole 11, pure steam inlet 12, liquid material inlet 13 and the steam (vapor) outlet 14.
Filler in the packing layer 21 is the ceramic Pall ring or the cylindrical shape net of being reeled and to be formed by stainless steel cloth.The material of described stainless steel cloth is the 316L stainless steel.
Pellet type catalyst in the catalyst layer 22 is that particle diameter is the solid super acid catalyst of 3～10mm.
Described solid super acid catalyst can be commercially available SO
4 2-/ ZrO
2, SO
4 2-/ Fe
2O
3Perhaps SO
4 2-/ Al
2O
3, or be 02151526.3 according to document number for the CN1425500A(application number) in the granule type solid super catalyst S O of embodiment 1 to embodiment 4 preparation
4 2-/ ZrO
2-Al
2O
3Or granule type solid super catalyst S O
4 2-/ TiO
2-SnO
2-Al
2O
3(φ in the embodiment 1=3 millimeter particulate vector also be the granular pattern carrier is carrier described in its summary of the invention), or the technical grade solid super acidic catalyst sold of Qufu Fu Ruide catalytic applications Science and Technology Ltd..
(application examples 1)
See Fig. 3, the device of employing present embodiment prepares the medium high carbon fatty acid ester also to be needed: liquid alcohol storage tank 31, first measuring pump 33, vaporizer 34, heat insulated tank 41, second measuring pump 42, heat exchanger 43, product pump 51 and mixed vapour treatment system 6.
Vaporizer 34 is steam heating water bath type vaporizers, this vaporizer comprises outer cylinder body and is arranged in the internal duct of outer cylinder body, feed temperature as medium in the outer cylinder body and be 100 ℃ steam, feed methyl alcohol in the internal duct, vaporizer 34 by its liquid-inlet that communicates with internal duct as the liquid material import, by its gas vent that communicates with internal duct as the gaseous state material outlet.
Mixed vapour treatment system 6 comprises second heat exchanger 61, first reservoir 62, the 3rd measuring pump 63, vertical pipe type destilling tower 64, the 3rd heat exchanger 65, molecular sieve adsorption jar 66, second product pump 67 and liquid alcohol buffering recycling can 68.Vertical pipe type destilling tower 64 is provided with the liquid material import that is positioned at the sidepiece below, is positioned at the gaseous state material outlet and the liquid material outlet that is positioned at the bottom of cat head.Molecular sieve adsorption jar 66 is provided with the material inlet that is positioned at the top and is positioned at the material outlet of bottom, and the intensive particulate molecular sieve adsorbent that is stacked with in the tank body.
The material outlet of second heat exchanger 61 links to each other by the material inlet of exterior line with first reservoir 62, the material outlet of first reservoir 62 links to each other with the material inlet of the 3rd measuring pump 63 is airtight by exterior line, the material outlet of the 3rd measuring pump 63 is by liquid material import airtight link to each other of exterior line with vertical pipe type destilling tower 64, the gaseous state material outlet of vertical pipe type destilling tower 64 links to each other with the material inlet of the 3rd heat exchanger 65 is airtight by exterior line, the material outlet of the 3rd heat exchanger 65 links to each other with the material inlet of molecular sieve adsorption jar 66 is airtight by exterior line, the material outlet of molecular sieve adsorption jar 66 links to each other with the material inlet of second product pump 67 is airtight by exterior line, and the material outlet of second product pump 67 is by material inlet airtight link to each other of exterior line with liquid alcohol buffering recycling can 68.
Liquid alcohol storage tank 31 links to each other with the material inlet of first measuring pump 33 is airtight by exterior line, and the material inlet of first measuring pump 33 is also by material outlet airtight link to each other of corresponding exterior line with liquid alcohol buffering recycling can 68; The material outlet of first measuring pump 33 is by liquid material import airtight link to each other of exterior line with vaporizer 34, and the gaseous state material outlet of vaporizer 34 is by pure steam inlet 12 airtight link to each other of exterior line with tower reactor 1.
The discharging opening of heat insulated tank 41 links to each other with the material inlet of second measuring pump 42 is airtight by exterior line, the material outlet of second measuring pump 42 links to each other with the material inlet of heat exchanger 43 is airtight by exterior line, and the material outlet of heat exchanger 43 entered the mouth for 13 airtight linking to each other with the liquid material of tower reactor 1 by exterior line.
The steam (vapor) outlet 14 of tower reactor 1 is by second heat exchanger 61 material inlets airtight link to each other of exterior line with mixed vapour treatment system 6.
Still see Fig. 3, concrete preparation method has following steps:
1. continuously the excessive liquid methanol in the liquid alcohol storage tank 31 being pumped in the operating vaporizer 34 (temperature of the steam in the outer cylinder body is 100 ℃) by first measuring pump 33 makes it to be heated and is vaporizated into methanol steam, methanol steam then enters bottom in the tower main body 10 of air film type reaction unit 1 by the pure steam inlet 12 of the gas vent of vaporizer 34, corresponding pipeline and air film type reaction unit 1, enters the pure steam motion from bottom to top in tower main body 10 in the tower main body 10.The used raw material liquid methyl alcohol of present embodiment is the absolute methanol of purity 〉=99.5%.
2. carry out step 1. in, continuously (carbon number of carbochain is 12 to 18 with the medium high carbon aliphatic acid of the liquid state in the heat insulated tank 41, in different embodiment, select laurate respectively, myristic acid, palmitic acid or stearic acid, purity 〉=99.5%) pumps into by second measuring pump 42 and make it to be heated to 120 ℃～150 ℃ in the operating heat exchanger 43, under second measuring pump, 42 pump pressures, liquid medium high carbon aliphatic acid is by the material outlet of heat exchanger 43, the liquid material inlet 13 of corresponding pipeline and air film type reaction unit 1 enters (medium high carbon aliphatic acid is 1: 2.5～1: 3.5 with the mol ratio of alcohol, and present embodiment is 1: 3) in the dish type atomizing distributor 17.
3. under second measuring pump, 42 pump pressures, liquid medium high carbon aliphatic acid then becomes vaporific drop ejection after through dish type atomizing distributor 17 and enters in the upper cavity of tower main body 10, under the gravity effect, fall to earlier on the filler of packing layer 21 of ground floor grid of the top, then carry out downward the flowing of general trend drops down onto on the catalyst of catalyst layer 22 of second layer grid along the surface of each filler again, under the gravity effect, successively move downward again, and in flowing the filling surface of process form uniform liquid film, and be in the liquid film on the filler of each packing layer 21 of catalyst layer 22 belows because be acid liquid film through catalyst layer 22.
4. the methanol steam that 1. enters tower main body 10 by step passes through packing layer 21 and catalyst layer 22(from bottom to top continuously promptly from bottom to top earlier through a packing layer 21 of below, upwards successively pass through corresponding catalyst layer 22 and packing layer 21 more successively), methanol steam is because of becoming acid methanol steam through catalyst layer 22, thereby the catalytic esterification of medium high carbon fatty acid methyl ester and water not only directly takes place to generate in this methanol steam with the medium high carbon aliphatic acid that falls to catalyst surface in the zone of each catalyst layer 22, also in each packing layer 21 with filler on the medium high carbon aliphatic acid of the liquid film state that is in the catalytic esterification (so esterification is called steam film formula esterification or air film type esterification) of medium high carbon fatty acid methyl ester and water takes place to generate.The time that medium high carbon aliphatic acid stops with catalyst surface on filler is can to change by the filling total height of adjusting packing layer 21 and catalyst layer 22 this time of staying of 3～9min(, present embodiment is 5 min), because of complete reaction time of catalytic esterification is about 3min, so the time of staying of present embodiment medium high carbon aliphatic acid in packing layer 21 and catalyst layer 22 is set to 5 min, guarantees carrying out fully of esterification.The required reaction heat of the catalytic esterification of above-mentioned two kinds of forms provides by the heat of being brought into as the medium high carbon aliphatic acid of raw material.
5. the medium high carbon fatty acid methyl ester that is generated by step catalytic esterification 4. is under the effect of gravity, falls to the liquid storage portion 15 of bottom of the tower main body 10 of air film type reaction unit 1, sends into the crude product storage tank through by-pass valve control by product pump 51 again.The water that is generated by step esterification 4. is vaporized into water vapour (mean temperature of whole system is a little less than the temperature of the medium high carbon aliphatic acid that just enters tower main body 10 at this moment) under the effect of the heat of being brought into as the medium high carbon aliphatic acid of raw material, form mixed vapour stream and motion from bottom to top in the tower main body 10 of air film type reaction unit 1 with excessive methanol steam, during through dish type atomizing distributor 17, then pass the space between the adjacent body of its coil pipe, rise to the top then and from the give vent to anger tower main body 10 of film type reaction device 1 of steam (vapor) outlet 14 Continuous Flow.
6. the medium high carbon fatty acid methyl ester crude product that 5. step is obtained is sent into and is carried out decompression distillation in the destilling tower, and the residual voltage in the control destilling tower is that 10～20mm mercury column, temperature are 250 ℃～280 ℃, makes medium high carbon fatty acid methyl ester crude product become finished product by distillation.The mixed vapour stream that step is flowed out continuously at the top of air film type reaction unit 1 in 5. enters in the mixed vapour treatment system 6 by corresponding pipeline.Mixed vapour earlier becomes the mixing material of methyl alcohol and water by chilled water (7 ℃～12 ℃ the water) cooling as cooling medium in second heat exchanger 61 after, flow under the influence of gravity in first reservoir 62, with the 3rd measuring pump 63 mixing material is pumped in the vertical pipe type destilling tower 64 by first reservoir 62 again every a period of time, the heat medium of vertical pipe type destilling tower 64 is a steam, the amount of pumping into by the control mixing material under certain steam flow makes the temperature of the material system in the vertical pipe type destilling tower 64 between 80 ℃～85 ℃, thereby methyl alcohol vaporization in the mixing material is formed to the gaseous state material that the contains little water gaseous state material outlet from the cat head of vertical pipe type destilling tower 64 flows out, after moisture gaseous methanol flow in the 3rd heat exchanger 65, become aqueous liquid methyl alcohol by chilled water as cooling medium, aqueous liquid methyl alcohol flows under the influence of gravity in the molecular sieve adsorption jar 66, the adsorbent of molecular sieve of flowing through becomes liquid methanol outflow molecular sieve adsorption jar 66 after being adsorbed moisture, liquid methanol is pumped in the liquid alcohol buffering recycling can 68 by second product pump 67, pumps in the operating vaporizer 34 through first measuring pump 33 and recycles.
(application examples 2)
Remainder and application examples 1 that should use-case be basic identical, difference is: the alcohol described in should use-case is ethanol rather than methyl alcohol, used raw alcohol is the absolute ethyl alcohol of purity 〉=99.5%, thereby being heated vaporization in vaporizer 34, what obtain then is alcohol vapour, what generate with the medium high carbon fatty acid response in tower reactor 1 then is the medium high carbon fatty-acid ethyl ester, the mixed vapour that flows out continuously at the top of air film type reaction unit 1 is the mixed vapour of second alcohol and water, in the liquid alcohol buffering recycling can 68 the alcohol that is used to recycle be ethanol.Because the boiling point of ethanol is higher than methyl alcohol, so, when pumping in vertical pipe type destilling tower 64 by first reservoir 62 mixing material with the 3rd measuring pump 63, the amount of pumping into of control mixing material and make the temperature of the material system in the vertical pipe type destilling tower 64 between 85 ℃～90 ℃.
(embodiment 2)
See Fig. 4, the device that the continous way that present embodiment adopts prepares the medium high carbon fatty acid ester comprises air film type reaction unit 1, and this air film type reaction unit 1 is a tower reactor, and it highly is 27m, and diameter is 3m, and its material is the 316L stainless steel.This tower reactor 1 comprises the tower main body 10 of cylinder shelly and is separately positioned on the ester floss hole 11 on the tower main body 10, pure inlet 12 ', aliphatic acid inlet 13 ' and steam (vapor) outlet 14 from bottom to top.Be respectively equipped with by-pass valve control on ester floss hole 11, alcohol inlet 12 ', aliphatic acid inlet 13 ' and the steam (vapor) outlet 14.
Filler in the packing layer 21 is the ceramic Pall ring or the cylindrical shape net of being reeled and to be formed by stainless steel cloth.The material of described stainless steel cloth is the 316L stainless steel.
(application examples 3)
See Fig. 5, adopting the device of present embodiment to prepare the medium high carbon fatty acid ester also needs: liquid alcohol storage tank 31, first measuring pump 33, heat insulated tank 41, second measuring pump 42, heat exchanger 43, product pump 51 and pure steam treatment system 6 '.
Alcohol steam treatment system 6 ' comprises second heat exchanger 61 and liquid alcohol buffering recycling can 68.The material outlet of second heat exchanger 61 is by material inlet airtight link to each other of exterior line with liquid alcohol buffering recycling can 68.
Liquid alcohol storage tank 31 links to each other with the material inlet of first measuring pump 33 is airtight by exterior line, and the material outlet of first measuring pump 33 is by alcohol inlet 12 ' airtight link to each other of exterior line with tower reactor 1.
The discharging opening of heat insulated tank 41 links to each other with the material inlet of second measuring pump 42 is airtight by exterior line, and the material inlet of first measuring pump 33 is also by material outlet airtight link to each other of corresponding exterior line with liquid alcohol buffering recycling can 68; The material outlet of second measuring pump 42 links to each other with the material inlet of heat exchanger 43 is airtight by exterior line, and the material outlet of heat exchanger 43 is by aliphatic acid inlet 13 ' airtight link to each other of exterior line with tower reactor 1.
The steam (vapor) outlet 14 of tower reactor 1 is by second heat exchanger 61 material inlets airtight link to each other of exterior line with pure steam treatment system 6 '.
Still see Fig. 5, concrete preparation method has following steps:
1. continuously the excessive liquid methanol that is dissolved with base metal catalysts KOH in the liquid alcohol storage tank 31 is pumped into the bottom in the tower main body 10 of operating air film type reaction unit 1 by first measuring pump 33.The used liquid methanol of present embodiment is KOH to be dissolved in the absolute methanol of purity 〉=99.5% obtain, and wherein, the weight of KOH accounts for 0.3% of KOH and liquid methanol gross weight.
2. carry out step 1. in, (be the medium high carbon fatty glyceride with the liquid fat in the heat insulated tank 41 continuously, wherein the carbon number of the carbochain of medium high carbon fatty acid radical is 6 to 18, in different embodiment, select coconut oil or carbon palm oil respectively, the grease temperature is 80 ℃) be that 1: 6 ratio pumps into by second measuring pump 42 and makes it to be heated to 120 ℃～150 ℃ in the operating heat exchanger 43 with the mol ratio of grease and liquid alcohol, under second measuring pump, 42 pump pressures, liquid fat is by the material outlet of heat exchanger 43, the aliphatic acid inlet 13 ' of corresponding pipeline and air film type reaction unit 1 enters in the dish type atomizing distributor 17.
Described coconut oil is for through refining impurity and the hydrogenation coconut oil after saturated of removing, contained medium high carbon fatty glyceride is 95wt%～98 wt%, in the medium high carbon fatty glyceride, the fatty glyceride of 6～10 carbon accounts for 15wt%, 12, the fatty glyceride of 14 carbon accounts for 70 wt%, and the fatty glyceride of 16,18 carbon accounts for 15wt%.
Described palm oil also is that contained medium high carbon fatty glyceride is 98.5wt%, all is the fatty glyceride of 16,18 carbon through refining impurity and the hydrogenation palm oil after saturated of removing.
3. under second measuring pump, 42 pump pressures, liquid fat then becomes vaporific drop ejection after through dish type atomizing distributor 17 and enters in the upper cavity of tower main body 10, under the gravity effect, fall to earlier on the filler of packing layer 21 of ground floor grid of the top, then carry out downward the flowing of general trend drops down onto on the filler of packing layer 21 of second layer grid along the surface of each filler again, under the gravity effect, successively move downward again, and in flowing the filling surface of process form uniform liquid film.
4. the liquid methanol that 1. enters tower main body 10 by step is vaporizated into methanol steam and passes through packing layer 21 from bottom to top continuously under the effect of the heat that spiral heater 18 is sent, thus this methanol steam in each packing layer 21 with filler on the effect of the grease that is in the liquid film state at KOH under the catalyzed alcoholysis reaction (so alcoholysis reaction is called steam film formula alcoholysis reaction or air film type alcoholysis reaction) of medium high carbon fatty acid methyl ester and glycerine takes place to generate.Grease is can to change by the loading height of adjusting packing layer 21 this time of staying of 3～9min(in the time that the filler upper surface stops, present embodiment is 5 min), the complete reaction time of reacting because of catalyzed alcoholysis is about 3min, so the time of staying of present embodiment medium high carbon fatty glyceride in packing layer 21 is set to 5 min, guarantee carrying out fully of alcoholysis reaction.The required reaction heat of catalyzed alcoholysis reaction is provided by the heat of being brought into as the medium high carbon fatty glyceride of raw material.
5. medium high carbon fatty acid methyl ester that is generated by step catalyzed alcoholysis reaction 4. and glycerine are under the effect of gravity, fall to the liquid storage portion 15 of bottom of the tower main body 10 of air film type reaction unit 1, send in the refining separating still by product pump 51 through by-pass valve control again and leave standstill, sedimentation is separated into two-layer up and down under the gravity effect, glycerine is following, and the medium high carbon fatty acid methyl ester is last.Tell glycerine from the bottom, remaining medium high carbon fatty acid methyl ester is sent into the crude product storage tank.
The reacted excessive methanol steam of catalyzed alcoholysis is motion from bottom to top in the tower main body 10 of air film type reaction unit 1, during through dish type atomizing distributor 17, then pass the space between the adjacent body of its coil pipe, rise to the top then and from the give vent to anger tower main body 10 of film type reaction device 1 of steam (vapor) outlet 14 Continuous Flow.
6. the medium high carbon fatty acid methyl ester that 5. step is obtained is sent into from the crude product storage tank and is carried out decompression distillation the destilling tower, residual voltage in the control destilling tower is that 10～20mm mercury column, temperature are 250 ℃～280 ℃, makes medium high carbon fatty acid methyl ester crude product become finished product by distillation.The methanol steam stream that step is flowed out continuously at the top of air film type reaction unit 1 in 5. enters by corresponding pipeline in the pure steam treatment system 6 '.Methanol steam earlier in second heat exchanger 61 by chilled water (7 ℃～12 ℃ water) cooling becoming liquid methanol as cooling medium, this liquid methanol flows under the influence of gravity into liquid alcohol buffering recycling can 68 and pumps in the operating tower reactor 1 through first measuring pump 33 and recycle.
(application examples 4)
Remainder and application examples 3 that should use-case be basic identical, difference is: the alcohol described in should use-case is ethanol rather than methyl alcohol, used raw alcohol is the absolute ethyl alcohol of purity 〉=99.5%, what generate with grease reaction in tower reactor 1 then is glycerine and medium high carbon fatty-acid ethyl ester, the pure steam that flows out continuously at the top of air film type reaction unit 1 is alcohol vapour, and the alcohol that is used to recycle in the liquid alcohol buffering recycling can 68 is ethanol.
Claims (10)
1. a continous way prepares the device of medium high carbon fatty acid ester, it is characterized in that: comprise air film type reaction unit (1); Air film type reaction unit (1) is a tower reactor; This tower reactor (1) comprises the tower main body (10) of cylinder shelly and is separately positioned on the ester floss hole (11) on the tower main body (10), pure steam inlet (12), liquid material inlet (13) and steam (vapor) outlet (14) from bottom to top; Ester floss hole (11) is positioned at the bottom of tower main body (10), and pure steam inlet (12) are positioned at tower main body (10) sidepiece below, and liquid material inlet (13) is positioned at tower main body (10) sidepiece top, and steam (vapor) outlet (14) is positioned at the top of tower main body (10); The bottom of tower main body (10) is liquid storage portion (15);
Tower reactor (1) also comprises 5 to the 21 layers of grid (16) that are fixed in the tower main body (10) and set gradually according to order up and down; Described grid (16) is arranged between pure steam inlet (12) and the liquid material inlet (13); Each layer grid (16) gone up intensive filler or the pellet type catalyst banked up, the filler of banking up on grid (16) then forms packing layer (21), the catalyst of banking up on grid (16) then forms catalyst layer (22), and packing layer (21) and catalyst layer (22) are according to the interlace mode setting; Described pellet type catalyst is the graininess acidic catalyst;
Tower reactor (1) also comprises the dish type atomizing distributor (17) that is fixed in the tower main body (10) and is positioned at tower main body (10) top; The charging aperture of dish type atomizing distributor (17) and (13) the airtight connection of the liquid material of tower reactor (1) inlet, dish type atomizing distributor (17) is for having the coil pipe of the conventional quantity and the atomizing spray orifice of size on tube wall.
2. continous way according to claim 1 prepares the device of medium high carbon fatty acid ester, it is characterized in that: the filler in the packing layer (21) is the ceramic Pall ring or the cylindrical shape net of being reeled and to be formed by stainless steel cloth.
3. continous way according to claim 1 prepares the device of medium high carbon fatty acid ester, it is characterized in that: described graininess acidic catalyst is that particle diameter is the solid acid catalyst of 3～10mm.
4. continous way according to claim 3 prepares the device of medium high carbon fatty acid ester, it is characterized in that: described solid acid catalyst is SO
4 2-/ M
xO
yThe solid super acid catalyst of type; Described SO
4 2-/ M
xO
yThe solid super acid catalyst of type is SO
4 2-/ ZrO
2, SO
4 2-/ Fe
2O
3, SO
4 2-/ Al
2O
3, SO
4 2-/ ZrO
2-Al
2O
3, or SO
4 2-/ TiO
2-SnO
2-Al
2O
3
5. continous way according to claim 1 prepares the device of medium high carbon fatty acid ester, it is characterized in that: the height of described cylindric tower reactor (1) is 15～30m, and diameter is 0.5～3m; Described liquid material inlet (13) to the distance at tower main body (10) top of cylindric tower reactor (1) is 0.5～1.5m; Described pure steam inlet (12) to the distance of tower main body (10) bottom of cylindric tower reactor (1) is 5～10m; Basecoat in the described grid (16) is positioned at top, described pure steam inlet (12) 0.5～1m; The nozzle diameter of described steam (vapor) outlet (14) is 0.1～0.5m; The loading height of described catalyst layer (22) is 5～20cm; The loading height of packing layer (21) is 1～5m; Distance between the upper end of the material on the lower end of last layer grid (16) and the following one deck grid (16) is 20～35cm.
6. prepare the device of medium high carbon fatty acid ester according to the described continous way of one of claim 1 to 5, it is characterized in that: total number of plies of described grid (16) is an odd number, and odd number layer wherein is packing layer (21), and the even numbers layer is catalyst layer (22).
7. a continous way prepares the device of medium high carbon fatty acid ester, it is characterized in that: comprise air film type reaction unit (1); Air film type reaction unit (1) is a tower reactor; This tower reactor (1) comprises the tower main body (10) of cylinder shelly and is separately positioned on ester floss hole (11) on the tower main body (10), alcohol inlet (12 '), aliphatic acid inlet (13 ') and steam (vapor) outlet (14) from bottom to top; Ester floss hole (11) is positioned at the bottom of tower main body (10), and alcohol inlet (12 ') is positioned at tower main body (10) sidepiece below, and aliphatic acid inlet (13 ') is positioned at tower main body (10) sidepiece top, and steam (vapor) outlet (14) is positioned at the top of tower main body (10); The bottom of tower main body (10) is liquid storage portion (15);
Tower reactor (1) also comprises the grid (16) that is fixed in the tower main body (10); Described grid (16) is arranged between alcohol inlet (12 ') and the aliphatic acid inlet (13 '); Grid (16) is provided with the formed packing layer of the intensive filler of banking up (21);
Tower reactor (1) also comprises dish type atomizing distributor (17) and the spiral heater (18) that is fixed in the tower main body (10); Spiral heater (18) is positioned at alcohol inlet (the 12 ') below of tower main body (10); Dish type atomizing distributor (17) is for having the coil pipe of the conventional quantity and the atomizing spray orifice of size on tube wall; Dish type atomizing distributor (17) is positioned at the top of tower main body (10), and its charging aperture enters the mouth (13 ') airtight linking to each other with the aliphatic acid of tower reactor (1).
8. continous way according to claim 7 prepares the device of medium high carbon fatty acid ester, it is characterized in that: the filler in the packing layer (21) is the ceramic Pall ring or the cylindrical shape net of being reeled and to be formed by stainless steel cloth.
9. continous way according to claim 7 prepares the device of medium high carbon fatty acid ester, it is characterized in that: grid (16) has 3 to 10 layers, is equipped with the formed packing layer of the intensive filler of banking up (21) on every layer of grid (16).
10. continous way according to claim 7 prepares the device of medium high carbon fatty acid ester, it is characterized in that: the height of described cylindric tower reactor (1) is 15～30m, and diameter is 0.5～3m; Described aliphatic acid inlet (13 ') to the distance at tower main body (10) top of cylindric tower reactor (1) is 0.5～1.5m; Described alcohol inlet (12 ') to the distance of tower main body (10) bottom of cylindric tower reactor (1) is 5～10m; Basecoat in the described grid (16) is positioned at described alcohol inlet (12) top 0.5～1m; The nozzle diameter of described steam (vapor) outlet (14) is 0.1～0.5m; The loading height of described packing layer (21) is 1～5m; Distance between the upper end of the material on the lower end of last layer grid (16) and the following one deck grid (16) is 20～35cm.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010205613428U CN201880521U (en) | 2010-10-14 | 2010-10-14 | Device for continuously preparing medium-high carbon fatty acid ester |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010205613428U CN201880521U (en) | 2010-10-14 | 2010-10-14 | Device for continuously preparing medium-high carbon fatty acid ester |
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| Publication Number | Publication Date |
|---|---|
| CN201880521U true CN201880521U (en) | 2011-06-29 |
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|---|---|---|---|
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| CN (1) | CN201880521U (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113522220A (en) * | 2020-04-22 | 2021-10-22 | 兆联实业股份有限公司 | Filling tower of composite filling material |
| CN113893787A (en) * | 2021-10-28 | 2022-01-07 | 八叶草健康产业研究院(厦门)有限公司 | Reactor for multiphase continuous reaction |
-
2010
- 2010-10-14 CN CN2010205613428U patent/CN201880521U/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113522220A (en) * | 2020-04-22 | 2021-10-22 | 兆联实业股份有限公司 | Filling tower of composite filling material |
| CN113893787A (en) * | 2021-10-28 | 2022-01-07 | 八叶草健康产业研究院(厦门)有限公司 | Reactor for multiphase continuous reaction |
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