CN102875328A - Catalyzing rectifying technology for synthesizing sec-butyl alcohol through ester exchange method and production equipment of catalyzing rectifying technology - Google Patents
Catalyzing rectifying technology for synthesizing sec-butyl alcohol through ester exchange method and production equipment of catalyzing rectifying technology Download PDFInfo
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- CN102875328A CN102875328A CN2012103497318A CN201210349731A CN102875328A CN 102875328 A CN102875328 A CN 102875328A CN 2012103497318 A CN2012103497318 A CN 2012103497318A CN 201210349731 A CN201210349731 A CN 201210349731A CN 102875328 A CN102875328 A CN 102875328A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
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Abstract
The invention provides a catalyzing rectifying technology for synthesizing sec-butyl alcohol through an ester exchange method and production equipment for the catalyzing rectifying technology. The catalyzing rectifying technology comprises the following steps of: feeding raw materials of acetic acid sec-butyl acetate and methanol from the upper part and the lower part of a reaction section of a catalyzing rectifying tower respectively; carrying out an ester exchange reaction for the two raw materials in the reaction section under a catalyzing effect of a cation exchange resin, and synchronously carrying out steam-liquid mass transfer, thus achieving a continuous catalyzing and rectifying process. According to the catalyzing rectifying technology provided by the invention, the cation exchange resin is served as a catalyst, and the catalyzing rectifying technology is adopted, therefore, operation can be continuously carried out, a technological process can be simplified, and a problem due to recycling of an alkali salt catalyst and a problem that the catalyst in the tower is easily crystallized and separated can be avoided; and the catalyzing rectifying technology has the characteristics of being low in energy consumption, low in material consumption, high in reaction transformation rate, and stable in product quality and the like.
Description
Technical field:
The present invention relates to a kind of catalytic rectification process and production unit thereof that adopts the synthetic sec-butyl alcohol of ester-interchange method take 2-butyl acetate and methyl alcohol as raw material.
Background technology:
Sec-butyl alcohol has another name called the 2-butanols, and colourless transparent liquid has strong aroma.Fusing point-114.7 ℃, 99.5 ℃ of boiling points, water-soluble and benzene is with ethanol, ether can be miscible arbitrarily, also is dissolved in acetone.Sec-butyl alcohol as solvent, emulsifying agent, dye dispersant, dewatering agent, paint remover, industrial detergent etc., also is used as softening agent, weedicide, oil extraction agent industrial.Because sec-butyl alcohol can increase processing characteristics and the ductility of coating, nitro sprays paint, the solubility promoter of thinner for nitrocellulose finishes so can be used as.Can be used as again the raw material of producing spices, dyestuff, wetting agent, flotation agent etc., also can be used as the intermediate of producing methylethylketone, be used for N-BUTYL ACETATE processed, secondary butyl ester etc.Can be used as the cosolvent of methyl alcohol, as the component that improves gasoline octane rating.
The production technique of sec-butyl alcohol mainly is preparation take n-butene as the raw material hydration at present, is divided into indirect hydration method and direct hydration method.The hydration method is the traditional method of n-butylene hydration sec-butyl alcohol processed indirectly, namely take sulfuric acid as catalyzer, prepares sec-butyl alcohol by esterification, hydrolysis reaction.This method is high to the transformation efficiency of the gentle n-butene of the not high reaction conditions of raw material n-butene purity requirement; But need to consume a large amount of sulfuric acid and caustic soda, equipment corrosion and seriously polluted, reaction preference is lower, and it is serious that the higher meeting of n-butene unit consumption produces a large amount of acid-bearing wastewater environmental pollutions.Direct hydration method is under an acidic catalyst effect, and n-butene and water hydration reaction directly occur generates sec-butyl alcohol.According to the difference of employed catalyzer, direct hydration method is divided into resin method and heteropolyacid method, though this technique have do not consume a large amount of sulfuric acid and caustic soda still can etching apparatus, require the per pass conversion of high (90%) n-butene low to material purity.
Summary of the invention:
The present invention is directed to the deficiency that above-mentioned technology exists, proposes a kind ofly take 2-butyl acetate and methyl alcohol as raw material, adopt ester-interchange method to synthesize the catalytic rectification process of sec-butyl alcohol.
Technical program of the present invention lies in:
1) the raw material 2-butyl acetate enters in the tower from catalytic rectifying tower conversion zone top behind volume pump, material benzenemethanol enters in the tower from catalytic rectifying tower conversion zone bottom behind volume pump, raw material 2-butyl acetate and methyl alcohol mix at the conversion zone that is positioned at the catalytic rectifying tower middle part, under the effect of catalyzer transesterification reaction occur;
2) in catalytic rectifying tower.The mixing steam of ritalin and methyl alcohol steams from the rectifying tower cat head, enters return tank after condenser condenses, is back to catalytic rectifying tower through a reflux pump part, and another part is with being pumped to the methyl esters rectifying tower.Tower reactor is that sec-butyl alcohol, methyl alcohol and a small amount of 2-butyl acetate escape and enter methanol distillation column with discharging pump;
3) the methyl esters rectifying tower separates rear cat head and obtains ritalin, and component methyl alcohol turns back to the catalytic rectifying tower methanol inlet at the bottom of the tower;
4) the catalytic rectifying tower materials at bottom of tower enters methanol distillation column and separates, and cat head light constituent methyl alcohol is after condenser condenses, and a part is back to methanol distillation column through reflux pump.Another part turns back to catalytic rectifying tower methanol inlet place, and tower reactor obtains sec-butyl alcohol and a small amount of 2-butyl acetate, and pump to sec-butyl alcohol treating tower is made with extra care;
5) in the sec-butyl alcohol treating tower, sec-butyl alcohol and 2-butyl acetate mixture carry out compression rectification, and cat head obtains the product sec-butyl alcohol, obtains 2-butyl acetate at the bottom of the tower.
Another object of the present invention is to provide a kind of sec-butyl alcohol transesterify catalysis catalytic distillation production unit, this equipment has yield height, few, the low power consumption and other advantages of internal circulating load.
Another technical scheme of the present invention is: a kind of sec-butyl alcohol transesterify catalytic distillation production unit, comprise catalytic rectifying tower, it is characterized in that: described catalytic rectifying tower comprises rectifying section from top to bottom, conversion zone and stripping section, be provided with the 2-butyl acetate opening for feed between described rectifying section and the conversion zone, be provided with the methanol feeding mouth between described conversion zone and the stripping section, described conversion zone filling male ion-exchange resin catalyzer, be provided with some sections catalyst structure unit that are stacked into certain altitude in the described reaction zone, the diameter of described catalyst structure unit is suitable with the diameter of conversion zone, and described catalyst structure unit is made of through curling bundled shape the solid acid resin catalyst pouch that one deck Stainless Steel Cloth and one deck are connected in series.
Remarkable advantage of the present invention is: take Zeo-karb as catalyzer, realize the synthetic sec-butyl alcohol of serialization in conjunction with catalytic rectification process, simplified technical process, reduce production energy consumption and material consumption, improve the transesterification reaction transformation efficiency.Be specially:
(1) the synthetic sec-butyl alcohol of 2-butyl acetate and methanol oxidation and separating substances are carried out in catalytic rectifying tower simultaneously, and sepn process and reaction process are mutually promoted, Effective Raise reaction conversion ratio and yield, and simultaneous reactions heat is fully utilized and has reduced the rectifying energy consumption;
(2) adopt continuous catalyzing rectifying can realize large-scale serialization production, constant product quality;
(3) in the continuous catalyzing rectifying tower, reaction is only carried out in conversion zone, in the conversion zone residence time of material little, potential side reaction is few, good product quality.
(4) reactive distillation processes of employing basic catalyst, need to add a large amount of methyl alcohol in reaction process affects the reactive distillation processes normal running to avoid catalyzer to separate out.And continuous catalyzing rectifying process using Zeo-karb is catalyzer, has avoided this problem fully, can greatly reduce material consumption, has also saved simultaneously the energy consumption of Separation and Recovery excessive methanol.
(5) continuous catalyzing rectifying process using Zeo-karb is catalyzer, and is little to equipment corrosion, and catalyst loading adopts and to tie up packet form, and not easy to wear and broken, catalyst life is long, need not by the recovery of the methods such as evaporation, and technique is simple.
Description of drawings:
Fig. 1 is the sec-butyl alcohol technological process of production of the present invention;
Fig. 2 is catalyst structure cell schematics of the present invention;
Fig. 3 is the schematic cross-section of catalyst structure of the present invention unit;
Fig. 4 is the synoptic diagram of the catalytic solid acidic resins pouch of series connection of the present invention;
Fig. 5 is Stainless Steel Cloth structural representation of the present invention;
Number in the figure is as follows: the T101-catalytic rectifying tower, T102-methyl esters rectifying tower, the T103-methanol rectifying tower, T104-sec-butyl alcohol treating tower, S1-catalytic rectifying tower rectifying section, S2 catalytic rectifying tower conversion zone, S3-catalytic rectifying tower stripping section, E1-catalytic rectifying tower overhead condenser, E2-methyl esters rectifying tower cat head condenser, E3-methanol rectifying tower overhead condenser, E4-sec-butyl alcohol treating tower overhead condenser, PL1-2-butyl acetate feed-pipe, PL2-methanol feeding pipe, PL3-catalytic rectifying tower overhead vapours pipe, PL4-catalytic rectifying tower trim the top of column pipe, PL5-catalytic rectifying tower overhead extraction pipe, PL6-methyl esters rectifying tower cat head vapour pipe, PL7-methyl esters rectifying column top return pipe, PL8-methyl esters rectifying tower cat head extraction pipe, PL9-catalytic rectifying tower tower reactor extraction pipe, PL10-methanol loop pipe, PL11-methanol rectifying tower overhead vapours pipe, PL12-methanol rectifying tower trim the top of column pipe, PL13-methanol rectifying tower overhead extraction pipe, PL14-methanol rectifying tower tower reactor extraction pipe, PL15-sec-butyl alcohol treating tower overhead vapours pipe, PL16-sec-butyl alcohol treating tower trim the top of column pipe, PL17-sec-butyl alcohol treating tower overhead extraction pipe, PL18-sec-butyl alcohol treating tower tower reactor extraction pipe, the 7-Stainless Steel Cloth, 8-pouch, 16-catalyzer bag internal pore.
Embodiment:
The present invention is take 2-butyl acetate and methyl alcohol as raw material, and the catalytic rectification process of the synthetic sec-butyl alcohol of ester-interchange method carries out according to the following steps:
1) the raw material 2-butyl acetate enters in the tower from catalytic rectifying tower T101 conversion zone S2 top behind volume pump, material benzenemethanol enters in the tower from catalytic rectifying tower conversion zone S2 bottom behind volume pump, raw material 2-butyl acetate and methyl alcohol mix at the conversion zone that is positioned at catalysis catalytic rectifying tower middle part, under the effect of catalyzer transesterification reaction occur;
2) ritalin that obtains at conversion zone and the mixing steam of methyl alcohol are discharged from the rectifying section top that is positioned at catalytic rectifying tower top, after condenser E1 condensation, enter return tank, be back to catalytic rectifying tower T101 through a pump part, another part is with being pumped to methyl esters rectifying tower T102.Transesterification reaction produce sec-butyl alcohol and at the bottom of the unconverted methyl alcohol of part and a small amount of acetic acid sec-butyl alcohol fall into still from the stripping section bottom of catalytic rectifying tower bottom, and discharge through pump and to enter methanol distillation column T103;
3) methyl esters rectifying tower T102 separates, and cat head obtains ritalin and methanol azeotrope after condenser E2 condensation, and to the methyl esters rectifying tower, another part is through the pump extraction through pump reflux for a part, and tower reactor obtains methyl alcohol and turns back to catalytic rectifying tower T101 methanol inlet;
4) materials at bottom of tower enters methanol distillation column T103 and separates, cat head light constituent methyl alcohol after condenser E3 condensation, a part through pump reflux to methanol distillation column.Another part turns back to catalytic rectifying tower T101 methanol inlet place, and tower reactor obtains sec-butyl alcohol and a small amount of 2-butyl acetate, and pump is made with extra care to sec-butyl alcohol treating tower T104;
5) sec-butyl alcohol and 2-butyl acetate carry out compression rectification in sec-butyl alcohol treating tower T104, and cat head obtains the product sec-butyl alcohol, and after condenser E4 condensation, a part is back to T104, and another part enters the product stock tank.Obtain 2-butyl acetate at the bottom of the tower.
Described catalyzer is Zeo-karb.
The mol ratio of described methyl alcohol and 2-butyl acetate is 1.0 ~ 1.5:1.3.
Described catalytic rectifying tower T101 operational condition is: tower top pressure is normal pressure, and tower top temperature is controlled at about 50 ~ 57, and the temperature of conversion zone is controlled at 65 ~ 85 ℃, and column bottom temperature is controlled at 100 ~ 110 ℃, and reflux ratio R is 0.5 ~ 4, and air speed is 0.2 ~ 0.5m
3/ (m
3Catalyzer h).
Sec-butyl alcohol catalysis catalytic distillation production unit of the present invention, comprise catalytic rectifying tower T101, described rectifying tower comprises rectifying section S1 from top to bottom, conversion zone S2 and stripping section S3, be provided with the 2-butyl acetate opening for feed between described rectifying section and the conversion zone, be provided with the methanol feeding mouth between described conversion zone and the stripping section, described conversion zone filling male ion-exchange resin catalyzer, be provided with some sections catalyst structure unit that are stacked into certain altitude in the described reaction zone, the diameter of described catalyst structure unit is suitable with the diameter of conversion zone, and described catalyst structure unit is made of through curling bundled shape the solid acid resin catalyst pouch that one deck Stainless Steel Cloth and one deck are connected in series.
The pouch that is used for the parcel cation exchange resin catalyst adopts spun silk cloth or nylon cloth or woven dacron to make, and the cation exchange resin catalyst of filling in the pouch accounts for 0.7 ~ 0.9 times of pouch volume, and pouch is of a size of 45 ~ 80mm * 9 ~ 16mm.Described Stainless Steel Cloth is that pore size is 60 ~ 90 order molybdenum titanium Stainless Steel Cloths.
The theoretical number of plates of rectifying section of described catalytic rectifying tower T101 is 10 ~ 25, and the number of theoretical plate of conversion zone is 15 ~ 30, and the number of theoretical plate of stripping section is 3 ~ 5.
With reference to figure 1, the catalytic rectifying tower epimere is rectifying section S1, interposition conversion zone S2, hypomere is stripping section S3, whole body of the tower material is SUS304, and rectifying section S1, stripping section S3 fill CY700 ripple silk net filler, and wherein theoretical number of plates of rectifying section is 10 ~ 25, the number of theoretical plate of conversion zone is 15 ~ 30, and the number of theoretical plate of stripping section is 3 ~ 5.Fill BX500 ripple silk net filler in the methyl esters rectifying tower T102 tower, wherein the number of theoretical plate of rectifying section S4 is 10 ~ 25, and the theoretical plate number of stripping section S5 is 3 ~ 5.Fill BX500 ripple silk net filler in the methanol rectification Tata, wherein the number of theoretical plate of rectifying section S6 is 10 ~ 30, and the number of theoretical plate of stripping section S7 is 10 ~ 20.Fill BX500 ripple silk net filler in the refining Tata of sec-butyl alcohol, 20 ~ 45 of the number of theoretical plates of rectifying section S8 wherein, the number of theoretical plate of stripping section S9 is 10 ~ 20.
Referring to figs. 2 to Fig. 5, the pouch that Zeo-karb is housed in the catalyst structure unit is tiffany or nylon cloth or woven dacron, and its support and gas passage are outer field Stainless Steel Cloth, and its specification is 01 ~ 0.15 string diameter, 60 ~ 90 purpose molybdenum titanium Stainless Steel Cloths.
The making method of catalyst structure unit is as follows: the pouch that is sewn into 45 ~ 80mm * 9 ~ 16mm with spun silk cloth or nylon cloth or woven dacron, be filled with the Zeo-karb of capacity 0.7 ~ 0.9 in the bag, pouch is connected with pouch to be sewn into a slice and to have wavy sheet bag; Get the Stainless Steel Cloth that size and sheet bag are fit to, it is 3 ~ 8mm that Stainless Steel Cloth is pressed into peak height, and tooth profile angle is 45 ~ 60.The Stainless Steel Cloth of line shape is laid Stainless Steel Cloth and sheet bag below, again they is rolled into a bundle together, and the right cylinder external diameter that is is suitable with the conversion zone diameter, in the Stainless Steel Cloth tooth ripple be arranged in parallel and with base obliquity at 45 °.
Conversion zone S2 overlaps reaction zone by some catalyst structures unit vertical interlaced, and the profile of tooth ripple of ripple Stainless Steel Cloth trend is staggered in the adjacent catalyst structure unit from top to down, to increase the turbulent extent of vapour-liquid fluid, vapour-liquid is fully contacted.
Embodiment 1:
Adopt the technical process shown in the accompanying drawing 1, catalytic rectifying tower T101 conversion zone raw material 2-butyl acetate and methyl alcohol pass through respectively the volume pump charging take mass ratio as 2-butyl acetate: methyl alcohol=1:1.3.Two kinds of raw materials are realized the process of continuous catalyzing rectifying in conversion zone generation transesterify catalyzed reaction and carry out the vapour-liquid mass exchange under the effect of catalyzer.
Catalytic rectifying tower T101 body of the tower material is SUS304, and rectifying section, stripping section, conversion zone are filled respectively CY700 ripple silk net filler, and wherein theoretical number of plates of rectifying section is 15, and the number of theoretical plate of conversion zone is 30, and the number of theoretical plate of stripping section is 4.Methyl esters rectifying tower stature material is SUS304, fills CY700 ripple silk net filler in the tower, and number of theoretical plate is 25.Methanol distillation column body of the tower material is SUS304, fills out CY700 ripple silk net filler in the tower, and number of theoretical plate is 35; Sec-butyl alcohol treating tower body of the tower material is SUS304, fills CY700 ripple silk net filler in the tower, and number of theoretical plate is 45.
To be the cylindrical structural unit be of a size of the pouch of filling the solid acid resin in 55 * 12mm by length and width to Catalyst capsule that to practice into shoulder to shoulder the corrugated body be that the corrugated 80 purpose stainless (steel) wires of 60 degree stack and are rolled into a bundle, the pitch angle that online every the tooth ripple of Stainless Steel Wire and silk screen formation 45 are spent with the onesize tooth profile angle that is pressed into.
The operational condition of catalytic rectifying tower T101: working pressure is 1atm, 56 ℃ of tower top temperatures, and reaction zone temperature is 83 ℃, 108 ℃ of tower reactor temperature, reflux ratio R=2, superficial velocity 0.25 m
3/ (m
3Catalyzer h).
Methyl esters rectifying tower T102 operational condition: working pressure 1atm, 54 ℃ of tower top temperatures, 64 ℃ of column bottom temperatures, reflux ratio R=2, superficial velocity 0.5 m
3/ (m
3Filler h).
Methanol rectifying tower T103 operational condition: working pressure 1atm, 65 ℃ of tower top temperatures, 102.5 ℃ of column bottom temperatures, reflux ratio R=2, superficial velocity 0.5 m
3/ (m
3Filler h).
Sec-butyl alcohol treating tower T104 operational condition: working pressure 5atm, 152.2 ℃ of tower top temperatures, 156.5 ℃ of column bottom temperatures, reflux ratio R=2, superficial velocity 0.5 m
3/ (m
3Filler h).
From catalytic rectifying tower T101 rectifying section top out ritalin and methanol steam through condenser E1 condensation, the material of condensation part backflow cat head, a part of extraction product, the overhead product ritalin: methyl alcohol is the 0.75:0.25(mass ratio); The sec-butyl alcohol, methyl alcohol, the 2-butyl acetate massfraction that fall into tower reactor from catalytic rectifying tower T101 stripping section are respectively 0.69,0.30,0.01.
Enter methyl esters rectifying tower T102 from catalytic rectifying tower T101 rectifying section evaporator overhead condenser part effluent liquid ritalin and methyl alcohol mixed liquor, in the methyl esters rectifying tower ritalin and methanol mixed steam through the rectifying section overhead stream to steam through condenser E12 condensation, the material part backflow cat head of condensation, a part of extraction product; The mass ratio of overhead product ritalin and methyl alcohol is 0.82:0.18; Can reach 88% from the methanol purity of methyl esters rectifying tower profit reduction and reserving section tower reactor extraction, enter catalytic rectifying tower as raw material.
Sec-butyl alcohol, methyl alcohol, 2-butyl acetate from the catalytic rectifying tower stripping section enter methanol rectifying tower T103, methyl alcohol through rectifying tower rectifying section top methanol steam out through condenser E3 condensation, the material of condensation part backflow cat head, a part of extraction product; The overhead product methanol purity is 99.5%; The mixed solution of methanol rectifying tower tower reactor extraction is sec-butyl alcohol and 2-butyl acetate, and the massfraction of product is respectively 0.95,0.05; Enter sec-butyl alcohol treating tower T104.
Sec-butyl alcohol treating tower T104 rectifying section top sec-butyl alcohol steam out is through condenser E4 condensation, the material of condensation part backflow cat head, and a part of extraction product, overhead product sec-butyl alcohol massfraction is 100%; Sec-butyl alcohol treating tower T104 tower reactor out be 2-butyl acetate, its mass concentration is 60%, can be used as raw material and enters catalytic rectifying tower.
2-butyl acetate transformation efficiency 0.89 sec-butyl alcohol yield 0.90.
Embodiment 2:
Adopt the technical process shown in the accompanying drawing 1, catalytic rectifying tower T101 conversion zone raw material 2-butyl acetate and methyl alcohol pass through respectively the volume pump charging take mass ratio as 2-butyl acetate: methyl alcohol=1:1.5.Two kinds of raw materials are realized the process of continuous catalyzing rectifying in conversion zone generation transesterification reaction and carry out the vapour-liquid mass exchange under the effect of cation exchange resin catalyst.
Catalytic rectifying tower T101 body of the tower material is SUS304, and rectifying section, stripping section, conversion zone are filled respectively CY700 ripple silk net filler, and wherein theoretical number of plates of rectifying section is 12, and the number of theoretical plate of conversion zone is 32, and the number of theoretical plate of stripping section is 5.Methyl esters rectifying tower stature material is SUS304, fills CY700 ripple silk net filler in the tower, and number of theoretical plate is 25.Methanol distillation column body of the tower material is SUS304, fills out CY700 ripple silk net filler in the tower, and number of theoretical plate is 40; Sec-butyl alcohol treating tower body of the tower material is SUS304, fills CY700 ripple silk net filler in the tower, and number of theoretical plate is 45.
To be the cylindrical structural unit be of a size of the pouch of filling the solid acid resin in 55 * 12mm by length and width to Catalyst capsule that to practice into shoulder to shoulder the corrugated body be that the corrugated 80 purpose stainless (steel) wires of 60 degree stack and are rolled into a bundle, the pitch angle that online every the tooth ripple of Stainless Steel Wire and silk screen formation 45 are spent with the onesize tooth profile angle that is pressed into.
Catalytic rectifying tower T101 operational condition: working pressure is 1atm, 57 ℃ of tower top temperatures, and reaction zone temperature is 88 ℃, 110 ℃ of tower reactor temperature, reflux ratio R=2, superficial velocity 0.25 m
3/ (m
3Catalyzer h).
Methyl esters rectifying tower T102 operational condition: working pressure 1atm, 55 ℃ of tower top temperatures, 64 ℃ of column bottom temperatures, reflux ratio R=2, superficial velocity 0.5 m
3/ (m
3Filler h).
Methanol rectifying tower T103 operational condition: working pressure 1atm, 64 ℃ of tower top temperatures, 101 ℃ of column bottom temperatures, reflux ratio R=2, superficial velocity 0.5 m
3/ (m
3Filler h).
Sec-butyl alcohol treating tower T104 operational condition: working pressure 5atm, tower top temperature 152..5 ℃, 156.0 ℃ of column bottom temperatures, reflux ratio R=2, superficial velocity 0.5 m
3/ (m
3Filler h).
From catalytic rectifying tower T101 rectifying section top out ritalin and methanol steam through condenser E1 condensation, the material of condensation part backflow cat head, a part of extraction product, the overhead product ritalin: methyl alcohol is the 0.7:0.3(mass ratio); The sec-butyl alcohol, methyl alcohol, the 2-butyl acetate massfraction that fall into tower reactor from catalytic rectifying tower T101 stripping section are respectively 0.65,0.34,0.01.
Enter methyl esters rectifying tower T102 from catalytic rectifying tower T101 rectifying section evaporator overhead condenser part effluent liquid ritalin and methyl alcohol mixed liquor, in the methyl esters rectifying tower ritalin and methanol mixed steam through the rectifying section overhead stream to steam through condenser E2 condensation, the material part backflow cat head of condensation, a part of extraction product; The mass ratio of overhead product ritalin and methyl alcohol is 0.8:0.2; Can reach 90% from the methanol purity of methyl esters rectifying tower profit reduction and reserving section tower reactor extraction, enter catalytic rectifying tower as raw material.
Sec-butyl alcohol, methyl alcohol, 2-butyl acetate from catalytic rectifying tower T101 stripping section enter methanol rectifying tower T103, methyl alcohol through rectifying tower rectifying section top methanol steam out through condenser E3 condensation, the material part backflow cat head of condensation, a part of extraction product; The overhead product methanol purity is 99.6%; The mixed solution of methanol rectifying tower tower reactor extraction is sec-butyl alcohol and 2-butyl acetate, and the massfraction of product is respectively 0.97,0.03; Enter sec-butyl alcohol treating tower T104.
Sec-butyl alcohol treating tower T104 rectifying section top sec-butyl alcohol steam out is through condenser E4 condensation, the material of condensation part backflow cat head, and a part of extraction product, overhead product sec-butyl alcohol massfraction is 100%; Sec-butyl alcohol treating tower T104 tower reactor out be 2-butyl acetate, its mass concentration is 58%, can be used as raw material and enters catalytic rectifying tower.
2-butyl acetate transformation efficiency 0.91, sec-butyl alcohol yield 0.92.
Embodiment 3:
Adopt the technical process shown in the accompanying drawing 1, catalytic rectifying tower T101 conversion zone raw material 2-butyl acetate and methyl alcohol pass through respectively the volume pump charging take mass ratio as 2-butyl acetate: methyl alcohol=1:1.3.Two kinds of raw materials are realized the process of continuous catalyzing rectifying in conversion zone generation transesterification reaction and carry out the vapour-liquid mass exchange under the effect of cation exchange resin catalyst.
Catalytic rectifying tower T101 body of the tower material is SUS304, and rectifying section, stripping section, conversion zone are filled respectively CY700 ripple silk net filler, and wherein theoretical number of plates of rectifying section is 10, and the number of theoretical plate of conversion zone is 35, and the number of theoretical plate of stripping section is 5.Methyl esters rectifying tower stature material is SUS304, fills CY700 ripple silk net filler in the tower, and number of theoretical plate is 25.Methanol rectifying tower T101 body of the tower material is SUS304, fills out CY700 ripple silk net filler in the tower, and number of theoretical plate is 40; Sec-butyl alcohol treating tower T104 body of the tower material is SUS304, fills CY700 ripple silk net filler in the tower, and number of theoretical plate is 45.
To be the cylindrical structural unit be of a size of the pouch of filling the solid acid resin in 55 * 12mm by length and width to Catalyst capsule that to practice into shoulder to shoulder the corrugated body be that the corrugated 80 purpose stainless (steel) wires of 60 degree stack and are rolled into a bundle, the pitch angle that online every the tooth ripple of Stainless Steel Wire and silk screen formation 45 are spent with the onesize tooth profile angle that is pressed into.
Catalytic rectifying tower T101 operational condition: working pressure is 1atm, 55 ℃ of tower top temperatures, and reaction zone temperature is 96 ℃, 105 ℃ of tower reactor temperature, reflux ratio R=3, superficial velocity 0.3 m
3/ (m
3Catalyzer h).
Methyl esters rectifying tower T102 operational condition: working pressure 1atm, 54 ℃ of tower top temperatures, 64 ℃ of column bottom temperatures, reflux ratio R=2, superficial velocity 0.5 m
3/ (m
3Filler h).
Methanol rectifying tower T103 operational condition: working pressure 1atm, 65 ℃ of tower top temperatures, 102.5 ℃ of column bottom temperatures, reflux ratio R=2, superficial velocity 0.5 m
3/ (m
3Filler h).
Sec-butyl alcohol treating tower T104 operational condition: working pressure 5atm, 152.5 ℃ of tower top temperatures, 156 ℃ of column bottom temperatures, reflux ratio R=2, superficial velocity 0.5 m
3/ (m
3Filler h).
From catalytic rectifying tower T101 rectifying section top out ritalin and methanol steam through condenser condenses, the material of condensation part backflow cat head, a part of extraction product, the overhead product ritalin: methyl alcohol is the 0.72:0.28(mass ratio); The sec-butyl alcohol, methyl alcohol, the 2-butyl acetate massfraction that fall into tower reactor from catalytic rectifying tower T101 stripping section are respectively 0.70,0.29,0.01.
Enter methyl esters rectifying tower T102 from catalytic rectifying tower T101 rectifying section evaporator overhead condenser part effluent liquid ritalin and methyl alcohol mixed liquor, in the methyl esters rectifying tower ritalin and methanol mixed steam through the rectifying section overhead stream to steam through condenser E2 condensation, the material part backflow cat head of condensation, a part of extraction product; The mass ratio of overhead product ritalin and methyl alcohol is 0.82:0.18; Can reach 95% from the methanol purity of methyl esters rectifying tower T102 profit reduction and reserving section tower reactor extraction, enter catalytic rectifying tower as raw material.
Sec-butyl alcohol, methyl alcohol, 2-butyl acetate from catalytic rectifying tower T101 stripping section enter methanol rectifying tower T103, methyl alcohol through rectifying tower T103 rectifying section top methanol steam out through condenser E1 condensation, the material part backflow cat head of condensation, a part of extraction product; The overhead product methanol purity is 99.7%; The mixed solution of methanol rectifying tower T103 tower reactor extraction is sec-butyl alcohol and 2-butyl acetate, and the massfraction of product is respectively 0.98,0.02; Enter sec-butyl alcohol treating tower T104.
Sec-butyl alcohol treating tower T104 rectifying section top sec-butyl alcohol steam out is through condenser E4 condensation, the material of condensation part backflow cat head, and a part of extraction product, overhead product sec-butyl alcohol massfraction is 100%; Sec-butyl alcohol treating tower T104 tower reactor out be 2-butyl acetate, its mass concentration is 75%, can be used as raw material and enters catalytic rectifying tower.
2-butyl acetate transformation efficiency 0.92, sec-butyl alcohol yield 0.93.
Embodiment 4:
Adopt the technical process shown in the accompanying drawing 1, catalytic rectifying tower T101 conversion zone raw material 2-butyl acetate and methyl alcohol pass through respectively the volume pump charging take mass ratio as 2-butyl acetate: methyl alcohol=1:1.5.Two kinds of raw materials are realized the process of continuous catalyzing rectifying in conversion zone generation transesterification reaction and carry out the vapour-liquid mass exchange under the effect of cation exchange resin catalyst.
Catalytic rectifying tower T101 body of the tower material is SUS304, and rectifying section, stripping section, conversion zone are filled respectively CY700 ripple silk net filler, and wherein theoretical number of plates of rectifying section is 10, and the number of theoretical plate of conversion zone is 30, and the number of theoretical plate of stripping section is 4.Methyl esters rectifying tower T102 body of the tower material is SUS304, fills CY700 ripple silk net filler in the tower, and number of theoretical plate is 25.Methanol rectifying tower T103 body of the tower material is SUS304, fills out CY700 ripple silk net filler in the tower, and number of theoretical plate is 40; Sec-butyl alcohol treating tower T104 body of the tower material is SUS304, fills CY700 ripple silk net filler in the tower, and number of theoretical plate is 45.
To be the cylindrical structural unit be of a size of the pouch of filling the solid acid resin in 55 * 12mm by length and width to Catalyst capsule that to practice into shoulder to shoulder the corrugated body be that the corrugated 80 purpose stainless (steel) wires of 60 degree stack and are rolled into a bundle, the pitch angle that online every the tooth ripple of Stainless Steel Wire and silk screen formation 45 are spent with the onesize tooth profile angle that is pressed into.
Catalytic rectifying tower T101 operational condition: working pressure is 1atm, 56 ℃ of tower top temperatures, and reaction zone temperature is 93 ℃, 108 ℃ of tower reactor temperature, reflux ratio R=3, superficial velocity 0.25 m
3/ (m
3Catalyzer h).
Methyl esters rectifying tower T102 operational condition: working pressure 1atm, 55 ℃ of tower top temperatures, 64 ℃ of column bottom temperatures, reflux ratio R=2, superficial velocity 0.5 m
3/ (m
3Filler h).
Methanol rectifying tower T103 operational condition: working pressure 1atm, 65 ℃ of tower top temperatures, 101.5 ℃ of column bottom temperatures, reflux ratio R=2, superficial velocity 0.5 m
3/ (m
3Filler h).
Sec-butyl alcohol treating tower T104 operational condition: working pressure 4atm, 142.2 ℃ of tower top temperatures, 146.5 ℃ of column bottom temperatures, reflux ratio R=2, superficial velocity 0.5 m
3/ (m
3Filler h).
From catalytic rectifying tower T101 rectifying section top out ritalin and methanol steam through condenser condenses, the material of condensation part backflow cat head, a part of extraction product, the overhead product ritalin: methyl alcohol is the 0.70:0.30(mass ratio); The sec-butyl alcohol, methyl alcohol, the 2-butyl acetate massfraction that fall into tower reactor from catalytic rectifying tower T101 stripping section are respectively 0.64,0.35,0.01.
Enter methyl esters rectifying tower T102 from catalytic rectifying tower T101 rectifying section evaporator overhead condenser part effluent liquid ritalin and methyl alcohol mixed liquor, in the methyl esters rectifying tower ritalin and methanol mixed steam through the rectifying section overhead stream to steam through condenser E2 condensation, the material part backflow cat head of condensation, a part of extraction product; The mass ratio of overhead product ritalin and methyl alcohol is 0.80:0.20; Can reach 93% from the methanol purity of methyl esters rectifying tower T102 profit reduction and reserving section tower reactor extraction, enter catalytic rectifying tower as raw material.
Sec-butyl alcohol, methyl alcohol, 2-butyl acetate from catalytic rectifying tower T101 stripping section enter methanol rectifying tower, methyl alcohol through rectifying tower rectifying section top methanol steam out through condenser E3 condensation, the material of condensation part backflow cat head, a part of extraction product; The overhead product methanol purity is 99.8%; The mixed solution of methanol rectifying tower T103 tower reactor extraction is sec-butyl alcohol and 2-butyl acetate, and the massfraction of product is respectively 0.98,0.02; Enter sec-butyl alcohol treating tower T104.
Sec-butyl alcohol treating tower T104 rectifying section top sec-butyl alcohol steam out is through condenser condenses, the material of condensation part backflow cat head, and a part of extraction product, overhead product sec-butyl alcohol massfraction is 100%; Sec-butyl alcohol treating tower T104 tower reactor out be 2-butyl acetate, its mass concentration is 45%, can be used as raw material and enters catalytic rectifying tower.
2-butyl acetate transformation efficiency 0.86, sec-butyl alcohol yield 0.87.
The above only is preferred embodiment of the present invention, and all equalizations of doing according to the present patent application claim change and modify, and all should belong to covering scope of the present invention.
Claims (10)
1. the catalytic rectification process of the synthetic sec-butyl alcohol of an ester-interchange method take 2-butyl acetate and methyl alcohol as raw material, is characterized in that technique carries out as follows:
1) 2-butyl acetate and methyl alcohol pump into catalytic rectifying tower from the upper and lower of conversion zone respectively, 2-butyl acetate and methyl alcohol is reverse transmission of heat by contact mass transfer in the conversion zone at catalytic rectifying tower middle part, under the reacting section catalyst effect, carry out transesterification reaction, light constituent ritalin and methyl alcohol condensation after steaming from cat head after the rectifying section concentrate after the reaction, part phlegma is back to catalytic rectifying tower, another part condensate pump is to methyl esters rectifying tower concentrate, the catalytic rectifying tower tower kettle product is sec-butyl alcohol, methyl alcohol and a small amount of 2-butyl acetate enter methanol rectifying tower after the pump extraction;
2) ritalin of catalytic rectifying tower overhead extraction and methyl alcohol mixed liquor enter methyl esters rectifying tower middle part, and ritalin and the methanol azeotrope of cat head are back to methyl esters rectifying tower top, another part extraction through a condenser condenses part after separating; The methyl alcohol of high density returns catalytic rectifying tower conversion zone bottom as the part material recycled at the bottom of the tower;
3) catalytic rectifying tower tower reactor Produced Liquid enters methanol rectifying tower by the middle part and separates, light constituent methyl alcohol at cat head through condenser condenses, a part is back to the methanol rectification column overhead, another part extraction is returned catalytic rectifying tower conversion zone bottom as the part material recycled, and tower reactor still liquid sec-butyl alcohol and a small amount of 2-butyl acetate are purified through pump to sec-butyl alcohol treating tower;
4) sec-butyl alcohol of methanol rectifying tower tower reactor extraction and a small amount of 2-butyl acetate enter the sec-butyl alcohol treating tower by the middle part after the pump pressurization, the highly purified sec-butyl alcohol steam of cat head is after condenser condenses, a part is back to sec-butyl alcohol treating tower cat head, and another part extraction obtains the sec-butyl alcohol product; The 2-butyl acetate of minute quantity and sec-butyl alcohol mixed solution are by the tower reactor extraction.
2. realize that the described ester-interchange method of claim 1 synthesizes the production unit of the catalytic rectification process of sec-butyl alcohol for one kind, it is characterized in that: described production unit comprises catalytic rectifying tower, methyl esters rectifying tower, methanol rectifying tower and sec-butyl alcohol treating tower.
3. the catalytic distillation production unit of the synthetic sec-butyl alcohol of described ester-interchange method according to claim 2, it is characterized in that: the raw material of the catalytic rectification process of the synthetic sec-butyl alcohol of described ester-interchange method is 2-butyl acetate and methyl alcohol, 2-butyl acetate is by the top charging of described catalytic rectifying tower conversion zone, and methyl alcohol is by the underfeed of described catalytic rectifying tower conversion zone.
4. according to claim 2 or the catalytic distillation production unit of the synthetic sec-butyl alcohol of 3 described ester-interchange methods, it is characterized in that: described catalytic rectifying tower comprises rectifying section, conversion zone and stripping section from top to bottom, wherein the stripping section number of theoretical plate is 3 ~ 5, theoretical number of plates of rectifying section is 10 ~ 25, and the conversion zone number of theoretical plate is 15～35; Described conversion zone filling male ion-exchange resin catalyzer, be provided with the some catalyst structures unit that is stacked into certain altitude in the described conversion zone, described catalyst structure unit is made of through curling bundled shape the cation exchange resin catalyst pouch that one deck Stainless Steel Cloth and one deck are connected in series.
5. the catalytic distillation production unit of the synthetic sec-butyl alcohol of described ester-interchange method according to claim 4, it is characterized in that: the pouch that is used for the parcel cation exchange resin catalyst adopts spun silk cloth, nylon cloth or woven dacron to make, and described Stainless Steel Cloth is that pore size is 60 ~ 90 order molybdenum titanium Stainless Steel Cloths; Described cation exchange resin catalyst pouch is of a size of 45 ~ 80mm * 9 ~ 16mm; The Zeo-karb of filling in the described cation exchange resin catalyst pouch accounts for 70～90% of pouch volume.
6. the catalytic distillation production unit of the synthetic sec-butyl alcohol of described ester-interchange method according to claim 2, it is characterized in that: the working pressure of described catalytic rectifying tower is 0.09 ~ 0.11MPa(absolute pressure), raw material 2-butyl acetate and methanol feeding mol ratio are 1:1.5 ~ 1:3, and the charging air speed of 2-butyl acetate is 0.2 ~ 0.5 m
3/ (m
3Catalyzer h), control of reflux ratio is 0.5～4, and tower top temperature is controlled at 55 ~ 62 ℃, 65 ~ 90 ℃ of tower reactor temperature; Described catalytic rectifying tower transesterification reaction transformation efficiency is more than 95%.
7. the catalytic distillation production unit of the synthetic sec-butyl alcohol of described ester-interchange method according to claim 2, it is characterized in that: the ritalin massfraction is 60% ~ 75% in the described catalytic rectifying tower overhead extraction liquid, the methanol quality mark is 25% ~ 40%, the sec-butyl alcohol massfraction is 70% ~ 80% in the tower reactor Produced Liquid, and methanol content is 20% ~ 30%; The reaction conversion ratio of described catalytic rectifying tower is greater than 95%.
8. the catalytic distillation production unit of the synthetic sec-butyl alcohol of described ester-interchange method according to claim 2, it is characterized in that: described methyl esters rectifying tower is made of rectifying section and stripping section, and wherein theoretical number of plates of rectifying section is 10～15, and stripping section plate number is 10～20; Working pressure is 0.09 ~ 0.11MPa(absolute pressure), control of reflux ratio is 1 ~ 3; Described methyl esters rectifying tower cat head obtains the ritalin of massfraction more than 75%, and the tower reactor Produced Liquid is the methyl alcohol more than 99%, and circulation is as the raw material of catalytic rectifying tower.
9. the catalytic distillation production unit of the synthetic sec-butyl alcohol of described ester-interchange method according to claim 2, it is characterized in that: described methanol rectifying tower is made of rectifying section and stripping section, and wherein the number of theoretical plate of rectifying section is 15～25, and the number of theoretical plate of stripping section is 10～20; Working pressure is 0.09 ~ 0.11MPa(absolute pressure), control of reflux ratio is 1 ~ 3; Described methanol rectifying tower overhead extraction is methyl alcohol, returns catalytic rectifying tower as raw material; Tower reactor extraction massfraction is greater than 95% sec-butyl alcohol and a small amount of 2-butyl acetate.
10. the catalytic distillation production unit of the synthetic sec-butyl alcohol of described ester-interchange method according to claim 2, it is characterized in that: described sec-butyl alcohol treating tower is made of rectifying section and stripping section, wherein the number of theoretical plate of rectifying section is 20～40, and the number of theoretical plate of stripping section is 10～15; Working pressure is 0.2 ~ 0.6MPa(absolute pressure), control of reflux ratio is 2～5, and the overhead extraction liquid of described sec-butyl alcohol treating tower is purity greater than 99% product sec-butyl alcohol.
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| CN104549372A (en) * | 2015-01-24 | 2015-04-29 | 福州大学 | Solid super acid for catalytically synthesizing PMA (2-acetoxy-1-methoxypropane), and catalytic rectification technique and apparatus thereof |
| CN105111079A (en) * | 2015-09-14 | 2015-12-02 | 湖南中创化工股份有限公司 | Method and device for separating acetic acid sec-butyl ester and sec-butyl alcohol |
| CN108017507A (en) * | 2017-12-04 | 2018-05-11 | 福州大学 | A kind of method of fixed bed-reactive distillation Joint Production high-purity sec-butyl alcohol |
| CN113651691A (en) * | 2021-09-15 | 2021-11-16 | 河北工业大学 | Method for preparing asymmetric oxalate through catalytic rectification |
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| CN104549372A (en) * | 2015-01-24 | 2015-04-29 | 福州大学 | Solid super acid for catalytically synthesizing PMA (2-acetoxy-1-methoxypropane), and catalytic rectification technique and apparatus thereof |
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| CN115318232A (en) * | 2022-07-12 | 2022-11-11 | 铜陵贝斯美科技有限公司 | Device and production process for coproducing amyl alcohol and methyl acetate |
| CN115318232B (en) * | 2022-07-12 | 2024-02-23 | 铜陵贝斯美科技有限公司 | Device and production process for co-producing amyl alcohol and methyl acetate |
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