CN105418423A - Method and device for benzene-removal and purification of n-propyl acetate - Google Patents
Method and device for benzene-removal and purification of n-propyl acetate Download PDFInfo
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- CN105418423A CN105418423A CN201510975746.9A CN201510975746A CN105418423A CN 105418423 A CN105418423 A CN 105418423A CN 201510975746 A CN201510975746 A CN 201510975746A CN 105418423 A CN105418423 A CN 105418423A
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- lightness
- benzene
- tower
- propyl acetate
- removing column
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- YKYONYBAUNKHLG-UHFFFAOYSA-N propyl acetate Chemical compound CCCOC(C)=O YKYONYBAUNKHLG-UHFFFAOYSA-N 0.000 title claims abstract description 102
- 238000000034 method Methods 0.000 title claims abstract description 39
- 238000000746 purification Methods 0.000 title claims abstract description 12
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims abstract description 123
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 37
- 238000010992 reflux Methods 0.000 claims abstract description 19
- 230000008569 process Effects 0.000 claims abstract description 16
- 239000000470 constituent Substances 0.000 claims description 46
- 239000000047 product Substances 0.000 claims description 43
- 239000012043 crude product Substances 0.000 claims description 31
- 239000002253 acid Substances 0.000 claims description 27
- 125000004123 n-propyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])* 0.000 claims description 27
- 230000008676 import Effects 0.000 claims description 21
- 238000007670 refining Methods 0.000 claims description 18
- 238000000605 extraction Methods 0.000 claims description 14
- 239000008346 aqueous phase Substances 0.000 claims description 13
- 239000000523 sample Substances 0.000 claims description 13
- NBBJYMSMWIIQGU-UHFFFAOYSA-N Propionic aldehyde Chemical compound CCC=O NBBJYMSMWIIQGU-UHFFFAOYSA-N 0.000 claims description 12
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 8
- 238000002360 preparation method Methods 0.000 claims description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- 150000001336 alkenes Chemical class 0.000 claims description 6
- 239000003054 catalyst Substances 0.000 claims description 6
- 229910052739 hydrogen Inorganic materials 0.000 claims description 6
- 239000001257 hydrogen Substances 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 5
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 238000006170 formylation reaction Methods 0.000 claims description 4
- 150000002431 hydrogen Chemical class 0.000 claims description 4
- 238000005984 hydrogenation reaction Methods 0.000 claims description 4
- 239000012071 phase Substances 0.000 claims description 4
- 230000000694 effects Effects 0.000 claims description 3
- 230000032050 esterification Effects 0.000 claims description 3
- 238000005886 esterification reaction Methods 0.000 claims description 3
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 2
- 230000009471 action Effects 0.000 claims description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 2
- 229910002091 carbon monoxide Inorganic materials 0.000 claims description 2
- 238000002309 gasification Methods 0.000 claims description 2
- 238000007037 hydroformylation reaction Methods 0.000 claims description 2
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 claims description 2
- WJIBZZVTNMAURL-UHFFFAOYSA-N phosphane;rhodium Chemical compound P.[Rh] WJIBZZVTNMAURL-UHFFFAOYSA-N 0.000 claims description 2
- CGFYHILWFSGVJS-UHFFFAOYSA-N silicic acid;trioxotungsten Chemical compound O[Si](O)(O)O.O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1.O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1.O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1.O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 CGFYHILWFSGVJS-UHFFFAOYSA-N 0.000 claims description 2
- XTHPWXDJESJLNJ-UHFFFAOYSA-N sulfurochloridic acid Chemical compound OS(Cl)(=O)=O XTHPWXDJESJLNJ-UHFFFAOYSA-N 0.000 claims description 2
- 239000012535 impurity Substances 0.000 abstract description 4
- 239000012074 organic phase Substances 0.000 abstract description 3
- 238000009833 condensation Methods 0.000 abstract 1
- 230000005494 condensation Effects 0.000 abstract 1
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 15
- 239000000463 material Substances 0.000 description 6
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 5
- 235000019439 ethyl acetate Nutrition 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 4
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 4
- 230000001105 regulatory effect Effects 0.000 description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 1
- JTXMVXSTHSMVQF-UHFFFAOYSA-N 2-acetyloxyethyl acetate Chemical compound CC(=O)OCCOC(C)=O JTXMVXSTHSMVQF-UHFFFAOYSA-N 0.000 description 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 150000001555 benzenes Chemical class 0.000 description 1
- XZKRXPZXQLARHH-UHFFFAOYSA-N buta-1,3-dienylbenzene Chemical compound C=CC=CC1=CC=CC=C1 XZKRXPZXQLARHH-UHFFFAOYSA-N 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000003209 petroleum derivative Substances 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
- C07C67/52—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a method and a device for benzene-removal and purification of n-propyl acetate. According to the invention, a crude benzene-contained n-propyl acetate product and water are mixed and introduced into a light-component removing tower, and light components are totally produced from the tower top of the light-component removing tower; the light components totally produced from the tower top are introduced into a condenser; after condensation, cooled products are introduced into a reflux tank, wherein one part of the light components are introduced out by the reflux tank, and the other part of the light components are introduced into the top part of the light-component removing tower by a reflux pump for light-component removing treatment again; a primary benzene-removed refined n-propyl acetate product is obtained from the tower bottom of the light-component removing tower; the tower-bottom primary refined product is circularly introduced into the light-component removing tower through a reboiler for circular light-component removing treatment; and after circular treatment, the benzene-removed refined n-propyl acetate is obtained. The device provided by the invention employs a total producing process, so separated organic phases can be reutilized; and through adjusting of an adding proportion of the water and the crude benzene-contained n-propyl acetate product, and further adjusting of temperatures of the tower top and the tower bottom of the light-component removing tower, organic micromolecules and water are formed into an azeotrope and discharged out, so the content of impurities like benzene is reduced.
Description
Technical field
The invention belongs to chemical field, be specifically related to a kind of de-benzene method of purification and device of n-propyl acetate.
Background technology
Along with popularizing of non-toluene solvent, n-propyl acetate starts to show one's capabilities in printing industry as the favorable substitutes of toluene, acetone equal solvent.Be mainly derived from petroleum products owing to producing in n-propyl acetate raw material, keep away unavoidable containing arene materials such as benzene, make to there is micro-benzene in product thus cannot all kinds of packaging industry quality index such as food be reached.Therefore, in acetic ester production process, need the content as far as possible reducing the arene materials such as benzene from raw material and last handling process.
Reduce the residual volume of benzene in n-propyl acetate, not only will reduce the content of raw material containing the arene material such as benzene, and will avoid extraneously introducing the content that the arene materials such as benzene increase the arene materials such as remaining benzene in product as far as possible, affect product quality.In current acetic ester production technique, general employing contains the ion exchange resin of benzene as catalyzer, as the preparation method of publication number a kind of acetic ester disclosed in the patent of invention of CN102264685A, adopt porousness Zeo-karb as catalyzer, described catalyzer is the sulfonic structure of addition on the multipolymer of vinylbenzene and Vinylstyrene; The synthetic method of publication number a kind of ethylene diacetate disclosed in the patent of invention of CN103724195A, adopts p-methyl benzenesulfonic acid to be that catalyzer completes esterification, all contains benzene class material in above-mentioned catalyzer, increases the impurity benzene content of final product.For making acetic ester use safely, needing to carry out de-benzene process further to its product, different de-benzene process can be selected according to the difference of benzol content and the difference of production technique.But, still there is de-benzene in prior art not thorough, the phenomenon that in product, benzene content exceeds standard.In addition, different according to purposes, also different to the content requirement of acetic ester in product, for adapting to the different market requirements, reducing production cost, need the production equipment of acetate content in a set of easy adjustment product.
Summary of the invention
Goal of the invention: the object of the invention is for the deficiencies in the prior art, the de-benzene method of purification of the n-propyl acetate providing a kind of easy-regulating n-propyl acetate content, de-benzene effective and device.
Technical scheme: the de-benzene method of purification of a kind of n-propyl acetate of the present invention, you will import in lightness-removing column after mixing than 5 ~ 10:1 containing ALPHA Tolylic acid n-propyl crude product and hydromassage, de-light process is carried out under 100 ~ 110 DEG C of conditions, light constituent is from the full extraction of lightness-removing column tower top, and described light constituent comprises azeotrope and the fluorescence probe of water, water and fluorescence probe; Imported in condenser by the light constituent of complete for tower top extraction, will cool after product after being condensed to 30 ~ 80 DEG C and import return tank, part light constituent is derived by described return tank, and another part light constituent is imported lightness-removing column top through reflux pump, again carries out de-light process;
Obtain n-propyl acetate at the bottom of tower and take off benzene refining head product, benzene refining head product is taken off to the n-propyl acetate at the bottom of tower and to import in lightness-removing column through reboiler circulation and carry out that circulation is de-gently to be processed, after circular treatment 2 ~ 5 times, obtain de-benzene refining n-propyl acetate.
Preferably, for reducing the benzene content in product as far as possible, the described preparation method containing ALPHA Tolylic acid n-propyl crude product comprises the following steps:
A. be raw material with alkene, water miscible rhodium phosphine complex is catalyzer, aqueous catalyst solution is sent into formylation reaction device, then passes into alkene, carbon monoxide and hydrogen, and hydroformylation of olefin occurs, and isolates propionic aldehyde after reaction terminates from formylation reaction device;
B. mix obtaining propionic aldehyde in step a with hydrogen, after gasification, propionic aldehyde and hydrogen enter fixed-bed reactor, under Cu-series catalyst effect, carry out hydrogenation reaction, obtain propyl alcohol product after reaction terminates;
C. the propyl alcohol obtained in step b and acetic acid are imported in esterifier, under catalyst action, carry out esterification obtain containing the thick product of ALPHA Tolylic acid n-propyl.
Preferably, for avoiding introducing impurity benzene, the catalyzer described in step c is the one in sulfuric acid, phosphoric acid, silicotungstic acid or chlorsulfonic acid.
Preferably, for improving de-benzene effect, the tower top temperature of described lightness-removing column is 80 ~ 105 DEG C; The column bottom temperature of described lightness-removing column is 100 ~ 110 DEG C.
A kind of de-benzene purifying plant for n-propyl acetate, comprise water tower, containing ALPHA Tolylic acid n-propyl crude product tank, lightness-removing column, reboiler, product pump, condenser, return tank and reflux pump, the outlet of described water tower with described export to converge containing ALPHA Tolylic acid n-propyl crude product tank be connected with described lightness-removing column entrance afterwards, described lightness-removing column outlet at bottom is divided into two branch roads, article one, branch road is connected with described product pump entrance, another branch road is connected with described lightness-removing column bottom inlet through reboiler, described lightness-removing column top exit is connected with described condenser inlet, described condensator outlet is connected with described return tank entrance, baffled in described return tank, return tank inside forms light constituent phase and aqueous phase two regions, described aqueous phase imports aqueous phase treatment unit through conduit, described light constituent is divided into two to export mutually derives, part light constituent is derived outside system by an outlet mutually, light constituent is imported described lightness-removing column top entry through reflux pump by another outlet mutually.
Preferably, for widening the boundary of light constituent and aqueous phase, described baffle plate is vertically arranged in described return tank, is highly 20% ~ 80% of described return tank total height.
Preferably, for convenience of regulating water and the adding proportion containing ALPHA Tolylic acid n-propyl crude product, described water tower outlet connection traffic variable valve.
Preferably, for convenience of regulating water and the adding proportion containing ALPHA Tolylic acid n-propyl crude product, described ALPHA Tolylic acid n-propyl crude product tank outlet connection traffic variable valve.
Preferably, for improving Operational Figure Of Merit and efficiency, described flow control valve, lightness-removing column, reboiler, product pump, condenser, return tank are connected with DCS Controlling System with reflux pump.
Beneficial effect: (1) the present invention adopts full extraction technique, can again utilize after organic phase being isolated, and not only reduces the discharge of moisture, also improves economic benefit and the environment friendly of technique; (2) the present invention is by regulating water and the adding proportion containing ALPHA Tolylic acid n-propyl crude product, a step of going forward side by side saves tower top and the column bottom temperature of lightness-removing column, fluorescence probe and water are formed azeotrope discharge, reduce the content of the impurity such as benzene, make the high purity 99.982% of n-propyl acetate; (3) in the de-benzene device in the present invention, by adding baffle plate in return tank, and regulate its height, increase the boundary of aqueous phase and light constituent phase, not only contribute to discharging unnecessary moisture, avoid organic phase to discharge with moisture, affect reuse factor, also improve the purity of n-propyl acetate in the finished product simultaneously; (4) the present invention can be different for the purity demanding criteria of market Dichlorodiphenyl Acetate n-propyl, by adjusting de-light cycle index, water and containing parameters such as the adding proportion of ALPHA Tolylic acid n-propyl crude product and temperature, obtain the product of different purity easily, improve utilization ratio of device.
Accompanying drawing explanation
Fig. 1 is apparatus structure schematic diagram of the present invention:
Wherein 1. water towers, 2. containing ALPHA Tolylic acid n-propyl crude product tank, 3. lightness-removing column, 4. reboiler, 5. product pump, 6. condenser, 7. return tank, 8. reflux pump, 9. Water Pipe Valve, 10. crude product pipe variable valve, A. light constituent export mouth, B. aqueous phase export mouth.
Embodiment
Below by accompanying drawing, technical solution of the present invention is described in detail, but protection scope of the present invention is not limited to described embodiment.
embodiment 1:by the preparation of method disclosed in patent CN101774912A containing ALPHA Tolylic acid n-propyl crude product, import in lightness-removing column to carry out taking off after mixing than 8:1 containing ALPHA Tolylic acid n-propyl crude product and hydromassage that and gently process, lightness-removing column column bottom temperature is 105 ~ 107 DEG C, lightness-removing column tower top temperature is 95 ~ 98 DEG C, light constituent is from the full extraction of lightness-removing column tower top, and described light constituent comprises azeotrope and the fluorescence probe of water, water and fluorescence probe; Imported in condenser by the light constituent of complete for tower top extraction, will cool after product after being condensed to 72 DEG C and import return tank, part light constituent is derived by described return tank, and another part light constituent is imported lightness-removing column top through reflux pump, again carries out de-light process; Obtain n-propyl acetate at the bottom of tower to take off benzene and take off benzene refining head product, benzene is taken off to the n-propyl acetate at the bottom of tower and takes off benzene refining head product and to import in lightness-removing column through reboiler circulation and carry out that circulation is de-gently to be processed, after circular treatment 3 times, obtain de-benzene refining n-propyl acetate.
Complete the device of above-mentioned de-benzene method, comprise water tower 1, containing ALPHA Tolylic acid n-propyl crude product tank 2, lightness-removing column 3, reboiler 4, product pump 5, condenser 6, return tank 7 and reflux pump 8, described water tower 1 outlet is connected with water pipe, water pipe is arranged Water Pipe Valve 9, be connected with crude product pipe containing the outlet of ALPHA Tolylic acid n-propyl crude product tank 2, crude product pipe is arranged crude product pipe variable valve 10, be connected with described lightness-removing column 3 entrance after water pipe and crude product manifold close, described lightness-removing column 3 outlet at bottom is divided into two branch roads, article one, branch road is connected with described product pump 5 entrance, another branch road is connected with described lightness-removing column 3 bottom inlet through reboiler 4, described lightness-removing column 3 top exit is connected with described condenser 6 entrance, described condenser 6 outlet is connected with described return tank 7 entrance, baffled in described return tank 7, return tank 7 inside forms light constituent phase and aqueous phase two regions, described aqueous phase imports aqueous phase treatment unit through aqueous phase export mouth B, described light constituent is divided into two to export mutually derives, an outlet is light constituent export mouth A, part light constituent is derived outside system mutually, light constituent is imported described lightness-removing column 3 top entry through reflux pump 8 by another outlet mutually.
Height of baffle plate in this device in return tank 7 is 80% of return tank total height, and lightness-removing column 3, reboiler 4, product pump 5, condenser 6, return tank 7, reflux pump 8, Water Pipe Valve 9 and crude product pipe variable valve 10 are connected with DCS Controlling System.
Analyze known through GC-MS, n-propyl acetate purity obtained in the present embodiment can reach 99.982%, and benzene content is 0.151 ‰.
embodiment 2:by the preparation of method disclosed in patent CN101774912A containing ALPHA Tolylic acid n-propyl crude product, import in lightness-removing column to carry out taking off after mixing than 7:1 containing ALPHA Tolylic acid n-propyl crude product and hydromassage that and gently process, lightness-removing column column bottom temperature is 102 ~ 105 DEG C, lightness-removing column tower top temperature is 80 ~ 83 DEG C, light constituent is from the full extraction of lightness-removing column tower top, and described light constituent comprises azeotrope and the fluorescence probe of water, water and fluorescence probe; Imported in condenser by the light constituent of complete for tower top extraction, will cool after product after being condensed to 62 DEG C and import return tank, part light constituent is derived by described return tank, and another part light constituent is imported lightness-removing column top through reflux pump, again carries out de-light process; Obtain n-propyl acetate at the bottom of tower and take off benzene refining head product, benzene refining head product is taken off to the n-propyl acetate at the bottom of tower and to import in lightness-removing column through reboiler circulation and carry out that circulation is de-gently to be processed, after circular treatment 5 times, obtain de-benzene refining n-propyl acetate.
The device preparing n-propyl acetate in the present embodiment is in the same manner as in Example 1, and its difference is: the height of baffle plate in the present embodiment in return tank 7 is 80% of return tank total height.
Analyze known through GC-MS, n-propyl acetate purity obtained in the present embodiment can reach 99.985%, and benzene content is 0.145 ‰.
embodiment 3:by the preparation of method disclosed in patent CN101774912A containing ALPHA Tolylic acid n-propyl crude product, import in lightness-removing column to carry out taking off after mixing than 5:1 containing ALPHA Tolylic acid n-propyl crude product and hydromassage that and gently process, lightness-removing column column bottom temperature is 100 ~ 102 DEG C, lightness-removing column tower top temperature is 80 ~ 83 DEG C, light constituent is from the full extraction of lightness-removing column tower top, and described light constituent comprises azeotrope and the fluorescence probe of water, water and fluorescence probe; Imported in condenser by the light constituent of complete for tower top extraction, will cool after product after being condensed to 32 DEG C and import return tank, part light constituent is derived by described return tank, and another part light constituent is imported lightness-removing column top through reflux pump, again carries out de-light process; Obtain n-propyl acetate at the bottom of tower and take off benzene refining head product, benzene refining head product is taken off to the n-propyl acetate at the bottom of tower and to import in lightness-removing column through reboiler circulation and carry out that circulation is de-gently to be processed, after circular treatment 2 times, obtain de-benzene refining n-propyl acetate.
The device preparing n-propyl acetate in the present embodiment is in the same manner as in Example 1, and its difference is: the height of baffle plate in the present embodiment in return tank 7 is 65% of return tank total height.
Analyze known through GC-MS, n-propyl acetate purity obtained in the present embodiment can reach 99.882%, and benzene content is 0.211 ‰.
embodiment 4:by the preparation of method disclosed in patent CN101774912A containing ALPHA Tolylic acid n-propyl crude product, import in lightness-removing column to carry out taking off after mixing than 10:1 containing ALPHA Tolylic acid n-propyl crude product and hydromassage that and gently process, lightness-removing column column bottom temperature is 108 ~ 110 DEG C, lightness-removing column tower top temperature is 102 ~ 105 DEG C, light constituent is from the full extraction of lightness-removing column tower top, and described light constituent comprises azeotrope and the fluorescence probe of water, water and fluorescence probe; Imported in condenser by the light constituent of complete for tower top extraction, will cool after product after being condensed to 78 DEG C and import return tank, part light constituent is derived by described return tank, and another part light constituent is imported lightness-removing column top through reflux pump, again carries out de-light process; Obtain n-propyl acetate at the bottom of tower and take off benzene refining head product, benzene refining head product is taken off to the n-propyl acetate at the bottom of tower and to import in lightness-removing column through reboiler circulation and carry out that circulation is de-gently to be processed, after circular treatment 2 times, obtain de-benzene refining n-propyl acetate.
The device preparing n-propyl acetate in the present embodiment is in the same manner as in Example 1, and its difference is: the height of baffle plate in the present embodiment in return tank 7 is 22% of return tank total height.
Analyze known through GC-MS, n-propyl acetate purity obtained in the present embodiment can reach 99.663%, and benzene content is 1.412 ‰.
Present method and device, can to arrange in pairs or groups again full extraction technique by regulating cycle index and temperature condition, obtain the product of different mass standard, when circulation 3 times and above time can obtain purity and reach >=99.982%, benzene content be≤0.151 ‰ n-propyl acetate, be applicable to the industries such as food product pack; When circulation less than 3 times, obtain the n-propyl acetate of purity≤99.882%, benzol content≤1.412 ‰, can be used as and produce PTA supporting belt aqua; This device is easy to adjust, can meet the demand of market to different purity standard n-propyl acetate simultaneously, improve utilization ratio of device.
As mentioned above, although represented with reference to specific preferred embodiment and described the present invention, it shall not be construed as the restriction to the present invention self.Under the spirit and scope of the present invention prerequisite not departing from claims definition, various change can be made in the form and details to it.
Claims (10)
1. the de-benzene method of purification of a n-propyl acetate, it is characterized in that: you will import in lightness-removing column after mixing than 5 ~ 10:1 containing ALPHA Tolylic acid n-propyl crude product and hydromassage, de-light process is carried out under 100 ~ 110 DEG C of conditions, light constituent is from the full extraction of lightness-removing column tower top, and described light constituent comprises azeotrope and the fluorescence probe of water, water and fluorescence probe; Imported in condenser by the light constituent of complete for tower top extraction, will cool after product after being condensed to 30 ~ 80 DEG C and import return tank, part light constituent is derived by described return tank, and another part light constituent is imported lightness-removing column top through reflux pump, again carries out de-light process;
Obtain n-propyl acetate at the bottom of tower and take off benzene refining head product, benzene refining head product is taken off to the n-propyl acetate at the bottom of tower and to import in lightness-removing column through reboiler circulation and carry out that circulation is de-gently to be processed, after circular treatment 2 ~ 5 times, obtain de-benzene refining n-propyl acetate.
2. the de-benzene method of purification of n-propyl acetate according to claim 1, is characterized in that: the described preparation method containing ALPHA Tolylic acid n-propyl crude product comprises the following steps:
A. be raw material with alkene, water miscible rhodium phosphine complex is catalyzer, aqueous catalyst solution is sent into formylation reaction device, then passes into alkene, carbon monoxide and hydrogen, and hydroformylation of olefin occurs, and isolates propionic aldehyde after reaction terminates from formylation reaction device;
B. mix obtaining propionic aldehyde in step a with hydrogen, after gasification, propionic aldehyde and hydrogen enter fixed-bed reactor, under Cu-series catalyst effect, carry out hydrogenation reaction, obtain propyl alcohol product after reaction terminates;
C. the propyl alcohol obtained in step b and acetic acid are imported in esterifier, under catalyst action, carry out esterification obtain containing the thick product of ALPHA Tolylic acid n-propyl.
3. the de-benzene method of purification of n-propyl acetate according to claim 2, is characterized in that: the catalyzer described in step c is the one in sulfuric acid, phosphoric acid, silicotungstic acid or chlorsulfonic acid.
4. the de-benzene method of purification of n-propyl acetate according to claim 1, is characterized in that: the tower top temperature of described lightness-removing column is 80 ~ 105 DEG C.
5. the de-benzene method of purification of n-propyl acetate according to claim 1, is characterized in that: the column bottom temperature of described lightness-removing column is 100 ~ 110 DEG C.
6. the device of the de-benzene method of purification of the n-propyl acetate described in claim 1 ~ 5 any one, comprise water tower, containing ALPHA Tolylic acid n-propyl crude product tank, lightness-removing column, reboiler, product pump, condenser, return tank and reflux pump, it is characterized in that: the outlet of described water tower with described export to converge containing ALPHA Tolylic acid n-propyl crude product tank be connected with described lightness-removing column entrance afterwards, described lightness-removing column outlet at bottom is divided into two branch roads, article one, branch road is connected with described product pump entrance, another branch road is connected with described lightness-removing column bottom inlet through reboiler, described lightness-removing column top exit is connected with described condenser inlet, described condensator outlet is connected with described return tank entrance, baffled in described return tank, return tank inside forms light constituent phase and aqueous phase two regions, described aqueous phase imports aqueous phase treatment unit through conduit, described light constituent is divided into two to export mutually derives, part light constituent is derived outside system by an outlet mutually, light constituent is imported described lightness-removing column top entry through reflux pump by another outlet mutually.
7. device according to claim 6, is characterized in that: described baffle plate is vertically arranged in described return tank, is highly 20% ~ 80% of described return tank total height.
8. device according to claim 6, is characterized in that: described water tower outlet connection traffic variable valve.
9. device according to claim 6, is characterized in that: described ALPHA Tolylic acid n-propyl crude product tank outlet connection traffic variable valve.
10. device according to claim 6, is characterized in that: described flow control valve, lightness-removing column, reboiler, product pump, condenser, return tank are connected with DCS Controlling System with reflux pump.
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