CN109824628A - A kind of purification process of chromatography pure tetrahydrofuran - Google Patents
A kind of purification process of chromatography pure tetrahydrofuran Download PDFInfo
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- CN109824628A CN109824628A CN201811524351.7A CN201811524351A CN109824628A CN 109824628 A CN109824628 A CN 109824628A CN 201811524351 A CN201811524351 A CN 201811524351A CN 109824628 A CN109824628 A CN 109824628A
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- tetrahydrofuran
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- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 title claims abstract description 151
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 title claims abstract description 76
- 238000004587 chromatography analysis Methods 0.000 title claims abstract description 27
- 238000000746 purification Methods 0.000 title claims abstract description 23
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 58
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000000835 fiber Substances 0.000 claims abstract description 24
- 238000001179 sorption measurement Methods 0.000 claims abstract description 21
- 239000012279 sodium borohydride Substances 0.000 claims abstract description 18
- 229910000033 sodium borohydride Inorganic materials 0.000 claims abstract description 18
- CSDQQAQKBAQLLE-UHFFFAOYSA-N 4-(4-chlorophenyl)-4,5,6,7-tetrahydrothieno[3,2-c]pyridine Chemical compound C1=CC(Cl)=CC=C1C1C(C=CS2)=C2CCN1 CSDQQAQKBAQLLE-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 16
- 150000002978 peroxides Chemical class 0.000 claims abstract description 14
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 13
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000000292 calcium oxide Substances 0.000 claims abstract description 9
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 4
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 4
- 238000012512 characterization method Methods 0.000 claims abstract description 4
- 230000009467 reduction Effects 0.000 claims description 28
- 238000001914 filtration Methods 0.000 claims description 17
- 239000002994 raw material Substances 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 11
- 238000011049 filling Methods 0.000 claims description 10
- 230000000694 effects Effects 0.000 claims description 9
- 229910052799 carbon Inorganic materials 0.000 claims description 8
- 238000004458 analytical method Methods 0.000 claims description 7
- 239000002274 desiccant Substances 0.000 claims description 7
- 239000002033 PVDF binder Substances 0.000 claims description 5
- 238000003556 assay Methods 0.000 claims description 5
- 239000012530 fluid Substances 0.000 claims description 5
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 5
- 239000003039 volatile agent Substances 0.000 claims description 5
- 238000010992 reflux Methods 0.000 claims description 4
- 239000003381 stabilizer Substances 0.000 claims description 4
- 235000008733 Citrus aurantifolia Nutrition 0.000 claims description 3
- 235000011941 Tilia x europaea Nutrition 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 239000004571 lime Substances 0.000 claims description 3
- 239000007800 oxidant agent Substances 0.000 claims description 2
- 230000001590 oxidative effect Effects 0.000 claims description 2
- 238000010521 absorption reaction Methods 0.000 abstract description 5
- 239000003463 adsorbent Substances 0.000 abstract description 4
- 238000004821 distillation Methods 0.000 abstract description 3
- 229920000049 Carbon (fiber) Polymers 0.000 abstract 1
- 239000004917 carbon fiber Substances 0.000 abstract 1
- 238000007084 catalytic combustion reaction Methods 0.000 abstract 1
- 230000007613 environmental effect Effects 0.000 abstract 1
- 239000000463 material Substances 0.000 abstract 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 abstract 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 7
- 239000012535 impurity Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 5
- 230000009102 absorption Effects 0.000 description 4
- 230000008030 elimination Effects 0.000 description 4
- 238000003379 elimination reaction Methods 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- -1 heterocycle class organic compound Chemical class 0.000 description 4
- 239000001257 hydrogen Substances 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 239000003610 charcoal Substances 0.000 description 3
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 229910052796 boron Inorganic materials 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 description 1
- 230000002596 correlated effect Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 239000011790 ferrous sulphate Substances 0.000 description 1
- 235000003891 ferrous sulphate Nutrition 0.000 description 1
- 150000002240 furans Chemical class 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 1
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 1
- 239000012280 lithium aluminium hydride Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Abstract
The present invention relates to a kind of purification process of chromatography pure tetrahydrofuran, and steps are as follows, (1) utilize the characterization of adsorption adsorption-edulcoration of activated carbon fibre module；(2), using the dry water removal of anhydrous calcium oxide, reducing agent service life is extended；(3) the peroxide in tetrahydrofuran is removed by two concatenated sodium borohydride adsorption columns and calcium hydride adsorption column；(4) rectifying under nitrogen protection prevents distillation process from generating new peroxide.(5) it may be optionally added antioxidant BHT, prevent peroxide from generating, extend shelf life of products.Carbon fiber adsorption and catalytic combustion involved in the present invention is high-efficient, absorption property is strong, Yi Zaisheng, and repeat performance is good., environmental protection more economical compared with other adsorbent materials.
Description
Technical field
The invention belongs to chemical reagent fields, are related to a kind of purification process of chromatography pure tetrahydrofuran.
Background technique
Tetrahydrofuran be colorless and transparent liquid, relative density 0.89, molecular weight 72.11,66 DEG C of boiling point, flash-point-
17.2 DEG C, it is one of strongest polarity ethers that index of refraction 1.407, which is heterocycle class organic compound,.Tetrahydrofuran is one
The important organic synthesis raw material of kind, dissolubility is splendid, there is the title of " alembroth ", has to many organic matters and inorganic matter
Preferable dissolubility, due to this characteristic, tetrahydrofuran is widely used in as extractant, reaction dissolvent, chromatographic solvent etc.
In all kinds of compound experiments.
With the increase of tetrahydrofuran market demand, before this, what my company proposed utilizes activated alumina and activity
The technique that tetrahydrofuran peroxide is eliminated in charcoal absorption is more suitable for a small amount of productions, is directed to mass production and then has one
A little disadvantages, activated alumina are solid powder, when producing chromatography pure tetrahydrofuran, need to be added into stainless steel rectifying still big
Activated alumina is measured, after rectifying experiment, rectifying still bottom can deposit a large amount of activated alumina solids, on the one hand, need to exist
Cleaning prevents danger in time after the completion of production, and the activated alumina after cleaning is not easy to maintain, and activated alumina is caused to utilize
The low adverse effect of rate, on the other hand, activated alumina are more expensive compared to price compared with other reducing agents, cause high-purity tetrahydro
The production cost of furans is higher.In order to solve problem above, company spy improves concrete technology by experimental study.
Summary of the invention
The purpose of the present invention is to provide a kind of purification process of chromatography pure tetrahydrofuran can by purifying of the invention
Obtain the chromatography pure tetrahydrofuran of purity >=99.9%, yield >=95%.
The present invention realizes that the technical solution of purpose is as follows:
A kind of purification process of chromatography pure tetrahydrofuran, steps are as follows
(1) the characterization of adsorption of activated carbon fibre module is utilized；
(2) the peroxidating in tetrahydrofuran is removed by two concatenated sodium borohydride adsorption columns and calcium hydride adsorption column
Object.
Moreover, specific purification process is as follows:
(1) adsorb: Industrial Grade Tetrahydrofuran raw material being filtered by activated carbon fibre module, filtration flow-rate 200
~400mL/min, the raw material after adsorption treatment enter stand-by in head tank；
(2) dry: the tetrahydrofuran feed liquid after adsorption treatment being squeezed into dry in dry column；
(3) restore: carrying out reduction treatment using the Filter column being composed in series by calcium hydride and sodium borohydride；
(4) rectifying: after the tetrahydrofuran feed liquid after reduction treatment is squeezed into rectifying still, it is filled with nitrogen protection, is arranged thermally conductive
100~300 DEG C of oil temperature, 70~80 DEG C of tetrahydrofuran fluid temperature in rectifying still, 65~67 DEG C of kettle top temperature, control reflux
Than 5:1~5, front-end volatiles are discarded, collect tetrahydrofuran finished product after the assay was approved；
(5) filtering, nitrogen charging are filling: product filters in the duct through 0.1~0.22 micron of the foldable filter element of selection PVDF,
Automatic nitrogen-charging is filling, and gained is chromatography pure tetrahydrofuran finished product；
(6) stabilizer is added: by the way that antioxidant BHT is added into product.
Moreover, the purity of the raw material tetrahydrofuran is about 99.5%.
Moreover, the activated carbon fibre module is the filtration system that three concatenated active Carbon fibes are constituted, active carbon
Fibre module is rendered as cylinder, and high 80cm, diameter 10cm, inside is filled with activated carbon fibre.
Moreover, the drying pillar height 1.0m, the diameter 8cm that are used in the drying process, it is internal using anhydrous calcium oxide as doing
Drying prescription, desiccant account for the 2/3 of dry column, and calcium oxide used is analysis carbonate-free lime.
Moreover, reduction pillar height 1.6m, diameter 4.2cm that the in-series reduction device is used, inside is with calcium hydride and boron hydrogen
Change sodium as reducing agent, reducing agent agent accounts for the 1/3 of reduction column, and the speed that tetrahydrofuran passes through reduction column is 100~200mL/
Min, sodium borohydride used are analysis net product.
Moreover, the oxidant BHT additive amount is mass percent 0.1%~0.3%.
Moreover, the water content of the chromatography pure tetrahydrofuran, less than 0.02%, purity 99.9%, peroxide content accords with
International indicator requirement is closed, is lower than 0.015%.
Chromatography tetrahydrofuran Testing index prepared by the present invention is as follows:
The invention has the advantages that
1) present invention replaces active carbon Filter column using activated carbon fibre module, and active carbon powder adsorbent contains largely
Charcoal ash, activated carbon fibre module is more environmentally-friendly, and adsorption treatment effect is also more preferable.
2) clearly, soaking effect is relatively good, will not introduce the impurity such as chloride, valence for the effect of the dry column of the present invention
Lattice are relatively cheap, by adding dry column in reduction column two sides, prevent the reducing agent moisture absorption with this, substantially prolong sodium borohydride
And the service life of the reducing agents such as calcium hydride.
3) present invention is had found by comparing to all kinds of reducing agents: lithium aluminium hydride reduction price is higher, and a large amount of uses are not easy to handle,
Ferrous sulfate and copper chloride etc. are easily introduced metal impurities, not as preferred reducing agent.Therefore, this test selection sodium borohydride
With calcium hydride as reducing agent, two reduction columns are used in series, and reduction effect is more preferable, due to two easy moisture absorptions of reducing agent, also
Former column two sides are added to drying process device, by repeatedly drying, the water content being greatly reduced in product.
4) present invention will be filled with nitrogen as protection gas before distillation process in entire distillation system, prevent heating process
Middle generation peroxide.
Case is embodied
Feature of the invention and other correlated characteristics are further described below by embodiment, so as to skill of going together
The understanding of art personnel:
A kind of purification process of new chromatographic pure tetrahydrofuran, steps are as follows:
(1) the characterization of adsorption for utilizing activated carbon fibre module, is adsorbed and removed some adsorbability impurity, activated carbon fibre mould
The advantage of itself of block is will not to introduce new impurity to product substantially, is contained in the active carbon powder adsorbent applied before this
A large amount of charcoal ash, this time the activated carbon fibre module adsorbent of application is more environmentally-friendly；
(2) the peroxidating in tetrahydrofuran is removed by two concatenated sodium borohydride adsorption columns and calcium hydride adsorption column
Object, one side sodium borohydride and the cascade filtration column impurity-eliminating effect that calcium hydride is formed are more preferable, and can be used repeatedly, and solve
Reducing agent is deposited on the intractable problem in rectifying still bottom, greatly reduces production risk；On the other hand, sodium borohydride and hydrogen
Change calcium advantage of lower cost.
The water content for the tetrahydrofuran product that the present invention purifies can reach 0.02%, purity 99.99%, peroxidating
Object content meets international indicator requirement, is lower than 0.015%.
The specific purification process of tetrahydrofuran provided by the invention, scheme are as follows:
(1) adsorb: firstly, Industrial Grade Tetrahydrofuran raw material is filtered by activated carbon fibre module, filtering out
Adsorbability impurity, filtration flow-rate are 200~400mL/min, and the raw material after adsorption treatment enters stand-by in head tank；
(2) dry: the tetrahydrofuran feed liquid after adsorption treatment squeezed into dry in dry column, water content in reduction sample,
To extend the service life of sodium borohydride and calcium hydride reducing agent.
(3) restore: by the Filter column being composed in series by calcium hydride and sodium borohydride, can both remove the mistake in tetrahydrofuran
Oxide can remove part moisture content again.
(4) rectifying: after the tetrahydrofuran feed liquid after reduction treatment is squeezed into rectifying still, it is filled with nitrogen protection, is arranged thermally conductive
100~300 DEG C of oil temperature, 70~80 DEG C of tetrahydrofuran fluid temperature in rectifying still, 65~67 DEG C of kettle top temperature, control reflux
Than 5:1~5, front-end volatiles are discarded, collect tetrahydrofuran finished product after the assay was approved.
(5) filtering, nitrogen charging are filling: product filters in the duct through 0.1~0.22 micron of the foldable filter element of selection PVDF,
Automatic nitrogen-charging is filling, and packaging is generally 500mL, 1L and 4L, and gained is chromatography pure tetrahydrofuran finished product.
(6) stabilizer is added: by the way that 0.1%~0.3% antioxidant BHT is added into product, preventing tetrahydrofuran from existing
Peroxide impurity is generated during storage.
The purity of the raw material tetrahydrofuran is about 99.5%.The activated carbon fibre module, which is three, concatenated has work
Property the filtration system that constitutes of Carbon fibe, activated carbon fibre module is rendered as cylinder, high 80cm, diameter 10cm, and inside is filled with
Activated carbon fibre；Drying pillar height 1.0m, the diameter 8cm used in the drying process, inside is using anhydrous calcium oxide as drying
Agent, desiccant account for the 2/3 of dry column, and calcium oxide used is analysis carbonate-free lime.
Reduction pillar height 1.6m, the diameter 4.2cm that the in-series reduction device is used, inside is with calcium hydride and sodium borohydride
As reducing agent, the effect of reducing agent agent accounts for the 1/3 of reduction column, this reduction column also further decreases moisture content.Tetrahydrofuran is logical
The speed for crossing reduction column is 100~200mL/min, and sodium borohydride used is analysis net product.The stabilizer is BHT, chemistry
Entitled 2,6- di-tert-butyl-4-methy phenol, purity are that analysis is pure, and additive amount is 0.1%~0.3%.
Embodiment 1
A kind of purification process of chromatography pure tetrahydrofuran: purification step is:
1) it adsorbs: being 99.5%, 0.05% tetrahydrofuran raw material of moisture content with the mistake filtering velocity of 100~200mL/min by content
Degree is squeezed into filtered product in 50L glass kettle by three high 80cm, the activated carbon fibre modular filtration of diameter 10cm,
The amount of squeezing into is 30L.
2) dry: the tetrahydrofuran feed liquid after adsorption treatment is squeezed into dry in dry column, dry pillar height 1m, diameter
4.2cm, built-in desiccant are anhydrous calcium oxide, account for the 2/3 of dry column volume, 100~150mL/min of coutroi velocity, after dry
It is passed through reduction column and carries out peroxide elimination.
3) it restores: the tetrahydrofuran after drying is passed sequentially through into two high 1.6m, the concatenated sodium borohydride of diameter 8cm
And calcium hydride reduction column carries out the elimination of peroxide, 50~150mL/min of coutroi velocity.Sample after reduction is directly squeezed into
Rectifying is carried out in 50L glass rectifying still.
5) rectifying: after the tetrahydrofuran feed liquid for removing peroxide is squeezed into rectifying still, it is filled with nitrogen protection, setting is led
100~110 DEG C of hot oil temperature, 70~80 DEG C of tetrahydrofuran fluid temperature in rectifying still, control back by 65~67 DEG C of kettle top temperature
Stream discards front-end volatiles than 5:1~5, collects tetrahydrofuran finished product after the assay was approved.
6) filtering, nitrogen charging are filling: the product of collection is through selecting 0.22 micron of the foldable filter element mistake in the duct of PVDF
Filter, automatic nitrogen-charging is filling, packs 500mL.
7), acquired product purity is 99.98%, and moisture content 0.012% meets chromatography pure tetrahydrofuran index request,
It can satisfy the customer demand of chromatography pure tetrahydrofuran, every testing result of the product is shown in Table 1
Table 1: tetrahydrofuran indices testing result
Embodiment 2
A kind of purification process of chromatography pure tetrahydrofuran: purification step is:
1) it adsorbs: being 99.5%, 0.08% tetrahydrofuran raw material of moisture content with the mistake filtering velocity of 150~200mL/min by content
Degree is squeezed into filtered product in 30L glass kettle by three high 80cm, the activated carbon fibre modular filtration of diameter 10cm,
The amount of squeezing into is 20L.
4) dry: the tetrahydrofuran feed liquid after absorption is squeezed into dry in dry column, dry pillar height 1m, diameter 4.2cm,
Built-in desiccant is anhydrous calcium oxide, accounts for the 2/3 of dry column volume, and 150~200mL/min of coutroi velocity is passed through also after dry
Former column carries out peroxide elimination.
5) it restores: the tetrahydrofuran feed liquid after drying is passed sequentially through into two high 1.6m, the concatenated boron hydrogen of diameter 8cm
Change sodium and calcium hydride reduction column carries out the elimination of peroxide, 100~150mL/min of coutroi velocity.Sample after reduction is direct
It squeezes into 30L glass rectifying still and carries out rectifying.
5) rectifying: after the tetrahydrofuran for removing peroxide is entered rectifying still, it is filled with nitrogen protection, conduction oil is set
100~110 DEG C of temperature, 70~80 DEG C of tetrahydrofuran fluid temperature in rectifying still, control reflux ratio 5 by 65~67 DEG C of kettle top temperature:
1~5, front-end volatiles are discarded, collect tetrahydrofuran finished product after the assay was approved.
6) filtering, nitrogen charging are filling: the product of collection is micro- in the duct through selecting 0.22 micron of the foldable filter element of PVDF
Filter, automatic nitrogen-charging is filling, packs 500mL, and acquired product purity is 99.99%, and moisture content 0.01% meets chromatographically pure four
Hydrogen furans index request, can satisfy the customer demand of chromatography pure tetrahydrofuran, and every testing result of the product is shown in Table 2.
2 tetrahydrofuran indices testing result of table
Claims (9)
1. a kind of purification process of chromatography pure tetrahydrofuran, it is characterised in that: steps are as follows
(1) the characterization of adsorption adsorption-edulcoration of activated carbon fibre module is utilized；
(2) the peroxide in tetrahydrofuran, series connection are removed by two concatenated sodium borohydride adsorption columns and calcium hydride adsorption column
Effect is more preferable.
2. the purification process of chromatography pure tetrahydrofuran according to claim 1, it is characterised in that: specific purification process is such as
Under:
(1) to adsorb: Industrial Grade Tetrahydrofuran raw material is filtered by activated carbon fibre module, filtration flow-rate is 200~
400mL/min, the raw material after adsorption treatment enter stand-by in head tank；
(2) dry: the tetrahydrofuran feed liquid after adsorption treatment being squeezed into dry in dry column；
(3) restore: carrying out reduction treatment using the Filter column being composed in series by calcium hydride and sodium borohydride；
(4) rectifying: after the tetrahydrofuran feed liquid after reduction treatment is squeezed into rectifying still, it is filled with nitrogen protection, thermally conductive oil temperature is set
100~300 DEG C, 70~80 DEG C of tetrahydrofuran fluid temperature in rectifying still, 65~67 DEG C of kettle top temperature, control reflux ratio 5:1~
5, front-end volatiles are discarded, collect tetrahydrofuran finished product after the assay was approved；
(5) filtering, nitrogen charging are filling: product is through selecting 0.1~0.22 micron of the foldable filter element of PVDF to filter in the duct, automatically
Nitrogen charging is filling, and gained is chromatography pure tetrahydrofuran finished product；
(6) stabilizer is added: by the way that antioxidant BHT is added into product.
3. the purification process of chromatography pure tetrahydrofuran according to claim 1, it is characterised in that: the raw material tetrahydrofuran
Purity be about 99.5%.
4. the purification process of chromatography pure tetrahydrofuran according to claim 1, it is characterised in that: the activated carbon fibre mould
Block is the filtration system that three concatenated active Carbon fibes are constituted, and activated carbon fibre module is rendered as cylinder, high 80cm, directly
Diameter 10cm, inside are filled with activated carbon fibre.
5. the purification process of chromatography pure tetrahydrofuran according to claim 1, it is characterised in that: the activated carbon fibre is
After third generation activated carbon product powdered, after granular active carbon, there is excellent adsorptivity compared with ordinary granular active carbon
Can, and activated carbon fibre easily regenerates, and opposite granular active carbon is more environmentally-friendly.
6. the purification process of chromatography pure tetrahydrofuran according to claim 1, it is characterised in that: used in the drying process
Drying pillar height 1.0m, the diameter 8cm arrived, using anhydrous calcium oxide as desiccant, desiccant accounts for the 2/3 of dry column, used for inside
Calcium oxide is analysis carbonate-free lime.
7. the purification process of chromatography pure tetrahydrofuran according to claim 1, it is characterised in that: the in-series reduction device
Reduction pillar height 1.6m, the diameter 4.2cm used, using calcium hydride and sodium borohydride as reducing agent, reducing agent agent accounts for reduction for inside
The 1/3 of column, the speed that tetrahydrofuran passes through reduction column are 100~200mL/min, and sodium borohydride used is analysis net product.
8. the purification process of chromatography pure tetrahydrofuran according to claim 1, it is characterised in that: the oxidant BHT adds
Dosage is mass percent 0.1%~0.3%.
9. the purification process of chromatography pure tetrahydrofuran according to claim 1, it is characterised in that: the chromatographically pure tetrahydro furan
For the water content muttered less than 0.02%, purity 99.9%, peroxide content meets international indicator requirement, is lower than 0.015%.
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| US4461676A (en) * | 1982-07-01 | 1984-07-24 | E. I. Du Pont De Nemours And Company | Process for refining tetrahydrofuran |
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