CN100384798C - Prepn process of high purity alcohol reagent - Google Patents
Prepn process of high purity alcohol reagent Download PDFInfo
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- CN100384798C CN100384798C CNB2006101226886A CN200610122688A CN100384798C CN 100384798 C CN100384798 C CN 100384798C CN B2006101226886 A CNB2006101226886 A CN B2006101226886A CN 200610122688 A CN200610122688 A CN 200610122688A CN 100384798 C CN100384798 C CN 100384798C
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- carbon fiber
- high purity
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 title claims abstract description 57
- 239000003153 chemical reaction reagent Substances 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title abstract description 31
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical class C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 41
- -1 alcohol compound Chemical class 0.000 claims abstract description 19
- 238000005406 washing Methods 0.000 claims abstract description 16
- 150000002500 ions Chemical class 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 9
- 239000002253 acid Substances 0.000 claims abstract description 8
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000007800 oxidant agent Substances 0.000 claims abstract description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000002791 soaking Methods 0.000 claims abstract description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical group OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 27
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 19
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 19
- 239000004917 carbon fiber Substances 0.000 claims description 19
- 238000004821 distillation Methods 0.000 claims description 15
- 238000002360 preparation method Methods 0.000 claims description 15
- 150000001721 carbon Chemical class 0.000 claims description 10
- 230000004913 activation Effects 0.000 claims description 8
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 6
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 6
- 238000010521 absorption reaction Methods 0.000 claims description 6
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims description 4
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 4
- 239000001117 sulphuric acid Substances 0.000 claims description 4
- 235000011149 sulphuric acid Nutrition 0.000 claims description 4
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 150000003839 salts Chemical class 0.000 claims description 3
- 239000002594 sorbent Substances 0.000 claims description 3
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical class CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 2
- SOCTUWSJJQCPFX-UHFFFAOYSA-N dichromate(2-) Chemical compound [O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O SOCTUWSJJQCPFX-UHFFFAOYSA-N 0.000 claims description 2
- ZXEKIIBDNHEJCQ-UHFFFAOYSA-N isobutanol Chemical compound CC(C)CO ZXEKIIBDNHEJCQ-UHFFFAOYSA-N 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims 1
- 238000001179 sorption measurement Methods 0.000 abstract description 10
- 239000003463 adsorbent Substances 0.000 abstract description 2
- 229910021645 metal ion Inorganic materials 0.000 abstract description 2
- 230000001590 oxidative effect Effects 0.000 abstract 2
- 150000001768 cations Chemical class 0.000 abstract 1
- 229910052755 nonmetal Inorganic materials 0.000 abstract 1
- 239000011347 resin Substances 0.000 description 10
- 229920005989 resin Polymers 0.000 description 10
- 239000000463 material Substances 0.000 description 9
- 239000000126 substance Substances 0.000 description 7
- 229960004756 ethanol Drugs 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 241001550224 Apha Species 0.000 description 5
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 5
- 239000003729 cation exchange resin Substances 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 238000001704 evaporation Methods 0.000 description 5
- 230000008020 evaporation Effects 0.000 description 5
- 238000005194 fractionation Methods 0.000 description 5
- 150000003016 phosphoric acids Chemical class 0.000 description 5
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 description 4
- NPYPAHLBTDXSSS-UHFFFAOYSA-N Potassium ion Chemical compound [K+] NPYPAHLBTDXSSS-UHFFFAOYSA-N 0.000 description 4
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 4
- 238000000746 purification Methods 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- 229910001415 sodium ion Inorganic materials 0.000 description 4
- 238000009835 boiling Methods 0.000 description 3
- 239000000835 fiber Substances 0.000 description 3
- 239000003960 organic solvent Substances 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 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 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 125000002091 cationic group Chemical group 0.000 description 2
- 238000005342 ion exchange Methods 0.000 description 2
- 239000003456 ion exchange resin Substances 0.000 description 2
- 229920003303 ion-exchange polymer Polymers 0.000 description 2
- KMUONIBRACKNSN-UHFFFAOYSA-N potassium dichromate Chemical compound [K+].[K+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O KMUONIBRACKNSN-UHFFFAOYSA-N 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000007670 refining Methods 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 1
- OUUQCZGPVNCOIJ-UHFFFAOYSA-M Superoxide Chemical group [O-][O] OUUQCZGPVNCOIJ-UHFFFAOYSA-M 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 230000031018 biological processes and functions Effects 0.000 description 1
- 229960004424 carbon dioxide Drugs 0.000 description 1
- 229910002090 carbon oxide Inorganic materials 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 229960000935 dehydrated alcohol Drugs 0.000 description 1
- AXZAYXJCENRGIM-UHFFFAOYSA-J dipotassium;tetrabromoplatinum(2-) Chemical compound [K+].[K+].[Br-].[Br-].[Br-].[Br-].[Pt+2] AXZAYXJCENRGIM-UHFFFAOYSA-J 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000000895 extractive distillation Methods 0.000 description 1
- 125000002485 formyl group Chemical class [H]C(*)=O 0.000 description 1
- 238000013467 fragmentation Methods 0.000 description 1
- 238000006062 fragmentation reaction Methods 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 238000013178 mathematical model Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910052752 metalloid Inorganic materials 0.000 description 1
- 229910001487 potassium perchlorate Inorganic materials 0.000 description 1
- 239000012286 potassium permanganate Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910021654 trace metal Inorganic materials 0.000 description 1
- 238000005292 vacuum distillation Methods 0.000 description 1
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- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The present invention is adsorption process to eliminate micro amount of metal ion and non-metal ion from alcohol compound to obtain high purity alcohol reagent. In the process, modified carbon fiber treated with oxidant is used as the adsorbent and made to contact with distilled alcohol compound. The modified carbon fiber is treated through soaking in water solution of oxidant in 2-4 mol/L concentration at 20-60 deg.c for 2-6 hr, washing with dilute hydrochloric acid or sulfuric acid solution, washing with pure water to no acid ion, drying, and stoving at 80-250 deg.c to activate. The present invention has simple modified carbon fiber preparing process, capacity of obtaining high purity alcohol reagent with cation content in ppt level and high industrial application value.
Description
Technical field
The present invention relates to a kind of method of purification of alcohol compound, especially adopt sorbing material to remove the method for trace metal positively charged ion and metalloid anion in the alcohol compound.
Background technology
High-purity alcohol compound is because miscible with water, and boiling point is low, and is volatile, is the extensive clean-out system that uses in the production processes such as unicircuit, wafer, printed circuit plate, precision components.Also be solar cell and high tension battery important source material.High-purity alcohol compound mainly comprises low carbon chain alcohol such as methyl alcohol, ethanol and Virahol, and global annual requirement has few hundred thousand tonnes of, and also there is tens thousand of tons scale the domestic market.
The purification techniques commonly used of preparation ultra-clean and high pure chemical reagent mainly contains technology such as rectifying, distillation, sub-boiling distillation, isothermal distillation, underpressure distillation, low-temperature distillation, chemical treatment, resins exchange, film processing both at home and abroad at present.U.S. Patent Publication specification sheets US5585527 and US5571387 disclose fractionation and the isolating method of vapor permeable membrane in single container, can be used for separating alcohol for example Virahol and water.US5868906 has introduced a kind of multistage distillation tower that adopts and removed the method that moisture and boiling point are lower than any organic impurity of Virahol from contains the Virahol less than 2000ppm water.US5897750 discloses a kind of method of coming acetone, Virahol and water with extractive distillation.Chinese patent prospectus CN1417183 discloses a kind of ultrapure ethanol process for refining technology.The production equipment that this technological process mainly is made up of topping still, dealdehyder tower, treating tower, eparating methanol tower and recovery tower, realization is the ultrapure ethanol of raw material production with the raw materials for production liquid of the ethanol content 5-30% that biological process or chemical method are produced, and it mainly solves is aldehyde, ester and fusel wet goods problem in the fermenting alcohol.CN1600762 has introduced the method for the high purity methanol of rectification method preparation, and purpose is to be that the refining synthetic methanol of 95.50wt% is highly purified methyl alcohol with purity.Above-mentioned these patents mainly study to as if alcohol compound in the moisture isolation technique, and the separation method of the zwitterion of trace is not related to.
Chinese patent prospectus CN1431984 discloses the method that a kind of continuous rectification method is produced high-purity isopropanol.This method is included in from knockout tower and takes out high-purity isopropanol later on the step of high-purity isopropanol by ion exchange resin, and multistage distillation is combined with the anion-cation exchange resin treatment technology, can prepare the Virahol of positively charged ion in the ppb level.Simple multistage rectification method is restricted by capacity limit own, all has many difficulties in the high-purity alcohol compound process of preparation in equipment, technological design and production application, and also there is the too high problem of energy consumption in multistage distillation.This method provides a kind of effective means with the purifying that multistage distillation and anion-cation exchange resin adsorption technology are combined as alcohol compound, but the problem that exists is: 1, there is considerable moisture in the resin after the activated processing, and alcohol compound can have been introduced high-load moisture after by ion exchange resin.For example adopt the product moisture content of dehydrated alcohol after the gel-type anion-cation exchange resin of drying is not handled of water content 0.05% to reach 5%, product moisture content after handling through 2 hours gel-type anion-cation exchange resin of 80 ℃ of oven dry reaches 2%, and the product after handling through 2 hours gel-type anion-cation exchange resin of 100 ℃ of oven dry still has 0.5% moisture; 2, along with the drying of resin, the exchange effect of resin and exchange capacity can descend fast, and production efficiency is produced adverse influence; When 3, resin is used to handle organic solvent, have the oligopolymer dissolving of trace, especially to the processing of the organic solvent of heat, the dissolved oligopolymer is more, causes the non-volatile matter index exceeding standard; 4, the oxidation-resistance of resin is relatively poor.When there is superoxide in alcohol compound, use resin place adsorption and purification to cause oxidation fragmentation, inefficacy to resin itself.5, specific resin refers to the adsorption and purification with oxidisability ultra-clean high-purity chemicals such as hydrogen peroxide also needs to carry out in freezing conditions and antiknock device.
Summary of the invention
The objective of the invention is to overcome the above-mentioned defective of multistage rectification and multistage distillation and resin method combined method, a kind of method for preparing the high purity alcohol compound of not introducing moisture is provided.
For achieving the above object, the present invention adopts the modified carbon fiber of crossing through oxidizer treatment as sorbent material, will contact with modified carbon fiber through the alcohol reagent after the distillation to obtain high purity alcohol reagent after adsorbing; Described modified carbon fiber is in sour environment, and at 20～60 ℃, concentration is after soaking 2～6 hours in the aqueous oxidizing agent solution of 2～4mol/L with carbon fiber, with dilute hydrochloric acid or dilute sulphuric acid washing, washing to washings with pure water does not have acid ion again, and drying is again 80～250 ℃ of oven dry activation down; Described oxygenant is: nitric acid, dichromate, permanganate, the mixture of one or more in perchloric acid or its salt; Described alcohol reagent is to be liquid alcohol compound under the normal temperature and pressure.
Among the present invention, bake out temperature is preferably 120～200 ℃.Alcohol compound contacts absorption with modified carbon fiber temperature can preferably 10～75 ℃, be more preferably room temperature between 10～83 ℃.
A preferred version of aforesaid method is: alcohol reagent is flowed through and is obtained high purity alcohol reagent behind the one or more modified carbon fiber post, flow velocity can be 1～20ml/ minute/50 gram modified carbon fibers, preferably 2～10ml/ minute/50 gram modified carbon fibers are more preferably 5～10ml/ minute/50 gram modified carbon fibers.
Another preferred version of aforesaid method is: described modified carbon fiber joins in the alcohol reagent, shakes, and filter to take out modified carbon fiber and obtains high purity alcohol reagent, and the weight ratio of modified carbon fiber and alcohol compound is preferably 1: 10～and 100.
Among the present invention, alcohol reagent is methyl alcohol, ethanol, propyl alcohol, Virahol, butanols, isopropylcarbinol, the trimethyl carbinol, ethylene glycol or propylene glycol preferably.
Modified carbon fiber of the present invention is particularly a kind of porous fiber shape sorbing material of forming through 800～1000 ℃ of carbonizations of cellulose materials of organic fibre.The pore widths great majority are distributed between 0.5～1.5nm, and micro pore volume accounts for about 90% of total pore volume.Therefore, carbon fiber has very big specific surface area, is generally 800～1500m
2/ g, suitable activation condition can make specific surface area reach 3000m
2More than/the g.Carry out oxidation by oxygenant at carbon fiber surface, form the oxidation carbon-coating of one deck band portion negative charge, thereby possess absorption cationic ability, simultaneously because the carbonoxide top layer of modified carbon fiber is a covalent linkage, adsorption process is to form one on the modified carbon fiber surface to wait charge layer, in the cationic while of absorption, also will wait the negatively charged ion of electric charge to remove in the lump.Therefore the present invention adopts modified carbon fiber as negatively charged ion in the adsorbents adsorb alcohol compound and positively charged ion, can prepare the extremely low high purity alcohol compound of metal ion content easily.Use the sorbent material that lost efficacy in the back to regenerate, reuse.
This modified carbon fiber has following structure and performance advantage:
(1) both had abundant microporous and high specific surface area, contained abundant ion-exchange group again, the absorption of this sorbing material and the advantage of ion-exchange are fully played.
(2) determined that by the approximate infinitely-great characteristics of this slenderness ratio of filamentary material this modified active carbon fiber material is different with the multidimensional mass transfer characteristics of spherical ion-exchanger on reaction kinetics, can be handled with the mathematical model of approximate one dimension mass transfer.Exchange velocity is fast, and resistance drop is littler.
(3) because framework material is the carbon fibre material of handling through high temperature cabonization, its thermostability, acid and alkali-resistance, water-fast, organic solvent-resistant, anti-oxidant, erosion-resisting performance are better; Its thermal conduction capability is stronger, can prevent the danger that heat built-up caused of adsorption bed.
(4) modified carbon fiber preparation method of the present invention is simpler, and operational safety has higher industrial applications and is worth, and the index that high-purity alcohol reagent that the present invention makes can reach is as follows:
1. colourity (Apha)≤10
2. pure content 〉=99.9%
3. residue on evaporation≤1.0ppm
4. muriate (Cl
-)≤50ppb
5. nitrate (NO
3 -)≤50ppb
6. phosphoric acid salt (PO
4 3-)≤50ppb
7. vitriol (SO
4 2-)≤50ppb
8. single positively charged ion≤1.0ppb
Embodiment 1
Industrial anhydrous methanol with 99.0% adds in the fractionation plant, adds thermal distillation, and the distillate diameters that 50 gram modified carbon fibers are housed of flowing through are 50mm, are about the adsorption column of 600mm, and the control take-off rate is 2.5ml/ minute.When collection was finished, recirculation was adsorbed once, finally collects refined solution 4910mL, single treatment yield 98.20%.The index analysis result is as follows before and after handling:
| Chemical index | Before the processing | After the processing |
| Colourity (Apha) | - | ≤5 |
| Methyl alcohol | 99.90％ | 99.92％ |
| Moisture | 0.039％ | 0.031％ |
| Residue on evaporation | 25ppm | 0.09ppm |
| Muriate (Cl -) | 35ppm | 43ppb |
| Nitrate (NO 3 -) | 27ppm | 45ppb |
| Phosphoric acid salt (PO 4 3-) | 21ppm | 34ppb |
| Vitriol (SO 4 2-) | 30ppm | 34ppb |
| Sodium ion (Na +) | 6ppm | 0.90ppb |
| Potassium ion (K +) | 2ppm | 0.93ppb |
| Iron ion (Fe 3+) | 30ppm | 0.88ppb |
In the present embodiment, the treating processes of modified carbon fiber is as follows: in sour environment, with carbon fiber at room temperature, concentration is to soak in the aqueous nitric acid of 3.2mol/L after 4 hours, with the dilute hydrochloric acid washing, washs to washings with pure water and does not have acid ion, drying is again 150 ℃ of oven dry activation down.
Embodiment 2
99.0% industry anhydrous ethanol is added in the fractionation plant, add thermal distillation, the distillate diameters that 50 gram modified carbon fibers are housed of flowing through are 50mm, are about the adsorption column of 600mm, and the control take-off rate is 2.5ml/ minute.When collection was finished, recirculation was adsorbed once, finally collects refined solution 4921mL, single treatment yield 98.42%.The index analysis result is as follows before and after handling:
| Chemical index | Before the processing | After the processing |
| Colourity (Apha) | - | ≤5 |
| Ethanol | 99.87％ | 99.90％ |
| Moisture | 0.039％ | 0.033％ |
| Residue on evaporation | 39ppm | 0.09ppm |
| Muriate (Cl -) | 38ppm | 40ppb |
| Nitrate (NO 3 -) | 19ppm | 46ppb |
| Phosphoric acid salt (PO 4 3-) | 20ppm | 38ppb |
| Vitriol (SO 4 2-) | 45ppm | 37ppb |
| Sodium ion (Na +) | 4ppm | 0.91ppb |
| Potassium ion (k +) | 9ppm | 0.95ppb |
| Iron ion (Fe 3+) | 11ppm | 0.88ppb |
In the present embodiment, the modified carbon fiber treating processes is as follows: at 40 ℃, concentration is to soak in the potassium permanganate solution of 2.5mol/L after 3 hours with carbon fiber, wash with dilute hydrochloric acid, washing to washings with pure water does not have acid ion again, and drying is again 120 ℃ of oven dry activation down.
Embodiment 3
Industrial anhydrous isopropyl alcohol with 99.0% adds in the fractionation plant, adds thermal distillation, and the distillate diameters that 50 gram modified carbon fibers are housed of flowing through are 50mm, are about the adsorption column of 600mm, and the control take-off rate is 2.5ml/ minute.When collection was finished, recirculation was adsorbed once, finally collects refined solution 4925mL, single treatment yield 98.50%.The index analysis result is as follows before and after handling::
| Chemical index | Before the processing | After the processing |
| Colourity (Apha) | - | ≤5 |
| Virahol | 99.87％ | 99.91％ |
| Moisture | 0.036％ | 0.033％ |
| Residue on evaporation | 60ppm | 0.09ppm |
| Muriate (C1 -) | 39ppm | 48ppb |
| Nitrate (NO 3 -) | 35ppm | 42ppb |
| Phosphoric acid salt (PO 4 3-) | 41ppm | 37ppb |
| Vitriol (SO 4 2-) | 53ppm | 31ppb |
| Sodium ion (Na +) | 14ppm | 0.89ppb |
| Potassium ion (k +) | 23ppm | 0.92ppb |
| Iron ion (Fe 3+) | 18ppm | 0.81ppb |
In the present embodiment, the modified carbon fiber treating processes is as follows: with carbon fiber at 50 ℃, after concentration is to soak 4 hours in the potassium dichromate aqueous solution of 4mol/L, wash with dilute sulphuric acid, washing to washings with pure water does not have acid ion again, and drying is again 100 ℃ of oven dry activation down.
Embodiment 4
Industrial anhydrous tertiary butanol with 99.0% adds in the fractionation plant, adds thermal distillation, and the distillate diameters that 50 gram modified carbon fibers are housed of flowing through are 50mm, are about the adsorption column of 600mm, and the control take-off rate is 5ml/ minute.When collection was finished, recirculation was adsorbed once, finally collects refined solution 4923mL, single treatment yield 98.46%.The index analysis result is as follows before and after handling:
| Chemical index | Before the processing | After the processing |
| Colourity (Apha) | - | ≤5 |
| Virahol | 99.86％ | 99.83％ |
| Moisture | 0.038％ | 0.037％ |
| Residue on evaporation | 59ppm | 0.089ppm |
| Muriate (Cl -) | 41ppm | 68ppb |
| Nitrate (NO 3 -) | 30ppm | 52ppb |
| Phosphoric acid salt (PO 4 3-) | 40ppm | 47ppb |
| Vitriol (SO 4 2-) | 33ppm | 41ppb |
| Sodium ion (Na +) | 11ppm | 1.9ppb |
| Potassium ion (k +) | 18ppm | 1.8ppb |
| Iron ion (Fe 3+) | 19ppm | 0.9ppb |
In the present embodiment, the modified carbon fiber treating processes is as follows: with carbon fiber at 40 ℃, after concentration is to soak 4 hours in the potassium perchlorate aqueous solution of 2.3mol/L, wash with dilute sulphuric acid, washing to washings with pure water does not have acid ion again, and drying is again 100 ℃ of oven dry activation down.
Claims (10)
1. the preparation method of a high purity alcohol reagent is characterized in that, adopts the modified carbon fiber of crossing through oxidizer treatment as sorbent material, will contact with modified carbon fiber through the alcohol reagent after the distillation to obtain high purity alcohol reagent after adsorbing; Described modified carbon fiber is in sour environment, and at 20～60 ℃, concentration is after soaking 2～6 hours in the aqueous oxidizing agent solution of 2～4mol/L with carbon fiber, with dilute hydrochloric acid or dilute sulphuric acid washing, washing to washings with pure water does not have acid ion again, and drying is again 80～250 ℃ of oven dry activation down; Described oxygenant is: nitric acid, dichromate, permanganate, the mixture of one or more in perchloric acid or its salt; Described alcohol reagent is to be liquid alcohol compound under the normal temperature and pressure.
2. according to the preparation method of the described high purity alcohol reagent of claim 1, it is characterized in that described oxygenant is nitric acid, permanganate, the mixture of one or more in perchloric acid or its salt.
3. according to the preparation method of the described high purity alcohol reagent of claim 1, it is characterized in that described oven dry activation temperature is 120～200 ℃.
4. according to the preparation method of the described high purity alcohol reagent of claim 1, it is characterized in that described alcohol reagent contacts temperature 10-83 ℃ of absorption with modified carbon fiber.
5. according to the preparation method of the described high purity alcohol reagent of claim 4, it is characterized in that described alcohol reagent contacts temperature 10-75 ℃ of absorption with modified carbon fiber.
6. according to the preparation method of the described high purity alcohol reagent of claim 1, it is characterized in that described alcohol reagent is flowed through and obtained high purity alcohol reagent behind the one or more modified carbon fiber post, flow velocity is 1～20ml/ minute/50 gram modified carbon fibers.
7. according to the preparation method of the described high purity alcohol reagent of claim 1, it is characterized in that described modified carbon fiber joins in the alcohol reagent, stir, filter the taking-up modified carbon fiber and obtain high purity alcohol reagent, the weight ratio of modified carbon fiber and alcohol reagent is 1: 10～100.
8. according to the preparation method of the described high purity alcohol reagent of claim 6, it is characterized in that the flow through flow velocity of modified carbon fiber post of described alcohol reagent is 2～10ml/ minute/50 gram modified carbon fibers.
9. according to the preparation method of the described high purity alcohol reagent of claim 1, it is characterized in that described alcohol reagent is methyl alcohol, ethanol, propyl alcohol, Virahol, butanols, isopropylcarbinol, the trimethyl carbinol, ethylene glycol or propylene glycol.
10. the preparation method of described high purity alcohol reagent according to Claim 8 is characterized in that, the flow through flow velocity of modified carbon fiber post of described alcohol reagent is 5～10ml/ minute/50 gram modified carbon fibers.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006101226886A CN100384798C (en) | 2006-10-13 | 2006-10-13 | Prepn process of high purity alcohol reagent |
Applications Claiming Priority (1)
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| CN102060663A (en) * | 2009-11-18 | 2011-05-18 | 天津市康科德科技有限公司 | Method for preparing chromatographic pure isopropanol |
| CN102942447B (en) * | 2012-10-13 | 2015-09-30 | 江苏盈天化学有限公司 | A kind of process for purification of electronic-grade isopropanol recovering liquid |
| CN106029197B (en) * | 2013-10-08 | 2019-05-28 | 英国石油有限公司 | The processing of alcohol composition |
| CN105085175B (en) * | 2015-09-15 | 2017-11-17 | 华烁科技股份有限公司 | A kind of refining agent and process for purification of coal polymer grade ethylene glycol |
Citations (2)
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| US5726118A (en) * | 1995-08-08 | 1998-03-10 | Norit Americas, Inc. | Activated carbon for separation of fluids by adsorption and method for its preparation |
| CN1607973A (en) * | 2001-10-31 | 2005-04-20 | 霍尼韦尔国际公司 | Purification of organic solvents |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5726118A (en) * | 1995-08-08 | 1998-03-10 | Norit Americas, Inc. | Activated carbon for separation of fluids by adsorption and method for its preparation |
| CN1607973A (en) * | 2001-10-31 | 2005-04-20 | 霍尼韦尔国际公司 | Purification of organic solvents |
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| .化学世界，第（2）期. 2001 |
| 碳纤维的硝酸氧化及表面化学分析. 盛宏恩等 |
| 碳纤维的硝酸氧化及表面化学分析. 盛宏恩等；.化学世界，第（2）期. 2001 * |
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