CN101503866A - Solvent recovery method in cellulosic fiber preparation with ionic liquid as solvent - Google Patents
Solvent recovery method in cellulosic fiber preparation with ionic liquid as solvent Download PDFInfo
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- CN101503866A CN101503866A CNA2009100145565A CN200910014556A CN101503866A CN 101503866 A CN101503866 A CN 101503866A CN A2009100145565 A CNA2009100145565 A CN A2009100145565A CN 200910014556 A CN200910014556 A CN 200910014556A CN 101503866 A CN101503866 A CN 101503866A
- Authority
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- Prior art keywords
- solvent
- ionic liquid
- recovery method
- cellulose fibre
- solution
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- 239000002608 ionic liquid Substances 0.000 title claims abstract description 42
- 239000002904 solvent Substances 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 238000011084 recovery Methods 0.000 title claims description 21
- 239000000835 fiber Substances 0.000 title description 2
- 229920003043 Cellulose fiber Polymers 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000012535 impurity Substances 0.000 claims abstract description 9
- 239000007787 solid Substances 0.000 claims abstract description 9
- 239000012528 membrane Substances 0.000 claims abstract description 6
- 238000001223 reverse osmosis Methods 0.000 claims abstract description 6
- 150000002500 ions Chemical class 0.000 claims description 25
- 239000006193 liquid solution Substances 0.000 claims description 17
- 238000004821 distillation Methods 0.000 claims description 11
- FHDQNOXQSTVAIC-UHFFFAOYSA-M 1-butyl-3-methylimidazol-3-ium;chloride Chemical compound [Cl-].CCCCN1C=C[N+](C)=C1 FHDQNOXQSTVAIC-UHFFFAOYSA-M 0.000 claims description 10
- 230000006837 decompression Effects 0.000 claims description 10
- 239000012141 concentrate Substances 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 6
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 238000001914 filtration Methods 0.000 abstract description 2
- 238000009833 condensation Methods 0.000 abstract 1
- 230000005494 condensation Effects 0.000 abstract 1
- 239000002245 particle Substances 0.000 abstract 1
- 239000007788 liquid Substances 0.000 description 8
- 238000009987 spinning Methods 0.000 description 8
- 229920002678 cellulose Polymers 0.000 description 7
- 235000010980 cellulose Nutrition 0.000 description 7
- 239000001913 cellulose Substances 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- 239000003153 chemical reaction reagent Substances 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 238000004064 recycling Methods 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- QGJOPFRUJISHPQ-UHFFFAOYSA-N Carbon disulfide Chemical compound S=C=S QGJOPFRUJISHPQ-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000000701 coagulant Substances 0.000 description 3
- 238000007380 fibre production Methods 0.000 description 3
- 238000004448 titration Methods 0.000 description 3
- 238000002166 wet spinning Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 229920000742 Cotton Polymers 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 230000036541 health Effects 0.000 description 2
- IQQRAVYLUAZUGX-UHFFFAOYSA-N 1-butyl-3-methylimidazolium Chemical compound CCCCN1C=C[N+](C)=C1 IQQRAVYLUAZUGX-UHFFFAOYSA-N 0.000 description 1
- 241000894006 Bacteria Species 0.000 description 1
- 235000017166 Bambusa arundinacea Nutrition 0.000 description 1
- 235000017491 Bambusa tulda Nutrition 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 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 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 244000082204 Phyllostachys viridis Species 0.000 description 1
- 235000015334 Phyllostachys viridis Nutrition 0.000 description 1
- 239000004793 Polystyrene Substances 0.000 description 1
- 240000008042 Zea mays Species 0.000 description 1
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 1
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 239000011425 bamboo Substances 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000001112 coagulating effect Effects 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 235000005822 corn Nutrition 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 230000035800 maturation Effects 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000005120 petroleum cracking Methods 0.000 description 1
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 1
- 229920001083 polybutene Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000004926 polymethyl methacrylate Substances 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 230000028327 secretion Effects 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-L sulfite Chemical compound [O-]S([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-L 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 1
- 229960001763 zinc sulfate Drugs 0.000 description 1
- 229910000368 zinc sulfate Inorganic materials 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/10—Greenhouse gas [GHG] capture, material saving, heat recovery or other energy efficient measures, e.g. motor control, characterised by manufacturing processes, e.g. for rolling metal or metal working
Abstract
The invention discloses a method for reclaiming solvent in cellulose fiber preparation taking ionic liquid as the solvent, which comprises the following steps: filtering solution containing the ionic liquid to remove solid particle impurities; performing film condensation by a reverse osmosis membrane; and distilling the condensed solution containing the ionic liquid under reduced pressure to make the mass content of water in the solution containing the ionic liquid less than or equal to 2 percent, and obtaining the reclaimed ionic liquid. The method is suitable for reclaiming the solution containing the ionic liquid in wide concentration range, and has low energy consumption and easy implementation.
Description
Technical field
The present invention relates to a kind of recovery of purifying is the ion liquid method that produces in the cellulose fibre preparation process of solvent with the ionic liquid.
Background technology
Cellulose is a kind of renewable resource, is prevalent in the Nature.All contain a large amount of celluloses in the secretion of plants such as trees, cotton, rice bar, corn and some bacteriums.Cellulose fibre may become the renewable resource that replaces the petroleum cracking fiber product.The production of cellulose fibre at present mainly adopts NaOH, acetone, carbon disulfide etc. as solvent and auxiliary agent, and need carry out yellow, experienced and maturation to used cellulose, relate to chemical reagent such as formaldehyde, sulphite, vulcanized sodium, sulfuric acid and zinc sulfate again, all above-mentioned organic reagents all have volatility, the health that environment is caused serious pollution and jeopardizes operating personnel; And inorganic reagent all has severe corrosive, and is very big to the corrosion of equipment.In addition, the recovery of these chemical reagent not only technological process is loaded down with trivial details, strict to control of process parameters, and can produce a large amount of waste gas and waste water, again environment is caused severe contamination.
Ionic liquid at room temperature is compared with conventional solvent, and the boiling point height is non-volatile, exists with liquid state in wider temperature range, and good heat endurance is arranged; Can change its physicochemical properties by the combination of the yin, yang ion selecting to suit, be the good solvent of many organic matters, inorganic matter and macromolecular material.Ionic liquid is widely used in electrochemistry, organic synthesis, catalysis as a kind of green solvent and the field such as separates, and also is the good solvent of many macromolecular polymerization reactions and processing simultaneously, as poly-to benzene, polybutene, polymethyl methacrylate, polystyrene etc.United States Patent (USP) 20020010291 discloses a kind of method of making each high molecular polyisoolefines in ionic liquid, United States Patent (USP) 20030157351 discloses a kind of cellulose and has dissolved and method for processing in ionic liquid, and Chinese patent CN 1596282A discloses the method that adopts ion liquid dissolving and processing of cellulose.
Very big as ionic liquid [BMIM] Cl comparatively commonly used and [AMIM] Cl to cellulosic solubility, can reach 35% (mass percent), but when cellulosic concentration greater than 8% the time, solution viscosity sharp increase presents gel, is difficult to carry out spinning process.Adopt the ionic liquid cellulose solution of low concentration, both guaranteed the dissolubility of cellulose in ionic liquid, also guaranteed the machinability of spinning solution.
But ion liquid synthetic and purifying process complexity, the production cost height, especially as [BMIM] Cl and [AMIM] Cl of using in the cellulose fibre preparation, therefore the normal mode that the ionic liquid after using in the cellulose fibre production is carried out recycling that adopts, avoid waste, to reduce production costs.Patent 200510108024.X discloses a kind of way of recycling that adopts extracting process to reclaim hydrophobicity and hydrophilic ionic-liquid, and some adopt the distillation mode to reclaim ion liquid mode, but above-mentioned way of recycling, only be applicable under the lower situation of the content of water in the ionic liquid after cellulose fibre production is used and carry out ion liquid recovery, in the back ionic liquid is used in cellulose fibre production under the higher situation of content of water, it is higher that the employing aforesaid way carries out ion liquid recovery energy consumption, is difficult for carrying out.
Summary of the invention
It is method for recovering solvents in the cellulose fibre preparation process of solvent with the ionic liquid that technical problem to be solved by this invention is to provide a kind of, this method is suitable for reclaiming the ion liquid solution that contains in the big concentration range, to overcome the defective that prior art exists, and energy consumption is low, easily implements.
Of the present invention is the recovery method of solvent in the cellulose fibre preparation of solvent with the ionic liquid, may further comprise the steps:
1) will contain ion liquid solution and filter, remove solid granular impurity; After produce using, the solution that will contain ionic liquid and solid impurity filters, and removes solid granular impurity wherein, and the filter material of making as 80 white poplins that can use 1～3 layer filters;
2) the one-level film concentrates to utilize reverse osmosis membrane to carry out at least, and making the mass content that contains water in the ion liquid solution is 70%～85%; Preferably can be in 10 ℃～95 ℃ temperature range, utilizing the aperture is that the film of 15.0～50.0 nanometers carries out film and concentrates, and can carry out the primary, secondary, tertiary or multi-level film and concentrate, to reach production requirement according to practical condition;
3) the ion liquid solution that contains after concentrating is carried out decompression distillation, make mass content≤2% that contains water in the ion liquid solution; Preferably under the temperature conditions of the pressure condition of 10～1000Pa and 95～130 ℃, carry out decompression distillation.
And, be that the recovery method intermediate ion liquid of solvent in the cellulose fibre preparation of solvent is meant at least a among [BMIM] Cl and [AMIM] Cl with the ionic liquid in the present invention.
The invention has the advantages that:
The filter material that uses when (1) removing solid impurity is 80 white poplins, and cost is low, easy to operate, and white poplin is reusable;
(2) adopt film to concentrate and recoverys of purifying of two step of decompression distillation staircase method, reduced the high problem of employing decompression distillation energy consumption when low concentration content ionic liquid purified.And film is reusable.
(3) solvent that is adopted is an ionic liquid, and nontoxic, non-volatility helps environmental protection and operator ' s health;
(4) owing to the ionic liquid non-volatility, vapour pressure approaches zero, so recovery process is simple, has reduced production cost, has saved the resource and the energy;
(5) ionic liquid rate of recovery height, the recycling rate of waterused height.
The specific embodiment
Below in conjunction with the specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Embodiment 1
With [BMIM] Cl of mass content 100% as solvent, the spinning solution solution of preparation cotton pulp mass content 8% carries out wet spinning, use water as coagulating agent, after spinning a period of time, from solidifying water-bath taking-up 10000g temperature is 93 ℃ of solution that contain [BMIM] Cl, learns behind the chemistry titration that it is 2.7g that this 10000g solution includes ionic liquid [BMIM] Cl;
10000g solution is filtered, remove solid granular impurity wherein;
After filtering, fluid temperature drops to 75 ℃, and utilizing the aperture is that the reverse osmosis membrane of 20 nanometers carries out 3 grades of films and concentrates, and must contain ion liquid solution quality is 115g;
Under the condition of 300Pa, 125 ℃ of decompression distillation 2 hours, finally obtain quality content and be 0.8% contain ionic liquid solution 22.5g, the ionic liquid rate of recovery is 98.33%.
Embodiment 2
With [BMIM] Cl and [AMIM] Cl mol ratio is that the ionic liquid mixed liquor of 8:2 is as solvent, the spinning solution solution of preparation pulp quality content 5% carries out wet spinning, use water as coagulating agent, after spinning a period of time, taking out the 10000g temperature from water-bath is 90 ℃ of solution that contain [BMIM] Cl and [AMIM] Cl, learns behind the chemistry titration that this 10000g solution includes ionic liquid [BMIM] Cl30.7g;
Is that 80 white poplins of 1 layer filter with 10000g solution through filter material, removes solid granular impurity wherein;
After white poplin filtered, solution temperature dropped to 70 ℃, and utilizing the aperture is that the reverse osmosis membrane of 16 nanometers carries out 1 grade of film and concentrates, and containing ion liquid solution quality is 118g;
Under the condition of 70Pa, 106 ℃ of decompression distillation 4 hours finally obtain quality content and are 1.5% the ion liquid solution 30.9g that contains, and the rate of recovery is 99.14%.
Embodiment 3
Use mass content 100%[AMIM] ionic liquid of Cl is as solvent, the spinning solution solution of preparation bamboo pulp mass content 9% carries out wet spinning, use water as coagulating agent, after spinning a period of time, taking out the 10000g temperature from the water coagulating bath is 90 ℃ of solution that contain [AMIM] Cl, learns behind the chemistry titration that it is 39.5g that this 10000g solution includes ionic liquid [BMIM] Cl;
Is that 80 white poplins of 3 layers filter with 10000g solution through filter material, removes solid granular impurity wherein;
After white poplin filtered, solution temperature dropped to 65 ℃, and utilizing the aperture is that the film of 40 nanometers carries out 3 grades of films and concentrates, and containing ion liquid solution quality is 263g;
Under the condition of 800Pa, 96 ℃ of decompression distillation 5 hours, finally obtaining moisture is 2% the ion liquid solution 39.7g that contains, the rate of recovery is 98.50%.
Claims (6)
1, be the recovery method of solvent in the cellulose fibre preparation of solvent with the ionic liquid, it is characterized in that this recovery method may further comprise the steps:
1) will contain ion liquid solution and filter, remove solid granular impurity;
2) utilize reverse osmosis membrane to carry out at least the one-level film and concentrate, to the mass content that contains water in the ion liquid solution be 70%～85%;
3) the ion liquid solution that contains after concentrating is carried out decompression distillation, to the mass content that contains water in the ion liquid solution≤2%.
2, as claimed in claim 1 is the recovery method of solvent in the cellulose fibre preparation of solvent with the ionic liquid, it is characterized in that: described ionic liquid is meant at least a among [BMIM] Cl and [AMIM] Cl.
3, as claimed in claim 1 is the recovery method of solvent in the cellulose fibre preparation of solvent with the ionic liquid, it is characterized in that: when containing ion liquid solution and filter, the filter material of use is 80 public white poplins of 1～3 layer.
4, as claimed in claim 1 is the recovery method of solvent in the cellulose fibre preparation of solvent with the ionic liquid, it is characterized in that: utilize reverse osmosis membrane to carry out film when concentrating, the aperture of film is 15.0～50.0 nanometers, and temperature range is 10 ℃～95 ℃.
5, as claimed in claim 1 is the recovery method of solvent in the cellulose fibre preparation of solvent with the ionic liquid, and it is characterized in that: the ion liquid solution that contains after concentrating is carried out decompression distillation, is to carry out under the pressure condition of 10～1000Pa.
6, as in the claim 1 to 5 each described be the recovery method of solvent in the cellulose fibre preparation of solvent with the ionic liquid, it is characterized in that: the ion liquid solution that contains after concentrating is carried out decompression distillation, is to carry out under 95～130 ℃ temperature conditions.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2009100145565A CN101503866A (en) | 2009-03-07 | 2009-03-07 | Solvent recovery method in cellulosic fiber preparation with ionic liquid as solvent |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2009100145565A CN101503866A (en) | 2009-03-07 | 2009-03-07 | Solvent recovery method in cellulosic fiber preparation with ionic liquid as solvent |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101503866A true CN101503866A (en) | 2009-08-12 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2009100145565A Pending CN101503866A (en) | 2009-03-07 | 2009-03-07 | Solvent recovery method in cellulosic fiber preparation with ionic liquid as solvent |
Country Status (1)
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|---|---|
| CN (1) | CN101503866A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102167465A (en) * | 2011-03-17 | 2011-08-31 | 天津工业大学 | Recovery method of spinning waste liquor by means of concentrating |
| CN103147169A (en) * | 2013-03-26 | 2013-06-12 | 宏远纺织科技（泉州）有限公司 | Method for recycling spinning ionic liquid through adopting activated carbon |
| CN103147331A (en) * | 2013-03-08 | 2013-06-12 | 南开大学 | Method for extracting biomass cellulose of lignocellulose by using imidazolium ionic liquid |
| CN106149101A (en) * | 2016-08-09 | 2016-11-23 | 东华大学 | A kind of ion double solvents recovery method for cellulose spinning |
| CN107287700A (en) * | 2016-03-31 | 2017-10-24 | 东莞新科技术研究开发有限公司 | The recovery method of ionic liquid |
| CN109836606A (en) * | 2019-01-31 | 2019-06-04 | 华中科技大学鄂州工业技术研究院 | A kind of clean method for preparing of controlled pore cellulose products |
-
2009
- 2009-03-07 CN CNA2009100145565A patent/CN101503866A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102167465A (en) * | 2011-03-17 | 2011-08-31 | 天津工业大学 | Recovery method of spinning waste liquor by means of concentrating |
| CN103147331A (en) * | 2013-03-08 | 2013-06-12 | 南开大学 | Method for extracting biomass cellulose of lignocellulose by using imidazolium ionic liquid |
| CN103147331B (en) * | 2013-03-08 | 2015-05-13 | 南开大学 | Method for extracting biomass cellulose of lignocellulose by using imidazolium ionic liquid |
| CN103147169A (en) * | 2013-03-26 | 2013-06-12 | 宏远纺织科技（泉州）有限公司 | Method for recycling spinning ionic liquid through adopting activated carbon |
| CN103147169B (en) * | 2013-03-26 | 2015-04-08 | 宏远纺织科技（泉州）有限公司 | Method for recycling spinning ionic liquid through adopting activated carbon |
| CN107287700A (en) * | 2016-03-31 | 2017-10-24 | 东莞新科技术研究开发有限公司 | The recovery method of ionic liquid |
| CN106149101A (en) * | 2016-08-09 | 2016-11-23 | 东华大学 | A kind of ion double solvents recovery method for cellulose spinning |
| CN109836606A (en) * | 2019-01-31 | 2019-06-04 | 华中科技大学鄂州工业技术研究院 | A kind of clean method for preparing of controlled pore cellulose products |
| CN109836606B (en) * | 2019-01-31 | 2022-05-20 | 华中科技大学鄂州工业技术研究院 | Clean manufacturing method of controllable porous cellulose product |
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Open date: 20090812 |