CN103657419A - Process for recovering alkali by double-membrane separation method in chemical fiber production - Google Patents
Process for recovering alkali by double-membrane separation method in chemical fiber production Download PDFInfo
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- CN103657419A CN103657419A CN201310656576.9A CN201310656576A CN103657419A CN 103657419 A CN103657419 A CN 103657419A CN 201310656576 A CN201310656576 A CN 201310656576A CN 103657419 A CN103657419 A CN 103657419A
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- alkali
- membrane separation
- separation device
- membrane
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- 239000012528 membrane Substances 0.000 title claims abstract description 63
- 239000003513 alkali Substances 0.000 title claims abstract description 56
- 238000000034 method Methods 0.000 title claims abstract description 28
- 238000000926 separation method Methods 0.000 title claims abstract description 25
- 239000000126 substance Substances 0.000 title claims abstract description 8
- 238000007380 fibre production Methods 0.000 title abstract description 6
- 239000000919 ceramic Substances 0.000 claims abstract description 25
- 238000001728 nano-filtration Methods 0.000 claims abstract description 20
- 229920002488 Hemicellulose Polymers 0.000 claims abstract description 15
- 229920000297 Rayon Polymers 0.000 claims abstract description 14
- 238000011084 recovery Methods 0.000 claims abstract description 8
- 239000012535 impurity Substances 0.000 claims abstract description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical group [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 27
- 239000000463 material Substances 0.000 claims description 13
- 238000004519 manufacturing process Methods 0.000 claims description 12
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 7
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 7
- 239000000835 fiber Substances 0.000 claims description 6
- 238000005516 engineering process Methods 0.000 abstract description 4
- 238000001471 micro-filtration Methods 0.000 abstract description 3
- 239000002253 acid Substances 0.000 abstract description 2
- 238000005265 energy consumption Methods 0.000 abstract description 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Inorganic materials [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 54
- 235000011121 sodium hydroxide Nutrition 0.000 description 25
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 6
- 239000012530 fluid Substances 0.000 description 6
- 239000007788 liquid Substances 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 229920002678 cellulose Polymers 0.000 description 4
- 239000001913 cellulose Substances 0.000 description 4
- 238000000502 dialysis Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 230000000149 penetrating effect Effects 0.000 description 4
- 239000002699 waste material Substances 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000007598 dipping method Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 230000004907 flux Effects 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- 229920004933 Terylene® Polymers 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 239000005020 polyethylene terephthalate Substances 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000000108 ultra-filtration Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
- Y02P70/62—Manufacturing or production processes characterised by the final manufactured product related technologies for production or treatment of textile or flexible materials or products thereof, including footwear
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- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention provides a process for recovering alkali by a double-membrane separation method in chemical fiber production, which comprises the steps of pretreating alkali liquor discharged from a squeezing working section by a ceramic microfiltration membrane separation device to remove macromolecular impurities in the alkali liquor; and purifying the treated alkali liquor by a ceramic nanofiltration membrane separation device, wherein the purified alkali liquor can be directly reused for viscose fiber production. After the treatment by the process, the alkali concentration of the alkali liquor is 120-250g/L, and the hemicellulose content is less than 5 g/L. According to the characteristics of high-concentration alkali liquor in the viscose fiber production process, the invention adopts the combined technology of the ceramic microfiltration membrane and the ceramic nanofiltration membrane with excellent acid and alkali resistance to purify and recover the alkali liquor, and has the advantages of low energy consumption, high alkali recovery rate, stable operation, long service life and the like.
Description
Technical field:
The present invention relates to the recovery process of press lye in viscose rayon manufacture, also relate to ceramic membrane application technology simultaneously.
Technical background:
Viscose rayon is the important kind that is only second to terylene in China's chemical fibre industry.Viscose fiber production process in dipping workshop section, adds production of high concentration caustic soda solution in pulp, and cellulose and caustic soda effect, generate alkali cellulose; Pulp expands simultaneously, makes hemicellulose and other impurity stripping in pulp, and in squeezing section, uses plate and frame filter press to carry out squeeze and filter to alkali cellulose, obtains solid base cellulose to produce for next step; Filter liquor is the alkali lye that is dissolved with hemicellulose, and it is high that this part has COD containing alkali waste water, and turbidity is large, alkali content high, and direct processing discharge need to consume a large amount of acid and neutralize, and also causes the pollution in bad border and the waste of resource simultaneously.
Industrial general use dialysis is removed the hemicellulose in alkali lye, and gained alkali lye can be back to the reuse of dipping workshop section, and its idiographic flow is shown in Fig. 1, but the recycle of alkali liquor inefficiency of dialysis, and water consumption is large, and takies larger construction area.Have in recent years bibliographical information to use organic nanofiltration membrane to filter rear reuse to the soda bath after using, as shown in Figure 2, organic nanofiltration membrane waits composition to have to half fibre in spent lye and well holds back idiographic flow, and the alkali lye after filtration can be used in reuse completely; But the alkali resistance of organic film is poor, and the life-span is shorter, cause the rising of process costs.
Patent 03116940.6, name is called the patent of invention of " a kind of alkali and organic method of reclaiming from pulp waste liquid ", discloses a kind of alkali and organic method of reclaiming from pulp waste liquid.This invention comprises the steps: that be 20-60 ℃ by pulp waste liquid in temperature, and pressure is under the operating condition of 1.5-3.0 MPa, and through NF membrane separator isolated by filtration, obtaining organic concentration is the trapped fluid of 90 grams per liters and the liquid that sees through that contains NaOH; The liquid that sees through that contains NaOH can be used for pulp production; Contain organic trapped fluid evaporation and concentration, by follow-up modified technique, prepare high value added product.This patent does not take into full account the particularity of the chemical composition in viscose fiber spent lye, adopts conventional pretreatment mode, causes this technique alkali recovery low, the shortcoming such as film service life is short.
Ceramic membrane refers to a kind of pellicle prepared by materials such as adopting aluminium oxide, titanium oxide, silica, zirconia, can prepare at present the film of micro-filtration, ultrafiltration and nanofiltration equal aperture scope.Than organic film, ceramic membrane has the advantages such as chemical stability is good, mechanical strength is large, anti-microbe ability is strong, high temperature resistant, has been widely used in the fields such as environment-protecting industrial, food industry and biochemical and pharmaceuticals industry.
Summary of the invention:
The present invention is directed to the problems referred to above, proposed the technique of two membrane separation processes recovery alkali in a kind of chemical fibre production.Its technological process is as shown in Figure 3: the alkali lye of discharging in squeezing section is first carried out to pretreatment through ceramic micro filter membrane separation device, remove the large molecular impurity in alkali lye; Alkali lye after processing passes through nanofiltration membrane separation device purifying again, the alkali lye after purifying can direct reuse in the production of viscose rayon.After above-mentioned PROCESS FOR TREATMENT, the alkali concn of alkali lye is 120-250g/L, and hemicellulose level is less than 5g/L.The present invention is according to the feature of production process of viscose fiber middle and high concentration alkali lye, adopt superior ceramic micro filter film and the nanofiltration membrane GC-MS of acid-proof alkaline, alkali lye is carried out to purifying recovery, have that energy consumption is low, alkali recovery is high, stable, the advantages such as long service life.
Described alkali lye is the alkali lye that during viscose rayon is produced, squeezing section produces, and wherein contains alkali concn at 120-250g/l, and half fine content is between 25-40g/l, and other impurity on a small quantity.
In described ceramic micro filter membrane separation device, membrane material is aluminium oxide, titanium oxide, zirconic a kind of or its combination, and aperture is between 0.1-1um, and operating temperature is 40-50 ℃, and operating pressure is 2-5bar.
Described nanofiltration membrane material is aluminium oxide, titanium oxide, zirconic a kind of or its combination, and the aperture of nanofiltration membrane is 1-2nm, and operating parameter is: temperature is between 30-60 ℃, and operating pressure is between 10-20bar, and crossflow velocity is between 3-5m/s.
Described ceramic micro filter film and nanofiltration membrane component are single tube or multichannel.
Key of the present invention is to have used ceramic membrane to filter alkali lye, than organic polymer films, the acid-fast alkali-proof of ceramic membrane excellence and resistance to elevated temperatures, make ceramic membrane have good rejection effect to hemicellulose, also there is higher flux and longer life-span simultaneously, greatly reduce production cost; Adopt innovatively ceramic micro filter film preconditioning technique, reduced the impurity of the feed liquor of nanofiltration film device, further increased flux and the cutoff performance of NF membrane, improved production efficiency.
Accompanying drawing explanation:
Fig. 1 is the outline flowchart of dialysis technique;
Fig. 2 is the outline flowchart of organic film separating technology;
Fig. 3 is process chart of the present invention.
The specific embodiment:
Process chart described in 1 the present embodiment is as shown in Figure 1: by squeezing section alkali lye (alkali content 128g/l out; Hemicellulose level is 25.1g/l) under 40 ℃, 2bar condition through 19 passage ceramic micro filter membrane separation device (aperture 0.2um, membrane material is aluminium oxide), (membrane aperture is 1.2nm to enter afterwards 19 passage nanofiltration membrane separation devices again, membrane material is aluminium oxide), control operation temperature is 35 ℃, permeable membrane pressure reduction is 16bar, and crossflow velocity is 4m/s; The penetrating fluid water white transparency obtaining, alkali content 124g/L, hemicellulose level is 3.7g/l, can be back to viscose rayon production workshop section.
2 by squeezing section alkali lye (alkali content 140g/l out; Hemicellulose level is 26.7g/l) under 45 ℃, 3bar condition through 19 passage ceramic micro filter membrane separation device (aperture 0.5um, membrane material is titanium oxide), (membrane aperture is 1.2nm to enter afterwards 19 passage nanofiltration membrane separation devices, membrane material is aluminium oxide), control operation temperature is 55 ℃, permeable membrane pressure reduction is 16bar, and crossflow velocity is 4m/s; The penetrating fluid water white transparency obtaining, alkali content 136g/l, hemicellulose level is 4.8g/l, can be back to viscose rayon production workshop section.
3 by squeezing section alkali lye (alkali content 156g/l out; Hemicellulose level is 32.7g/l) under 45 ℃, 5bar condition through single hose ceramic micro filter membrane separation device (aperture 1um, membrane material is zirconia), (membrane aperture is 1.8nm to enter afterwards single hose nanofiltration membrane separation device, membrane material is titanium oxide), control operation temperature is 45 ℃, permeable membrane pressure reduction is 10bar, and crossflow velocity is 3m/s; The penetrating fluid water white transparency obtaining, alkali content 153g/l, hemicellulose level is 4.9g/l, can be back to viscose rayon production workshop section.
4 by squeezing section alkali lye (alkali content 162g/l out; Hemicellulose level is 34.29g/l) under 50 ℃, 5bar condition through 19 passage ceramic micro filter membrane separation device (aperture 0.5um, membrane material is aluminium oxide), (membrane aperture is 1.8nm to enter afterwards single hose nanofiltration membrane separation device, membrane material is zirconia), control operation temperature is 45 ℃, permeable membrane pressure reduction is 10bar, and crossflow velocity is 5m/s; The penetrating fluid water white transparency obtaining, alkali content 156g/l, hemicellulose level is 5g/l, can be back to viscose rayon production workshop section.
Table 1 is the treatment effect of three kinds of techniques, and contrast finds, technology all has obvious advantage with respect to dialysis technique and organic film technique described in this patent.
The treatment effect of each technique of table 1
Claims (6)
1. a technique for chemical fibre two membrane separation processes recovery alkali in producing, is characterized in that using ceramic micro filter membrane separation device to carry out pretreatment to press lye, removes the large molecular impurity in alkali lye; Alkali lye after processing enters nanofiltration membrane separation device purifying again, and NF membrane is by the hemicellulose of holding back wherein, and the alkali lye direct reuse infiltrating is in the production of viscose rayon.
2. technique as described in claim 1, the material that it is characterized in that the ceramic micro filter film in ceramic micro filter membrane separation device is aluminium oxide, titanium oxide or zirconic a kind of or its combination; Ceramic micro filter membrane aperture is between 0.1-1um.
3. technique as described in claim 1, is characterized in that pretreated operating temperature is 40-50 ℃, and operating pressure is 2-5bar.
4. technique as described in claim 1, the material that it is characterized in that the NF membrane in nanofiltration membrane separation device is aluminium oxide, titanium oxide or zirconic a kind of or its combination, the aperture of NF membrane is between 1-2nm.
5. technique as described in claim 1, the operating temperature that it is characterized in that nanofiltration membrane separation device purifying is 30-60 ℃, operating pressure is 10-20bar, crossflow velocity 3-5m/s.
6. technique as described in claim 1, is characterized in that ceramic micro filter in ceramic micro filter membrane separation device and the nanofiltration membrane in nanofiltration membrane separation device are single tube or multichannel.
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| CN201310656576.9A CN103657419A (en) | 2013-12-06 | 2013-12-06 | Process for recovering alkali by double-membrane separation method in chemical fiber production |
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| CN201310656576.9A CN103657419A (en) | 2013-12-06 | 2013-12-06 | Process for recovering alkali by double-membrane separation method in chemical fiber production |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104311705A (en) * | 2014-11-07 | 2015-01-28 | 宜宾雅泰生物科技有限公司 | Technology for exacting semi fibers by using viscose fiber pressed alkali liquor as raw materials |
| CN104311703A (en) * | 2014-11-07 | 2015-01-28 | 宜宾雅泰生物科技有限公司 | Membrane concentration process of extracting hemicellulose from pressed liquid produced by viscose fiber production |
| CN104311702A (en) * | 2014-11-07 | 2015-01-28 | 宜宾雅泰生物科技有限公司 | Method for extracting hemicellulose from viscose squeezing alkali liquor |
| CN104496756A (en) * | 2014-11-07 | 2015-04-08 | 宜宾雅泰生物科技有限公司 | Electrodialysis technology for preparing xylitol by taking viscose fiber squeezed alkali liquid |
| CN105413465A (en) * | 2015-11-17 | 2016-03-23 | 南京工业大学 | Horizontal high-pressure ceramic membrane filtering system and application |
| CN105417762A (en) * | 2015-12-31 | 2016-03-23 | 上海清如环保科技有限公司 | Novel process for recycling alkali through ceramic membrane and electrodialysis coupling |
| CN106243248A (en) * | 2016-08-23 | 2016-12-21 | 南京工业大学 | Method for extracting hemicellulose from recovered alkali in viscose fiber production |
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2013
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104311705A (en) * | 2014-11-07 | 2015-01-28 | 宜宾雅泰生物科技有限公司 | Technology for exacting semi fibers by using viscose fiber pressed alkali liquor as raw materials |
| CN104311703A (en) * | 2014-11-07 | 2015-01-28 | 宜宾雅泰生物科技有限公司 | Membrane concentration process of extracting hemicellulose from pressed liquid produced by viscose fiber production |
| CN104311702A (en) * | 2014-11-07 | 2015-01-28 | 宜宾雅泰生物科技有限公司 | Method for extracting hemicellulose from viscose squeezing alkali liquor |
| CN104496756A (en) * | 2014-11-07 | 2015-04-08 | 宜宾雅泰生物科技有限公司 | Electrodialysis technology for preparing xylitol by taking viscose fiber squeezed alkali liquid |
| CN105413465A (en) * | 2015-11-17 | 2016-03-23 | 南京工业大学 | Horizontal high-pressure ceramic membrane filtering system and application |
| CN105417762A (en) * | 2015-12-31 | 2016-03-23 | 上海清如环保科技有限公司 | Novel process for recycling alkali through ceramic membrane and electrodialysis coupling |
| CN106243248A (en) * | 2016-08-23 | 2016-12-21 | 南京工业大学 | Method for extracting hemicellulose from recovered alkali in viscose fiber production |
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