CN105040129A - Low-water-consumption washing process method for PAN (Polyacrylonitrile)-based carbon fiber precursor - Google Patents
Low-water-consumption washing process method for PAN (Polyacrylonitrile)-based carbon fiber precursor Download PDFInfo
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- CN105040129A CN105040129A CN201510339813.8A CN201510339813A CN105040129A CN 105040129 A CN105040129 A CN 105040129A CN 201510339813 A CN201510339813 A CN 201510339813A CN 105040129 A CN105040129 A CN 105040129A
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Abstract
The invention discloses a low-water-consumption washing process method for a PAN (Polyacrylonitrile)-based carbon fiber precursor. The method mainly comprises three main processes of pressed water throttling, wastewater recycling and ultra-filtration. The DMSO (Dimethylsulfoxide) carrying amount of strands carried into a pre-drafting tank is decreased by utilizing a pressed water roller device; the DMSO concentration of the pre-drafting tank is reasonably regulated by utilizing washing wastewater, the concentrations of a first coagulating bath, a second coagulating bath and a third coagulating bath are regulated by using pre-drafting waste liquid, the remaining parts are gathered in a coagulating bath waste liquid tank, and low-concentration DMSO is recycled, so that precursor production wastewater is fully utilized; the water supplementation amount of deionized water in the washing process is decreased, and the discharge amount of the washing wastewater is decreased, so that the consumption of the DMSO in the production process of the PAN precursor is reduced, and the discharge of DMSO wastewater is reduced; the amount of washing water is decreased to the greatest extent, so that the unit consumption of water for the precursor is reduced to be smaller than 40m<3>/ton, the zero discharge of the washing wastewater is realized, and an industry access standard that the water consumption of a ton PAN precursor product does not exceed 45 tons is met, wherein the industry access standard is offered in a Guiding Opinion about Acceleration of Continuous and Healthy Development of Carbon Fiber Industry given by the Ministry of Industry and Information Technology in 2013. The production cost of the precursor is greatly reduced, energy conservation and emission reduction are achieved, and high-efficient and environment-friendly green economy is realized.
Description
Technical field
The present invention relates to the process that one effectively can reduce polyacrylonitrile (PAN) base carbon fibre precursor production process water scouring water.
Background technology
Carbon fiber, with the performance of its excellence, is widely used in the every field such as Aero-Space, resource equipment, communications and transportation, architectural engineering, Leisure Sport, is the indispensable strategic new material of one of national economy and national defense construction.Wherein, maximum, most widely used general with polyacrylonitrile (PAN) base carbon fibre occupation rate of market.PAN base carbon fibre is obtained through peroxidating, carbonization process by PAN precursor, and the cost of precursor accounts for 50 ~ 60% of carbon fiber totle drilling cost.The production process of PAN precursor needs through operations such as polymerization, spinning, coagulating bath, washing, drying and drawing-offs.In order to reduce precursor cost, reducing dimethyl sulfoxide (DMSO) (DMSO) discharge of wastewater, needing to adopt advanced technologies to reduce coagulating bath and washing step DMSO loss, reducing washing water consumption.
In PAN wet spinning process, spinning solution through spraying silk, solidifying, forms nascent strand in coagulating bath operation.Owing to there is concentration difference, the DMSO solvent in spinning solution spreads to coagulating bath; Meanwhile, the hydrone in coagulating bath permeates to fibrous inside through the cortex of as-spun fibre, the process of this diffusion and infiltration, is precursor shaping " double diffusion " process.
In order to make tow be shaped with certain speed, coagulating bath is divided into four-stage by the difference of concentration gradient and other process conditions, is respectively that coagulating bath one is bathed, coagulating bath two is bathed, coagulating bath three is bathed and preliminary draft.Each stage DMSO concentration requirement controls in certain scope, and DMSO too high levels or too low is all unfavorable for the solidification forming of precursor.Coagulating bath four-stage control DMSO concentration reduces step by step, and when the preliminary draft stage, concentration is more low better, carries DMSO solution enter downstream washing step to reduce tow.
Tow mainly completes at washing step the washing work that DMSO is carried in filament surfaces and inside, to ensure that the inner DMSO content of tow is reduced to less than 0.2%.Under certain washing process condition, the DMSO that tow carries is more, and the washing water yield that water rinses consumes is larger, and wastewater discharge also can correspondingly increase, and DMSO wastage increases.Therefore, reduce precursor water scouring water, reduce precursor cost, need to set about from upstream coagulating bath and washing step, adopt advanced technology, reduce DMSO loss and discharge of wastewater.
Summary of the invention
The object of the invention is to: a kind of process that significantly can reduce PAN base carbon fiber protofilament water scouring water is provided, thus reduce the wastewater discharge in PAN base carbon fiber protofilament production process, reduce solvent DMSO loss, reduce precursor cost.
The technical solution used in the present invention is:
1, in three bath exits, a set of squeezing roll device is installed, reduces the DMSO entrainment that preliminary draft groove brought into by tow;
2, supplement washing waste water to preliminary draft fluid reservoir, regulate DMSO concentration to 0 ~ 5.0% scope in preliminary draft groove, utilize waste liquid in preliminary draft fluid reservoir to regulate coagulating bath one, two, three bath concentration further;
3, install a sets filtering device at preliminary draft groove circulating-pump outlet place, add coagulating bath one ~ tri-and bathe fluid reservoir after preliminary draft waste liquid is filtered, final remittance coagulating bath waste liquid tank, then delivers to distillation system, recycling design DMSO;
4, by pipeline, preliminary draft fluid reservoir top is connected with coagulating bath waste liquid tank, makes in preliminary draft fluid reservoir unnecessary waste liquid overflow to coagulating bath waste liquid tank, to reclaim DMSO further;
5, ensureing, under the condition that the DMSO content of rinsing bowl outlet tow is lower, to reduce washing rate of water make-up, to precursor use water ton consumption 10 ~ 40m
3/ t.
Described squeezing roll device adopts a kind of rubber rollers, diameter of section 50 ~ 300mm, smooth surface.
Washing waste water in described technical scheme 2 is the DMSO waste water at washing step water export place.
Filter in described technical scheme 3, adopts 316 stainless steel candle filters, and filter core is ultra micro reverse osmosis membrane.
Good effect of the present invention is: utilize squeezing roll device, reduces the DMSO entrainment that preliminary draft groove brought into by tow; Utilize washing waste water reasonable adjusting preliminary draft groove DMSO concentration, then regulate coagulating bath one ~ tri-bath concentration with leading waste liquid in advance, remainder overflow, to coagulating bath waste liquid tank, is reclaimed low concentration DMSO, precursor factory effluent is fully used; Reduce washing step deionized water rate of water make-up, reduce washing waste water and arrange outward, thus reduce DMSO loss in PAN precursor production process, reduce DMSO discharge of wastewater; Water scouring water can be saved to greatest extent, make precursor water unit consumption be reduced to 40m
3below/ton, realize washing waste water zero-emission; Significantly reduce precursor production cost, energy-saving and emission-reduction, realize the green economy of high-efficiency environment friendly.
Accompanying drawing explanation
Fig. 1 is the process chart of the inventive method.
Detailed description of the invention
Below in conjunction with accompanying drawing, the specific embodiment of the present invention is elaborated.
As shown in Figure 1, process of the present invention is: first, drive apparatus 2 place is exported at PAN spinning coagulation bath three bath 1, a set of compressed water generation apparatus 10 is installed, it is the combination of a kind of squeeze roll(s), squeeze roll(s) adopts a kind of special rubber rollers, diameter of section 50 ~ 300mm, heat-resisting, withstand voltage, corrosion-resistant, squeeze roll(s) smooth surface, hardness is moderate, under certain operating pressure to tow without any injury, mainly carry DMSO solution enter preliminary draft groove 3 and rinsing bowl 9 in order to reduce precursor tow, make DMSO concentration in three baths 1 control in 1.0% ~ 20% scope; The second, rinsing bowl 9 is connected with preliminary draft fluid reservoir 7 through pipeline 11, supplements washing waste water to preliminary draft fluid reservoir 7, regulate DMSO concentration to 0 ~ 5.0% scope in preliminary draft groove 3, utilize preliminary draft waste liquid to regulate coagulating bath one ~ tri-bath concentration further; 3rd, at preliminary draft groove circulating-pump outlet place, a set of filter for installation 13 is installed, adopt 316 stainless steel candle filters, filter core is ultra micro reverse osmosis membrane, make preliminary draft waste liquid after filtering as the regulator solution that coagulating bath one ~ tri-is bathed, fluid reservoir 4 is bathed in coagulating bath one, fluid reservoir 5 is bathed in coagulating bath two, fluid reservoir 6 is bathed in coagulating bath three in injection respectively, and final overflow delivers to distillation system after importing coagulating bath waste liquid tank 8, recycling design DMSO, Filter Precision requires below 5 μm; 4th, by pipeline 12, preliminary draft fluid reservoir 7 top is connected with coagulating bath waste liquid tank 8, makes in preliminary draft fluid reservoir 7 unnecessary waste liquid overflow to coagulating bath waste liquid tank 8, to reclaim DMSO further; 5th, under ensureing that rinsing bowl 9 exports the lower condition of the DMSO content of tow, reduce deionized water 14 rate of water make-up of continuous supplementation in tow washing process, to precursor use water ton consumption at 10 ~ 40m
3/ t scope.
Claims (5)
1. a low water consumption PAN base carbon fiber protofilament washing process method, is characterized in that:
1. in three bath exits, a set of compressed water generation apparatus is installed, reduces the DMSO entrainment that preliminary draft groove brought into by tow;
2. supplement washing waste water to preliminary draft fluid reservoir, regulate DMSO concentration to 0 ~ 5.0% scope in preliminary draft groove, utilize preliminary draft waste liquid to regulate coagulating bath one, two, three bath concentration;
3. at preliminary draft groove circulating-pump outlet place, one sets filtering device is installed, after preliminary draft waste liquid is filtered, enters coagulating bath waste liquid tank, recycling design DMSO;
4. by pipeline, preliminary draft fluid reservoir top is connected with coagulating bath waste liquid tank, makes unnecessary waste liquid overflow in preliminary draft fluid reservoir to coagulating bath waste liquid tank, reclaim DMSO further;
5. ensureing, under the condition that the DMSO content of rinsing bowl outlet tow is lower, to reduce washing rate of water make-up to precursor use water ton consumption 10 ~ 40m
3/ t.
2. low water consumption PAN base carbon fiber protofilament washing process method according to claim 1, is characterized in that: above-mentioned compressed water generation apparatus adopts a kind of rubber rollers, diameter of section 50 ~ 300mm, smooth surface.
3. low water consumption PAN base carbon fiber protofilament washing process method according to claim 1, is characterized in that: described step 2. in washing waste water, be all washing process waste water.
4. low water consumption PAN base carbon fiber protofilament washing process method according to claim 1, it is characterized in that: above-mentioned filter adopts 316 stainless steel candle filters, filter core is ultra micro reverse osmosis membrane.
5. low water consumption PAN base carbon fiber protofilament washing process method according to claim 4, is characterized in that: above-mentioned metre filter precision is less than 5 μm.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510339813.8A CN105040129A (en) | 2015-06-18 | 2015-06-18 | Low-water-consumption washing process method for PAN (Polyacrylonitrile)-based carbon fiber precursor |
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| CN201510339813.8A CN105040129A (en) | 2015-06-18 | 2015-06-18 | Low-water-consumption washing process method for PAN (Polyacrylonitrile)-based carbon fiber precursor |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106477827A (en) * | 2016-12-13 | 2017-03-08 | 北京北方节能环保有限公司 | A kind of tow method of wastewater treatment |
| CN106702509A (en) * | 2016-12-19 | 2017-05-24 | 哈尔滨天顺化工科技开发有限公司 | M-type solvent drafting device for carbon fiber precursor production |
| CN107447274A (en) * | 2017-08-31 | 2017-12-08 | 中安信科技有限公司 | A kind of high performance carbon fiber used polyacrylonitrile precursor production water washing device and method |
| CN112725915A (en) * | 2020-12-25 | 2021-04-30 | 内蒙古双欣环保材料股份有限公司 | Tow washing device and tow washing method |
| CN116334777A (en) * | 2023-05-26 | 2023-06-27 | 吉林富博纤维研究院有限公司 | Water bath drafting device and PAN-based carbon fiber precursor production system |
-
2015
- 2015-06-18 CN CN201510339813.8A patent/CN105040129A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106477827A (en) * | 2016-12-13 | 2017-03-08 | 北京北方节能环保有限公司 | A kind of tow method of wastewater treatment |
| CN106702509A (en) * | 2016-12-19 | 2017-05-24 | 哈尔滨天顺化工科技开发有限公司 | M-type solvent drafting device for carbon fiber precursor production |
| CN106702509B (en) * | 2016-12-19 | 2020-05-22 | 哈尔滨天顺化工科技开发有限公司 | A M type solvent drafting arrangement for carbon fiber precursor production |
| CN107447274A (en) * | 2017-08-31 | 2017-12-08 | 中安信科技有限公司 | A kind of high performance carbon fiber used polyacrylonitrile precursor production water washing device and method |
| CN107447274B (en) * | 2017-08-31 | 2018-08-17 | 中安信科技有限公司 | A kind of high performance carbon fiber used polyacrylonitrile precursor production water washing device and method |
| CN112725915A (en) * | 2020-12-25 | 2021-04-30 | 内蒙古双欣环保材料股份有限公司 | Tow washing device and tow washing method |
| CN115262040A (en) * | 2020-12-25 | 2022-11-01 | 内蒙古双欣环保材料股份有限公司 | Polyvinyl alcohol fiber strand mirabilite online recovery device and method |
| CN116334777A (en) * | 2023-05-26 | 2023-06-27 | 吉林富博纤维研究院有限公司 | Water bath drafting device and PAN-based carbon fiber precursor production system |
| CN116334777B (en) * | 2023-05-26 | 2023-07-21 | 吉林富博纤维研究院有限公司 | Water bath drafting device and PAN-based carbon fiber precursor production system |
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