CN106928486A - A kind of method of recovery of acetic acid fiber in filter tip from cigarette end - Google Patents
A kind of method of recovery of acetic acid fiber in filter tip from cigarette end Download PDFInfo
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- CN106928486A CN106928486A CN201710189827.5A CN201710189827A CN106928486A CN 106928486 A CN106928486 A CN 106928486A CN 201710189827 A CN201710189827 A CN 201710189827A CN 106928486 A CN106928486 A CN 106928486A
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- acetic acid
- fiber
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- recovery
- cigarette end
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- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 title claims abstract description 77
- 235000019504 cigarettes Nutrition 0.000 title claims abstract description 31
- 238000011084 recovery Methods 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims abstract description 21
- 239000000835 fiber Substances 0.000 title claims abstract description 20
- 239000002904 solvent Substances 0.000 claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 5
- 229920006221 acetate fiber Polymers 0.000 claims description 57
- 229960000583 acetic acid Drugs 0.000 claims description 23
- 239000007787 solid Substances 0.000 claims description 21
- 239000000047 product Substances 0.000 claims description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 238000005406 washing Methods 0.000 claims description 14
- 239000008367 deionised water Substances 0.000 claims description 13
- 229910021641 deionized water Inorganic materials 0.000 claims description 13
- 239000007788 liquid Substances 0.000 claims description 11
- 239000006210 lotion Substances 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 4
- 238000000926 separation method Methods 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 3
- 238000007654 immersion Methods 0.000 claims description 3
- 239000000084 colloidal system Substances 0.000 claims description 2
- 239000000706 filtrate Substances 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims description 2
- 238000001556 precipitation Methods 0.000 claims 1
- 230000008569 process Effects 0.000 abstract description 8
- 238000004090 dissolution Methods 0.000 abstract description 5
- 229920002678 cellulose Polymers 0.000 abstract description 2
- 239000001913 cellulose Substances 0.000 abstract description 2
- 229920002301 cellulose acetate Polymers 0.000 abstract description 2
- 230000000087 stabilizing effect Effects 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 8
- XOMKZKJEJBZBJJ-UHFFFAOYSA-N 1,2-dichloro-3-phenylbenzene Chemical group ClC1=CC=CC(C=2C=CC=CC=2)=C1Cl XOMKZKJEJBZBJJ-UHFFFAOYSA-N 0.000 description 6
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- 125000004122 cyclic group Chemical group 0.000 description 5
- WFDIJRYMOXRFFG-UHFFFAOYSA-N acetic acid anhydride Natural products CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 description 4
- 239000012362 glacial acetic acid Substances 0.000 description 4
- 241000208125 Nicotiana Species 0.000 description 3
- 235000002637 Nicotiana tabacum Nutrition 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- ZHNUHDYFZUAESO-UHFFFAOYSA-N Formamide Chemical compound NC=O ZHNUHDYFZUAESO-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000013019 agitation Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000001938 differential scanning calorimetry curve Methods 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 238000005457 optimization Methods 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 238000003672 processing method Methods 0.000 description 2
- 230000001988 toxicity Effects 0.000 description 2
- 231100000419 toxicity Toxicity 0.000 description 2
- 239000000052 vinegar Substances 0.000 description 2
- 235000021419 vinegar Nutrition 0.000 description 2
- 208000016261 weight loss Diseases 0.000 description 2
- 230000004580 weight loss Effects 0.000 description 2
- SNICXCGAKADSCV-JTQLQIEISA-N (-)-Nicotine Chemical compound CN1CCC[C@H]1C1=CC=CN=C1 SNICXCGAKADSCV-JTQLQIEISA-N 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 1
- 229920001587 Wood-plastic composite Polymers 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- VJMAITQRABEEKP-UHFFFAOYSA-N [6-(phenylmethoxymethyl)-1,4-dioxan-2-yl]methyl acetate Chemical compound O1C(COC(=O)C)COCC1COCC1=CC=CC=C1 VJMAITQRABEEKP-UHFFFAOYSA-N 0.000 description 1
- 150000008065 acid anhydrides Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 125000001309 chloro group Chemical group Cl* 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 238000004455 differential thermal analysis Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 238000013213 extrapolation Methods 0.000 description 1
- 238000007380 fibre production Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 239000002608 ionic liquid Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229960002715 nicotine Drugs 0.000 description 1
- SNICXCGAKADSCV-UHFFFAOYSA-N nicotine Natural products CN1CCCC1C1=CC=CN=C1 SNICXCGAKADSCV-UHFFFAOYSA-N 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
- 239000011155 wood-plastic composite Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J11/00—Recovery or working-up of waste materials
- C08J11/04—Recovery or working-up of waste materials of polymers
- C08J11/06—Recovery or working-up of waste materials of polymers without chemical reactions
- C08J11/08—Recovery or working-up of waste materials of polymers without chemical reactions using selective solvents for polymer components
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0288—Applications, solvents
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/005—Selection of auxiliary, e.g. for control of crystallisation nuclei, of crystal growth, of adherence to walls; Arrangements for introduction thereof
- B01D9/0054—Use of anti-solvent
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2301/08—Cellulose derivatives
- C08J2301/10—Esters of organic acids
- C08J2301/12—Cellulose acetate
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Crystallography & Structural Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Sustainable Development (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Artificial Filaments (AREA)
Abstract
The present invention is the method for solvent recovery of acetic acid fiber from cigarette end filter tip for a kind of utilization acetic acid, and its feature is the cellulose acetate in high efficiente callback cigarette end only with acetic acid as solvent.By controlling the reaction conditions such as solvent strength, quantity of solvent, dissolution time and solution temperature, recovery of acetic acid cellulose.Easy to operate, with low cost, equipment is simple, process stabilizing.
Description
Technical field
The invention belongs to technical field, a kind of method of recovery of acetic acid fiber in being related to filter tip from cigarette end, more particularly to
A kind of changing waste into resources, the cigarette end processing method beneficial to environmental protection.
Technical background
With the continuous improvement of the continuous progressive and living standard of science and technology, problem of environmental pollution has been increasingly becoming now
Most one of the stern challenge for facing.Nowadays, in numerous populations of China, 60% male and 4% women are all
Smoker, the cigarette end (i.e. cigarette end filter tip) of discarding has been even more into one of most common solid waste in our lives, and these
Cigarette end filter tip is made of acetate fiber mostly, it is difficult to be degraded in nature.In the long-standing situation of cigarette end toxicity
Under, food chain will be contaminated, and the harm to people is well imagined.Current common processing method is still to burn or fill, and consequence is just
It is that secondary pollution is caused to environment.
Acetate fiber production comes from early 1920s, is trial-produceed by Britain and realized successfully industrialization.Acetate fiber can
For manufacture textile, cigarette filter tip, chip base, plastic products etc..The acetate fiber of recovery can make wood-plastic composite floor
And plastics conveying tray etc..Whole world acetate fiber total output is about 75~800,000 tons, wherein pipe tobacco about 55~57 at present
Ten thousand tons, about 21~250,000 tons of weaving acetate fibre.There is family of acetate fiber manufacturer more than 20 in the whole world, and main manufacturer is concentrated
In American-European and Japan, 90% of Gross World Product or so is accounted for.The country starts late, especially the production of cigarette acetate fiber.
The eighties in 20th century, Chinese tobacco company built first factory with American technology cooperation in Nantong, established again later
Learn Industrial Co., Ltd (Sino-Japan joint), Zhuhai Acetate Fiber Co., Ltd's (sino-america joint-venture), and Zhengzhou boat in big Anhua, Ningbo
Its acetate fiber trial (demonstration) plant.From the point of view of with regard to the current acetate fiber development of China, mainly meet domestic demands, reduce into
Mouthful.
In sum, if the acetate fiber in these cigarette ends can be carried out into secondary recovery utilization, can be to a certain degree
Upper improvement environment, can alleviate some inlet pressures again.
At present, the method that acetate fiber in several recovery cigarette filters is reported both at home and abroad.1973,
Yu.I.Pravotorova et al. had found, the acetate fiber in cigarette end can be reclaimed with acetone solution, but mechanical agitation need 6~
8h, and the acetate fiber of preferable yield is just obtained at relatively high temperatures.2008, Liu Dengfeng et al. was with acetone and tetrahydrofuran
Solvent recovery simultaneously prepares the cellulose acetate homogeneous membrane of various concentrations., Min Zhao et al. acetone and N, N- diformazan in 2009
The mixed solution of base formamide dissolves acetate fiber, and a kind of asymmetric membrane is made after 24 hours by mechanical agitation, and can
To be applied in the production technology of enantioselectivity film.This several traditional methods dissolving recovery of acetic acid fiber not only need when
Between it is long, and the rate of recovery is relatively low.Based on this, Zhou Yawen et al. is with chloro 1- pi-allyl -3- methylimidazoles ([AMIM] Cl) come molten
Solution reclaims the acetate fiber in cigarette end, and dissolution time is fewer than above-mentioned several traditional methods, needs 70min, suitable solution temperature
It is 137 DEG C, but ionic liquid cost is higher, and about 500 yuan/100g, toxicity is also also to be assessed, if to be used to reclaim a large amount of
Cigarette end in acetate fiber, also need further research.Chinese patent CN201210183378.0 is using simple physicals such as cut-outs
Method after stub treatment to being used for papermaking, it is difficult to ensure that the purity of acetate fiber, therefore constrain its range of application.Peace and quiet et al.
《The Primary Study of discarded cigarette end class material recycling》In be briefly mentioned the mixture with acetic acid and acetic anhydride as solvent,
Acetate fiber in extracting stub under the catalytic action of sulfuric acid, but without quantitative.The present invention only needs finite concentration without catalyst
Acetic acid for solvent in room temperature in the range of 95 DEG C, can obtain the acetate fiber of higher extracted rate, comparatively speaking, the present invention
It is with the obvious advantage.
The content of the invention
It is with low cost it is an object of the invention to provide a kind of process is simple, it is easy to operate, in the recovery cigarette end of mild condition
The method of acetate fiber.Detailed process is as follows：
(1) cigarette end pretreatment
Using the different solubility in a solvent of the material in cigarette end, the impurity such as Salanesol first are removed with ethanol, then spend
Ionized water removes the impurity such as nicotine.
The detailed process of pretreatment is：Tear the pipe tobacco and paper wrapper remained in discarded cigarette end off, be cut into fiber with scissors
The segment long less than 1cm, then with soaked in absolute ethyl alcohol, then is fully washed with deionized water, pours out cleaning solution, uses deionized water
Segment of fiber is soaked at room temperature, the segment of fiber after immersion is sealed standby after drying.
(2) stub is reclaimed
A period of time is reacted with pretreated segment of fiber using certain density acetic acid, colloid substance is obtained, it is solid while hot
Liquid is separated, and to the multiple washing of solid, filtrate is aged at room temperature, washs the solid for separating out, and is then dried, that is, the vinegar for being regenerated
Sour fiber.
It is characterized in that：
(1) in the pretreatment stage of stub, stub is soaked about 18h at room temperature with absolute ethyl alcohol, then uses deionization
Water is fully washed three times, pours out cleaning solution, then segment of fiber is soaked into 9h at room temperature with deionized water, segment of fiber is taken out, in 70 DEG C
Under dry 24h.
(2) in acetate fiber recovery stage, use concentration anti-with stub for the acetic acid of 8-18mol/L at -95 DEG C of room temperature
0.25-4h is answered, product is washed three times with deionized water, the liquid after separation is stood into 2h at room temperature, by consolidating for separating out
The electrical conductivity that body is fully washed to washing lotion is 2 μ s/cm, and the solid after separation of solid and liquid then is dried into 3h at 80 DEG C.
By the optimization repeatedly of applicant, reaction time of optimization is 2h, acetate concentration 12mol/L, acetic acid amount be 50ml,
75 DEG C of solution temperature is optimum process condition.Under this process conditions, the rate of recovery is up to 92%.
Beneficial effects of the present invention are：Using this single solvent of acetic acid, vinegar can be extracted with stub reaction at room temperature
Sour fiber, process is simple, operating condition is gently controllable, with low cost.Highest recovery is up to 92%.
Fig. 1 is the XRD of the acetate fiber of recovery in the standard sample (A) of purchase, embodiment 1 to embodiment 5 (B)-(F).
The spectrogram of embodiment 5 (F) is closer to standard sample (A) figure, and diffraction maximum is had at 9.94 ° and 17.20 °, is in spectrogram
Now to there is peak of prominence on grand peak, but it is not sharp, show that acetate fiber is the two phase structure coexisted with crystalline state and amorphous state；
And the product spectrogram of embodiment 1- embodiments 4, compared with standard sample spectrogram, diffraction maximum is only present in 17.20 ° of position, spectrogram
In have the Long Feng of a widthization, illustrate that corresponding acetate fiber is solid-state amorphous state.
Fig. 2 is the product and the infrared spectrogram of standard items in embodiment 1.Figure it is seen that the acetate fiber for reclaiming
Spectrogram with acetate fiber standard sample is almost just the same.In 3448cm-1There is the strong absworption peak of a widthization at place, is the flexible of-OH
Vibration；2958cm-1Locate as-CH3、-CH2The stretching vibration of group；1753cm-1There is a sharp strong absworption peak at place, is the carbonyl of ester
The stretching vibration of base C=O；1633cm-1The absworption peak at place is the change angular oscillation of aqueous water；1379cm-1The absworption peak at place is-CH3
Symmetric deformation vibration；1238cm-1The absworption peak at place is acetyl ester bond；1043cm-1The absworption peak at place is chain acid anhydrides γ (C-
O-C stretching vibration).As can be seen that the product for extracting is acetate fiber from infrared spectrum.
Fig. 3 is the acetate fiber thermal multigraph that embodiment 1 is reclaimed.From the figure 3, it may be seen that from Fig. 3 acetate fiber TG curves, it is bent
Line shows three weightless ladders.Wherein, the first stage is room temperature~70 DEG C, it may be possible to a small amount of moisture adsorbed in acetate fiber
Or the evaporation of the solvent of residual；Second stage be 70~312 DEG C, this stage weightlessness for other two stages not
It is it is obvious that may be relevant with acetate fiber small molecular auxiliary agent；Phase III is 312~393 DEG C, weightless the one of this stage
As be considered as the main zero-g period, it is relevant with acetate fiber decomposition in itself；When temperature is more than 393 DEG C, with temperature
Raise, the quality of acetate fiber continues to decline, and when temperature is raised to 500 DEG C, the weight-loss ratio of acetate fiber reaches 93.06%.
Fig. 4 is the acetate fiber differential thermal analysis curve that embodiment 1 is reclaimed.As shown in Figure 4, with the rising of temperature, 64.4
1 endothermic peak is occurred in that on DEG C curve, it is and weightless corresponding at the first ladder of TG curves in Fig. 3, mainly and acetate fiber
The evaporation of middle moisture is relevant；At 200~250 DEG C, a more sharp absworption peak, mainly cellulose are showed in curve
The melting of itself, and peak point more substantially, and generally using peak point temperature as acetate fiber fusing point, i.e., 233 DEG C.Cut with double
Line extrapolation, can try to achieve extrapolated onset TeIt is 232 DEG C, is that fusing point is closer to peak temperature, therefore conventional this temperature or peak
Value temperature is compared as characteristic temperature.
To understand the hot property of the acetate fiber obtained under different experimental conditions, the product of embodiment 1,2,3,4,5 is chosen
TG and dsc analysis are carried out, as shown in Figure 5, Figure 6.Thus the characteristic temperature value of each condition products obtained therefrom can be tried to achieve, as shown in table 1.
The characteristic temperature value of product under each reaction condition of table 1
The fusing point of products obtained therefrom under different embodiments shown in Fig. 6 can be tried to achieve, as shown in table 2.
The melting point values of each condition product of table 2
Table 1, table 2 can be illustrated, in the condition and range that the application is limited, increase dissolution time, quantity of solvent, concentration of ordinary dissolution
And solution temperature, initial temperature and maximum weight loss rate temperature can increase, and final temperature can be reduced, and fusing point increase, i.e. acetic acid are fine
The heat endurance enhancing of dimension.The Multiple factors such as the rate of recovery, the cost recovery of Dichlorodiphenyl Acetate fiber are also wanted to consider in practical operation.
Fig. 7-Figure 10 is the influence of each process conditions Dichlorodiphenyl Acetate fiber recovery.So as to Optimizing Technical.
Brief description of the drawings
The XRD spectra of Fig. 1 recovery of acetic acid fibers；
The infrared spectrogram of Fig. 2 acetate fibers；
The TG curves of Fig. 3 acetate fibers；
The DSC curve of Fig. 4 acetate fibers；
The TG curves of acetate fiber under Fig. 5 different experimental conditions；
The DSC curve of acetate fiber under Fig. 6 different experimental conditions；
The influence of Fig. 7 dissolution time Dichlorodiphenyl Acetate fiber recoveries；
The influence of Fig. 8 acetate concentration Dichlorodiphenyl Acetate fiber recoveries；
The influence of Fig. 9 acetic acid volume Dichlorodiphenyl Acetate fiber recoveries；
The influence of Figure 10 solution temperature Dichlorodiphenyl Acetate fiber recoveries.
Specific embodiment
The present invention is further illustrated below by embodiment, but present invention protection content is not limited only to this.
Embodiment 1
By pretreated cigarette end, 4h is reacted at 95 DEG C with 50mL glacial acetic acid, product is washed with deionized, liquid exists
At room temperature by the standing of 2h, solid is separated out, and cyclic washing to washing lotion electrical conductivity is the electrical conductivity of deionized water, and solid is at 80 DEG C
Lower drying 3h, obtains acetate fiber.
Embodiment 2
By pretreated cigarette end, 0.25h is reacted at 95 DEG C with 50mL glacial acetic acid, product, liquid is washed with deionized
At room temperature by the standing of 2h, solid is separated out body, and cyclic washing to washing lotion electrical conductivity is the electrical conductivity of deionized water, and solid exists
3h is dried at 80 DEG C, acetate fiber is obtained.
Embodiment 3
By pretreated cigarette end, 4h is reacted at 95 DEG C with 30mL glacial acetic acid, product is washed with deionized, liquid exists
At room temperature by the standing of 2h, solid is separated out, and cyclic washing to washing lotion electrical conductivity is the electrical conductivity of deionized water, and solid is at 80 DEG C
Lower drying 3h, obtains acetate fiber.
Embodiment 4
By pretreated cigarette end, with 30mL concentration for the acetic acid of 8mol/L reacts 4h at 95 DEG C, it is washed with deionized water
Product is washed, at room temperature by the standing of 2h, solid is separated out liquid, and cyclic washing to washing lotion electrical conductivity is the conductance of deionized water
Rate, solid dries 3h at 80 DEG C, obtains acetate fiber.
Embodiment 5
By pretreated cigarette end, 4h being reacted at room temperature with 50mL glacial acetic acid, product being washed with deionized, liquid exists
At room temperature by the standing of 2h, solid is separated out, and cyclic washing to washing lotion electrical conductivity is the electrical conductivity of deionized water, and solid is at 80 DEG C
Lower drying 3h, obtains acetate fiber.
Claims (4)
1. in a kind of filter tip from cigarette end recovery of acetic acid fiber method, it is characterised in that：It is solvent to use common acetic acid,
Recovery of acetic acid fiber under conditions of gentle；Pretreated cigarette end is proceeded as follows：(1) finite concentration is used, it is a certain amount of
Acetic acid and pretreated segment of fiber react a period of time at a certain temperature, obtain colloid substance；(2) solid-liquid divides while hot
From to the multiple washing of solid, filtrate is aged at room temperature, washs the solid for separating out；(3) solid is dried, that is, is obtained again
Raw acetate fiber；Wherein, it is preferred that step (1) described concentration be 8-18mol/L, volume be 1L-6L acetic acid/1kg cigarette ends with
Stub is in -95 DEG C of reaction 2-4h of room temperature；Step (2) is fully washed product 3 times with deionized water, and the liquid after separation is existed
2h is stood at room temperature, is 2 μ s/cm by the electrical conductivity that the solid of precipitation is fully washed to washing lotion；Step (3) is by after separation of solid and liquid
Solid dries 3h at 80 DEG C.
2. method according to claim 1, it is characterised in that：The pretreatment is, with absolute ethyl alcohol by stub in room temperature
Lower immersion about 18h, is then fully washed three times with deionized water, pours out cleaning solution, then with deionized water by segment of fiber at room temperature
Immersion 9h, takes out segment of fiber, in drying 24h at 70 DEG C.
3. method according to claim 1, it is characterised in that：The rate of recovery of acetate fiber is 58-92% in cigarette end.
4. method according to claim 1, it is characterised in that：Preferably, reaction time 2h, acetate concentration 12mol/L, vinegar
Acid amount is 50ml, 75 DEG C of reaction temperature, and the rate of recovery is 92%.
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| CN201710189827.5A CN106928486B (en) | 2017-03-27 | 2017-03-27 | A kind of method of recovering acetate fiber from cigarette end filter |
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| CN201710189827.5A CN106928486B (en) | 2017-03-27 | 2017-03-27 | A kind of method of recovering acetate fiber from cigarette end filter |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108746150A (en) * | 2018-05-18 | 2018-11-06 | 昆明理工大学 | A kind of recoverying and utilizing method of discarded stub |
| CN111118670A (en) * | 2020-01-03 | 2020-05-08 | 内蒙古昆明卷烟有限责任公司 | Method for preparing carbon fiber by using waste cigarette butts, prepared carbon fiber and application |
| WO2020231362A1 (en) * | 2019-05-10 | 2020-11-19 | Kalabak Fevzi | Recycling method of cigarette butts |
| IT202000003745A1 (en) * | 2020-02-24 | 2021-08-24 | Consiglio Nazionale Ricerche | METHOD AND RELATED APPARATUS FOR THE TREATMENT OF CIGARETTE BUTTS |
| CN113471628A (en) * | 2021-07-30 | 2021-10-01 | 广东工业大学 | Multi-hydrogen bond cross-linked cellulose/carboxylated polyimide nanofiber composite diaphragm and preparation method and application thereof |
| EP3892393A1 (en) * | 2020-04-10 | 2021-10-13 | Luca Crivellin | Method for recycling cigarette filters |
| CN114728443A (en) * | 2019-11-26 | 2022-07-08 | 赫贰茨有限责任公司 | Method for producing semi-finished products and articles made of cellulose acetate |
| GR20210100730A (en) * | 2021-10-25 | 2023-05-10 | Κωνσταντινος Ανδρεα Ζαχαροπουλος | Cigarette filter cleaning method |
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| CN108746150A (en) * | 2018-05-18 | 2018-11-06 | 昆明理工大学 | A kind of recoverying and utilizing method of discarded stub |
| WO2020231362A1 (en) * | 2019-05-10 | 2020-11-19 | Kalabak Fevzi | Recycling method of cigarette butts |
| CN114728443A (en) * | 2019-11-26 | 2022-07-08 | 赫贰茨有限责任公司 | Method for producing semi-finished products and articles made of cellulose acetate |
| CN111118670A (en) * | 2020-01-03 | 2020-05-08 | 内蒙古昆明卷烟有限责任公司 | Method for preparing carbon fiber by using waste cigarette butts, prepared carbon fiber and application |
| CN111118670B (en) * | 2020-01-03 | 2022-07-05 | 内蒙古昆明卷烟有限责任公司 | Method for preparing carbon fiber by using waste cigarette butts, prepared carbon fiber and application |
| IT202000003745A1 (en) * | 2020-02-24 | 2021-08-24 | Consiglio Nazionale Ricerche | METHOD AND RELATED APPARATUS FOR THE TREATMENT OF CIGARETTE BUTTS |
| WO2021170381A1 (en) | 2020-02-24 | 2021-09-02 | Consiglio Nazionale Delle Ricerche | Method for treating cigarette butts |
| EP3892393A1 (en) * | 2020-04-10 | 2021-10-13 | Luca Crivellin | Method for recycling cigarette filters |
| CN113471628A (en) * | 2021-07-30 | 2021-10-01 | 广东工业大学 | Multi-hydrogen bond cross-linked cellulose/carboxylated polyimide nanofiber composite diaphragm and preparation method and application thereof |
| CN113471628B (en) * | 2021-07-30 | 2022-07-12 | 广东工业大学 | A kind of multi-hydrogen bond cross-linked cellulose/carboxylated polyimide nanofiber composite membrane and its preparation method and use |
| GR20210100730A (en) * | 2021-10-25 | 2023-05-10 | Κωνσταντινος Ανδρεα Ζαχαροπουλος | Cigarette filter cleaning method |
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