CN103103633A - Modified polylactic acid filament bundle and filter rod used for cigarette and preparation method - Google Patents
Modified polylactic acid filament bundle and filter rod used for cigarette and preparation method Download PDFInfo
- Publication number
- CN103103633A CN103103633A CN2013100488129A CN201310048812A CN103103633A CN 103103633 A CN103103633 A CN 103103633A CN 2013100488129 A CN2013100488129 A CN 2013100488129A CN 201310048812 A CN201310048812 A CN 201310048812A CN 103103633 A CN103103633 A CN 103103633A
- Authority
- CN
- China
- Prior art keywords
- pla
- tow
- filament bundle
- cigarette
- drying
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
- D01F6/62—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyesters
- D01F6/625—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyesters derived from hydroxy-carboxylic acids, e.g. lactones
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/92—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyesters
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Biological Depolymerization Polymers (AREA)
Abstract
The invention relates to a modified polylactic acid filament bundle and a filter rod used for cigarette and a preparation method, wherein the modified polylactic acid filament bundle is prepared by heating, fusing, mixing, drafting, curling, drying and forming of at least two of three raw materials of PLA-1, PLA-2 and PLA-3. The invention has the beneficial effects that three polylactic acids are mixed according to a certain proportion, the levorgyration content in the raw material is reduced, and the filament bundle surface crystallization degree is reduced, the filament bundle surface structure is loosened and unordered, so that when the filter rod is formed, a glyceryl triacetate plasticizer is applied, the filament bundle enables bonding and swelling, the hardness can reach more than 87% with low filling amount of the filament bundle, so that the utility value is provided. By analysis and detection, compared with an acetate fiber filter rod cigarette, the polylactic acid filament bundle filter rod has the conventional component release amount of flue gas similar to that of the acetate fiber filter rod cigarette, but has improved sensory quality; because polylactic acid has biodegradable characteristic, the environmental pollution is reduced.
Description
Technical field
The invention belongs to cigarette filter tip materials and preparing technical field thereof, be specifically related to a kind of PLA pipe tobacco of modification and filter stick and preparation method thereof.
Background technology
Cigarette filter is an important component part of cigarette.As the cigarette filter-tip material, except having good spinning property, also have a lot of unique requirements: (1) is rolled by it that the filter stick that forms is nontoxic, tasteless, security is good; (2) tow good stability can satisfy the requirement of filter stick formation equipment and process; (3) have suitable rigidity and crimp property, make it to have good elasticity and opening character, in the situation that less tow loading, after adding plasticizer or adhesive, filter stick satisfies certain hardness, resistance to suction and appearance requirement, and the higher excellent rate that goes out is arranged, and has practical value; (4) in the cigarette smoking process, filter tip does not subside, is out of shape; (5) filter stick has higher filter efficiency to harmful ingredients in flue gas.Up to now, a lot of fibers have been realized suitability for industrialized production, but real commercial cigarette filter tip materials only has cellulose diacetate and two kinds of polypropylene.
Cellulose diacetate fibers (vinegar is fine) is a kind of function admirable, the general filter-tip material of application, and its selection is adopted the mode of dry spinning in perennial high-quality timber, makes and is suitable for the filter tow that cigarette is used.The polar group that contains strong polarity on the fine molecule side chain of vinegar, tow surface have micropore and harsh feeling, so diacetate fiber to the harmful components in flue gas, has physical absorption and chemisorbed double effects simultaneously, it filters and the absorption property excellence; And, in the process of producing filter stick, carry out plasticising, bonding by adding triacetyl glycerine, in the situation that less tow loading, filter stick satisfies the quality requirements such as hardness, resistance to suction, and the higher excellent rate that goes out is arranged.But the raw material of producing cellulose diacetate are perennial high-quality timber, China at present can not be self-supporting, main dependence import, the more important thing is, along with the continuous expansion of domestic tobacco enterprise output, the demand of the fine filter stick of vinegar is grown with each passing day, but at present domestic diacetate fiber manufacturing enterprise can not satisfy the demand of tobacco enterprise fully, cause vinegar situation fine in short supply, limited to a certain extent further developing of China's tobacco business.In addition, more serious pollution problem is followed in wood pulp production, cellulose esterification and cellulose acetate spinning, and production cost is high, and is expensive, compares with timber, and the biodegradability of cellulose acetate is significantly deteriorated.
Polypropylene cigarette as the distinctive a kind of filtering material of China's cigarette industry, has raw material abundance at initial stage of development with filter tow, the advantage such as cheap and being greatly developed, and make a great contribution for China's tobacco business cost efficiency.Pp material is taken from oil, adopts the mode of melt spinning, and the fibre bundle that makes is in the process of producing filter stick, bond by adding special-purpose adhesive, in the situation that less tow loading, filter stick satisfies the quality requirements such as hardness, resistance to suction, and the higher excellent rate that goes out is arranged.But because polypropylene is the highly stable apolar substance of a kind of structure, own without any polar group, the tow smooth surface, its adsorption capacity can not show a candle to acetate fiber, smoke filtering effect is poor, and stronger acid is arranged during suction, generally can only be used for Low-end Cigarettes; Simultaneously, polypropylene is long chain hydrocarbon, can not biodegradation, environment is caused severe contamination; In addition, petroleum resources are day by day exhausted, and increasing price of raw materials is fast, and polyacrylic price advantage is just progressively lost.In recent years, along with the adjustment of tobacco business product structure, China's cigarette class improves constantly, and the Low-end Cigarettes consumption descends year by year, the third fine consumption reduced year by year, and trend is progressively withdrawn from the market.
No matter from the angle of resource, or the angle of environmental contamination reduction, seek a kind of combination property near the vinegar fibre, price is relatively cheap novel pipe tobacco again, substitute the production that polypropylene material is used for low and middle-grade cigarette, and the fine production that is used for medium-to-high grade cigarette of the alternative vinegar of part, to make up the deficiency of the fine supply of vinegar, be the tobacco business urgent problem.
PLA is a kind of novel environment friendly material, has good circular regeneration and biological degradability.It is take reproducible plant resources (corn, wheat, beet, rice, potato, sweet potato etc.) and organic waste (root of corncob or other crops, stem, leaf, skin etc.) as raw material, break away from the dependence to timber and petroleum resources, met the requirement of international community's sustainable development; The energy consumption of PLA lower than various fibers such as polypropylene and cellulose diacetates, is a kind of macromolecular material of low-resource carrying capacity of environment; PLA can complete biodegradable, can natural decomposition be water and carbon dioxide through certain hour in natural environment, do not cause environmental pollution, the carbon dioxide that produces is re-used by the photosynthesis of plant, becoming eternal, carbon cycle system sealing, is genuine " green material "; PLA has good processing characteristics, can adopt melt spinning method production; The fine structural similarity of acid fiber by polylactic and vinegar, molecular surface contains abundant polar group; Polar substances had stronger affinity, can carry out chemical reaction with tar component and lower-molecular substance, reactant is firmly stayed fiber surface, simultaneously, the tow surface has micropore and harsh feeling, in the adsorption process to flue gas, have simultaneously physical absorption and chemisorbed double effects, the filter stick that this tow is produced is obvious to the harmful substance filter effect in flue gas.Therefore, PLA is expected to become the suitable material that the preparation cigarette is used filter filament.
Polylactic fibre product as the cigarette filtering material, had the comprehensive advantages such as aboundresources, the excellent feature of environmental protection, good adsorptivity, reliable security, good processing and forming and economy; Applying of product, for China's tobacco business widen the raw material channel, cost efficiency has positive realistic meaning, will produce good economic results in society, and will drive the development of the whole industrial chain of China's poly-lactic acid material.
Present domestic existing several pieces of patents about the PLA pipe tobacco are in the patent No.: technique and the method for having introduced polylactic resin raw material spinning PLA pipe tobacco in 200610131699.0 " a kind of cigarette filter filaments and preparation method thereof "; 201010127357.8 introduced a kind of filament bundle for degrading cigarette in " preparation method of a kind of filament bundle for degrading cigarette and preparation thereof and filter stick ", its raw material is any one in the poly-levorotatory lactide that contains crystallization promoter, poly-dextrorotation lactide or both blends, and tow is made filter stick by shredding, gluing.But there are some problems in the patent of two pieces of tops, in " a kind of cigarette filter filament and preparation method thereof " patent, the percentage by weight of the L-lactic acid unit of polylactic resin used is 3-7%, degree of crystallinity is high, obtained tow can't by filter stick for cigarettes plasticizer triacetyl glycerine swelling, therefore, need to make filter stick hardness reach requirement by higher tow loading, cause the excellent rate of going out of PLA tow lower, improved the cost of PLA filter stick.In " preparation method of a kind of filament bundle for degrading cigarette and preparation thereof and filter stick " patent, when adopting the PLA filter stick formation, adopt Aqueous Adhesives to be bonded to rod to tow, just there are three problems in this: (1) filter-stick forming device used is the domestic filter-stick forming device that applies Aqueous Adhesives, and shaping speed is slow; (2) may contain some volatile organic compounds in Aqueous Adhesives, have potential safety hazard; (3) filter stick need to be dried in baking oven, has increased PLA filter stick manufacturing procedure and cost.
Summary of the invention
One object of the present invention is exactly the problem for above-mentioned existence, a kind of improved PLA pipe tobacco is provided, this tow surface crystallinity reduces, can adopt filter stick for cigarettes plasticizer triacetyl glycerine to carry out filter stick formation, under lower tow loading, filter stick hardness is reached more than 87%, have higher practical value.
the principles of science of institute of the present invention foundation is: be 94-99% by optical purity, the mol ratio of D-lactic acid unit is that (optical purity is 50-82% to two kinds of lower PLAs of D-lactic acid unit mol ratio of the PLA of 97%-99.5% and other, the mol ratio of D-lactic acid unit is that PLA and the optical purity of 75-91% is 0-20%, the mol ratio of D-lactic acid unit is the PLA of 40-60%) mix, make that in the PLA tow, the shared mol ratio of left-handed lactic acid units declines to a great extent, thereby cause the lactic acid molecules arrangement regularity decline on PLA tow surface, the degree of crystallinity that causes PLA tow surface decreases, make triacetyl glycerine play swelling action to the tow surface, make this kind tow can be under lower tow loading when filter stick formation, hardness reaches more than 87%, improved the excellent rate of going out of tow.This tow has good cost performance and practical value.
The objective of the invention is to be achieved through the following technical solutions:
A kind of PLA pipe tobacco of modification, to be mixed through heating and melting by two or more at least in PLA-1, PLA-2 and three kinds of raw materials of PLA-3, be prepared from through drawing-off, curling, drying and shaping operation, the ratio of three kinds of raw materials is that PLA-1: PLA-2: PLA-3 is 0-80%: 0-90%: 0-90%;
Described PLA-1: optical purity is 94-99%, the mol ratio of D-lactic acid unit is 97%-99.5%, and weight average molecular weight is 5-20 ten thousand, and melting range is 160-190 ℃, the melt melt index of measuring under loading with 2.16Kg at 190 ℃ is at 5-30g/10min, and degree of crystallinity is 35-55%;
Described PLA-2: optical purity is 50-82%, the mol ratio of D-lactic acid unit is 75-91%, and weight average molecular weight is 5-20 ten thousand, and melting range is 100-130 ℃, the melt melt index of measuring under loading with 2.16Kg at 190 ℃ is at 5-30g/10min, and degree of crystallinity is 2-12%;
Described PLA-3: optical purity is 0-20%, the mol ratio of D-lactic acid unit is 40-60%, and weight average molecular weight is 5-20 ten thousand, and melting range is 80-120 ℃, the melt melt index of measuring under loading with 2.16Kg at 190 ℃ is at 5-30g/10min, and degree of crystallinity is 0-5%.
The ratio of three kinds of raw materials is preferably PLA-1: PLA-2: PLA-3 is 15-80: 15-80: 5-50.
The PLA cigarette of modification is to be prepared from by following concrete grammar with silk:
(1) will tie PLA-1 and be dried to moisture less than 200ppm, 60～120 ℃ of baking temperatures, 4～8 hours drying times, PLA-2 is dried to moisture less than 200ppm, 50～60 ℃ of baking temperatures, are dried to moisture less than 200ppm with PLA-3 simultaneously at 8～16 hours drying times, 50～60 ℃ of baking temperatures, 8～16 hours drying times;
(2) send into spinning system after above-mentioned three kinds of polylactic resin heating and meltings mix, in 190～220 ℃ of meltings, filtration, quantitatively input filament spinning component through measuring pump; Melt is extruded through spinnerets; The spinnerets hole count is 8000～15000, and the spinneret orifice profile is three leaves (Y) types;
(3) adopting process air-conditioning cold radiator cooler carries out cooling forming to new spun tow, 10～20 ℃ of cooling wind-warm syndrome; By the finish oil disc that rotates with finish (TAKEMOTO OIL﹠amp; FAT CO., the DELION board finish of LTD company) be coated in the tow surface to improve rear road machinability;
(4) be temporary in fiber barrel after under suitable coiling speed, tow being reeled, coiling speed is controlled at 300～1500m/min;
(5) in the water-bath of uniform temperature, tow is carried out drawing-off, drawing temperature is 50～90 ℃, and the drawing-off multiplying power is 2～3.5 times;
(6) tow after drawing-off enters crimping machine and carries out curlingly, and curling temperature is 85～95 ℃;
(7) obtain PLA pipe tobacco of the present invention after the tow drying and shaping after curling, the drying and shaping temperature is at 60～90 ℃, drying and shaping time 10～15min.
A kind of method of utilizing above-mentioned PLA pipe tobacco to prepare filter stick is as follows: the PLA tow is carried out moulding by filter-stick forming devices such as YL21, KDF-2, KDF-3 or KDF-4, tow is after shredding, apply triacetyl glycerine as the filter stick plasticizer, the plasticizer addition is the 4-12%wt of tow by weight percentage, and the filter stick of preparation is put under normal temperature namely curable.
In this PLA filter stick, the tow bonding is good, and under lower tow loading, hardness is compared with the fine filter stick cigarette of vinegar after the tipping cigarette more than 87%, and flue gas conventional ingredient burst size approaches, and the aesthetic quality increases.Concrete contrast detects index as showing 1-3:
Filter stick index after the different wire-beam formings of table 1 (24.1mm * 120mm)
| Sample | Length m m | Weight g | Circumference mm | Resistance to suction pa | Hardness % |
| The fine filter stick of vinegar | 144 | 0.92 | 24.1 | 3480 | 88 |
| The PLA filter stick | 144 | 0.89 | 24.1 | 3494 | 88 |
Cigarette main stream flue gas index under table 2 variety classes filter stick detects table
Cigarette organoleptic attribute under the table 3 variety classes filter stick record sheet of smokeing panel test
Annotate: " ↑ " expression slightly is improved and promotes; " ↑ ↑ " obviously improvement and lifting of expression; " ↓ " expression slightly has variation; " ↓ ↓ " represent obvious variation; "=" expression is unchanged.
The present invention compared with prior art has following beneficial effect:
1. three kinds of PLAs are mixed by a certain percentage, owing to having added the high PLA of dextronic acid content as raw material in raw material, cause left-handed content decline in raw material, affected PLA tow surface crystallization, made loose, unordered that PLA tow surface texture becomes, so this tow applies the triacetyl glycerine plasticizer when filter stick formation after, can make tow bonding and swelling, under lower tow loading, hardness reaches more than 87%, has practical value.
2. detect by analysis, the invention provides the made filter stick of PLA tow, compare with the fine filter stick cigarette of vinegar, flue gas conventional ingredient burst size approaches, and the aesthetic quality increases.
3. in addition, because PLA has biodegradable characteristics, can reduce pollution on the environment.
The specific embodiment
The present invention is described further below with reference to embodiment, but content of the present invention is not limited to this.
Embodiment 1
Select the PLA-1 polylactic resin, adopt the vacuum drum drying machine to be dried, 80 ℃ of baking temperatures, 8 hours drying times, moisture is less than 200ppm; Select the PLA-2 polylactic resin, adopt the vacuum drum drying machine to be dried, 55 ℃ of baking temperatures, 8 hours drying times, moisture is less than 200ppm; Select the PLA-3 polylactic resin, adopt the vacuum drum drying machine to be dried, 50 ℃ of baking temperatures, 8 hours drying times, moisture is less than 200ppm; Dried above-mentioned three kinds of raw materials are pressed 60:20:20 mix, in 210 ℃ of lower meltings, filtration, quantitatively input filament spinning component through measuring pump, the spinnerets hole count is 11400, and the spinneret orifice profile is trilobal cross; Adopt the cooling air of 11 ℃ to carry out cooling forming, by finish oil disc, finish is coated in the tow surface; In being temporary in fiber barrel after under the coiling speed of 550m/min, tow being reeled; In the water-bath of 75 ℃, tow is carried out drawing-off, draft speed 100～200m/min, the drawing-off multiplying power is 2.3; Tow after counter extensioin carries out curling on crimping machine, and curling temperature is 90 ℃; Tow after curling enters drying and setting machine, and the drying and shaping temperature is at 65～75 ℃, drying and shaping time 12min; Finally, obtaining monofilament linear density is 3.4dtex, and tow line density is 3.89ktex, and crispation number is the PLA tow of 23/25mm.The moulding on the KDF-2 filter-stick forming device of this tow, triacetyl glycerine applied amount are the 5%wt of tow, and after filter stick solidified, filter stick hardness reached 88%.
Embodiment 2
Select the PLA-1 polylactic resin, adopt the vacuum drum drying machine to be dried, 90 ℃ of baking temperatures, 8 hours drying times, moisture is less than 200ppm; Select the PLA-2 polylactic resin, adopt the vacuum drum drying machine to be dried, 55 ℃ of baking temperatures, 8 hours drying times, moisture is less than 200ppm; Select the PLA-3 polylactic resin, adopt the vacuum drum drying machine to be dried, 50 ℃ of baking temperatures, 8 hours drying times, moisture is less than 200ppm; Dried above-mentioned three kinds of raw materials are pressed 70:20:10 mix, in 215 ℃ of lower meltings, filtration, quantitatively input filament spinning component through measuring pump, the spinnerets hole count is 11400, and the spinneret orifice profile is trilobal cross; Adopt the cooling air of 11 ℃ to carry out cooling forming, by finish oil disc, finish is coated in the tow surface; In being temporary in fiber barrel after under the coiling speed of 450m/min, tow being reeled; In the water-bath of 75 ℃, tow is carried out drawing-off, draft speed 100～200m/min, the drawing-off multiplying power is 2.5; Tow after counter extensioin carries out curling on crimping machine, and curling temperature is 95 ℃; Tow after curling enters drying and setting machine, and the drying and shaping temperature is at 70～85 ℃, drying and shaping time 12min; Finally, obtaining monofilament linear density is 3.7dtex, and tow line density is 4.22ktex, and crispation number is the PLA tow of 23/25mm.The moulding on the KDF-2 filter-stick forming device of this tow, triacetyl glycerine applied amount are the 6%wt of tow, and after filter stick solidified, filter stick hardness reached 88%.
Embodiment 3
Select the PLA-1 polylactic resin, adopt the vacuum drum drying machine to be dried, 100 ℃ of baking temperatures, 8 hours drying times, moisture is less than 200ppm; Select the PLA-2 polylactic resin, adopt the vacuum drum drying machine to be dried, 55 ℃ of baking temperatures, 8 hours drying times, moisture is less than 200ppm; Select the PLA-3 polylactic resin, adopt the vacuum drum drying machine to be dried, 50 ℃ of baking temperatures, 8 hours drying times, moisture is less than 200ppm; Dried above-mentioned three kinds of raw materials are pressed 50:30:20 mix, in 205 ℃ of lower meltings, filtration, quantitatively input filament spinning component through measuring pump, the spinnerets hole count is 13200, and the spinneret orifice profile is trilobal cross; Adopt the cooling air of 11 ℃ to carry out cooling forming, by finish oil disc, finish is coated in the tow surface; In being temporary in fiber barrel after under the coiling speed of 450m/min, tow being reeled; In the water-bath of 75 ℃, tow is carried out drawing-off, draft speed 100～200m/min, the drawing-off multiplying power is 2.5; Tow after counter extensioin carries out curling on crimping machine, and curling temperature is 85 ℃; Tow after curling enters drying and setting machine, and the drying and shaping temperature is at 65～75 ℃, drying and shaping time 12min; Finally, obtaining monofilament linear density is 3.4dtex, and tow line density is 4.44ktex, and crispation number is the PLA tow of 21/25mm.The moulding on the KDF-3 filter-stick forming device of this tow, triacetyl glycerine applied amount are the 5%wt of tow, and after filter stick solidified, filter stick hardness reached 88%.
Embodiment 4
Select the PLA-1 polylactic resin, adopt the vacuum drum drying machine to be dried, 90 ℃ of baking temperatures, 8 hours drying times, moisture is less than 200ppm; Select the PLA-2 polylactic resin, adopt the vacuum drum drying machine to be dried, 55 ℃ of baking temperatures, 8 hours drying times, moisture is less than 200ppm; Select the PLA-3 polylactic resin, adopt the vacuum drum drying machine to be dried, 50 ℃ of baking temperatures, 8 hours drying times, moisture is less than 200ppm; Dried above-mentioned three kinds of raw materials are pressed 40:40:20 mix, in 210 ℃ of lower meltings, filtration, quantitatively input filament spinning component through measuring pump, the spinnerets hole count is 11400, and the spinneret orifice profile is trilobal cross; Adopt the cooling air of 11 ℃ to carry out cooling forming, by finish oil disc, finish is coated in the tow surface; In being temporary in fiber barrel after under the coiling speed of 550m/min, tow being reeled; In the water-bath of 75 ℃, tow is carried out drawing-off, draft speed 100～200m/min, the drawing-off multiplying power is 2.3; Tow after counter extensioin carries out curling on crimping machine, and curling temperature is 90 ℃; Tow after curling enters drying and setting machine, and the drying and shaping temperature is at 65～75 ℃, drying and shaping time 12min; Finally, obtaining monofilament linear density is 3.4dtex, and tow line density is 3.89ktex, and crispation number is the PLA tow of 23/25mm.The moulding on the KDF-3 filter-stick forming device of this tow, triacetyl glycerine applied amount are the 7%wt of tow, and after filter stick solidified, filter stick hardness reached 88%.
Embodiment 5
Select the PLA-1 polylactic resin, adopt the vacuum drum drying machine to be dried, 90 ℃ of baking temperatures, 8 hours drying times, moisture is less than 200ppm; Select the PLA-2 polylactic resin, adopt the vacuum drum drying machine to be dried, 55 ℃ of baking temperatures, 8 hours drying times, moisture is less than 200ppm; Select the PLA-3 polylactic resin, adopt the vacuum drum drying machine to be dried, 50 ℃ of baking temperatures, 8 hours drying times, moisture is less than 200ppm; Dried above-mentioned three kinds of raw materials are pressed 30:50:20 mix, in 215 ℃ of lower meltings, filtration, quantitatively input filament spinning component through measuring pump, the spinnerets hole count is 11400, and the spinneret orifice profile is trilobal cross; Adopt the cooling air of 11 ℃ to carry out cooling forming, by finish oil disc, finish is coated in the tow surface; In being temporary in fiber barrel after under the coiling speed of 450m/min, tow being reeled; In the water-bath of 75 ℃, tow is carried out drawing-off, draft speed 100～200m/min, the drawing-off multiplying power is 2.5; Tow after counter extensioin carries out curling on crimping machine, and curling temperature is 95 ℃; Tow after curling enters drying and setting machine, and the drying and shaping temperature is at 70～85 ℃, drying and shaping time 12min; Finally, obtaining monofilament linear density is 3.7dtex, and tow line density is 4.22ktex, and crispation number is the PLA tow of 23/25mm.The moulding on the KDF-4 filter-stick forming device of this tow, triacetyl glycerine applied amount are the 5%wt of tow, and after filter stick solidified, filter stick hardness reached 88%.
Embodiment 6
Select the PLA-1 polylactic resin, adopt the vacuum drum drying machine to be dried, 70 ℃ of baking temperatures, 8 hours drying times, moisture is less than 200ppm; Select the PLA-2 polylactic resin, adopt the vacuum drum drying machine to be dried, 60 ℃ of baking temperatures, 8 hours drying times, moisture is less than 200ppm; Select the PLA-3 polylactic resin, adopt the vacuum drum drying machine to be dried, 50 ℃ of baking temperatures, 8 hours drying times, moisture is less than 200ppm; Dried above-mentioned three kinds of raw materials are pressed 20:50:30 mix, in 210 ℃ of lower meltings, filtration, quantitatively input filament spinning component through measuring pump, the spinnerets hole count is 11400, and the spinneret orifice profile is trilobal cross; Adopt the cooling air of 11 ℃ to carry out cooling forming, by finish oil disc, finish is coated in the tow surface; In being temporary in fiber barrel after under the coiling speed of 550m/min, tow being reeled; In the water-bath of 75 ℃, tow is carried out drawing-off, draft speed 100～200m/min, the drawing-off multiplying power is 2.3; Tow after counter extensioin carries out curling on crimping machine, and curling temperature is 90 ℃; Tow after curling enters drying and setting machine, and the drying and shaping temperature is at 65～75 ℃, drying and shaping time 12min; Finally, obtaining monofilament linear density is 3.4dtex, and tow line density is 3.89ktex, and crispation number is the PLA tow of 23/25mm.The moulding on the YL21 filter-stick forming device of this tow, triacetyl glycerine applied amount are the 8%wt of tow, and after filter stick solidified, filter stick hardness reached 88%.
Embodiment 7
Select the PLA-2 polylactic resin, adopt the vacuum drum drying machine to be dried, 60 ℃ of baking temperatures, 8 hours drying times, moisture is less than 200ppm; Select the PLA-3 polylactic resin, adopt the vacuum drum drying machine to be dried, 50 ℃ of baking temperatures, 10 hours drying times, moisture is less than 200ppm; Dried above-mentioned two kinds of raw materials are pressed 80:20 mix, in 210 ℃ of lower meltings, filtration, quantitatively input filament spinning component through measuring pump, the spinnerets hole count is 11400, and the spinneret orifice profile is trilobal cross; Adopt the cooling air of 11 ℃ to carry out cooling forming, by finish oil disc, finish is coated in the tow surface; In being temporary in fiber barrel after under the coiling speed of 550m/min, tow being reeled; In the water-bath of 75 ℃, tow is carried out drawing-off, draft speed 100～200m/min, the drawing-off multiplying power is 2.3; Tow after counter extensioin carries out curling on crimping machine, and curling temperature is 90 ℃; Tow after curling enters drying and setting machine, and the drying and shaping temperature is at 65～75 ℃, drying and shaping time 12min; Finally, obtaining monofilament linear density is 3.4dtex, and tow line density is 3.89ktex, and crispation number is the PLA tow of 23/25mm.The moulding on the KDF-2 filter-stick forming device of this tow, triacetyl glycerine applied amount are the 5%wt of tow, and after filter stick solidified, filter stick hardness reached 87%.
Embodiment 8
Select the PLA-1 polylactic resin, adopt the vacuum drum drying machine to be dried, 70 ℃ of baking temperatures, 8 hours drying times, moisture is less than 200ppm; Select the PLA-3 polylactic resin, adopt the vacuum drum drying machine to be dried, 50 ℃ of baking temperatures, 10 hours drying times, moisture is less than 200ppm; Dried above-mentioned two kinds of raw materials are pressed 70:30 mix, in 210 ℃ of lower meltings, filtration, quantitatively input filament spinning component through measuring pump, the spinnerets hole count is 11400, and the spinneret orifice profile is trilobal cross; Adopt the cooling air of 11 ℃ to carry out cooling forming, by finish oil disc, finish is coated in the tow surface; In being temporary in fiber barrel after under the coiling speed of 550m/min, tow being reeled; In the water-bath of 75 ℃, tow is carried out drawing-off, draft speed 100～200m/min, the drawing-off multiplying power is 2.3; Tow after counter extensioin carries out curling on crimping machine, and curling temperature is 90 ℃; Tow after curling enters drying and setting machine, and the drying and shaping temperature is at 65～75 ℃, drying and shaping time 12min; Finally, obtaining monofilament linear density is 3.4dtex, and tow line density is 3.89ktex, and crispation number is the PLA tow of 23/25mm.The moulding on the KDF-2 filter-stick forming device of this tow, triacetyl glycerine applied amount are the 5%wt of tow, and after filter stick solidified, filter stick hardness reached 87%.
Claims (4)
1. the PLA pipe tobacco of a modification, it is characterized in that: be to be mixed through heating and melting by two or more at least in PLA-1, PLA-2 and three kinds of raw materials of PLA-3, be prepared from through drawing-off, curling, drying and shaping operation, the ratio of three kinds of raw materials is that PLA-1: PLA-2: PLA-3 is 0-80%: 0-90%: 0-90%;
Described PLA-1: optical purity is 94-99%, the mol ratio of D-lactic acid unit is 97%-99.5%, and weight average molecular weight is 5-20 ten thousand, and melting range is 160-190 ℃, the melt melt index of measuring under loading with 2.16Kg at 190 ℃ is at 5-30g/10min, and degree of crystallinity is 35-55%;
Described PLA-2: optical purity is 50-82%, the mol ratio of D-lactic acid unit is 75-91%, and weight average molecular weight is 5-20 ten thousand, and melting range is 100-130 ℃, the melt melt index of measuring under loading with 2.16Kg at 190 ℃ is at 5-30g/10min, and degree of crystallinity is 2-12%;
Described PLA-3: optical purity is 0-20%, the mol ratio of D-lactic acid unit is 40-60%, and weight average molecular weight is 5-20 ten thousand, and melting range is 80-120 ℃, the melt melt index of measuring under loading with 2.16Kg at 190 ℃ is at 5-30g/10min, and degree of crystallinity is 0-5%.
2. the PLA pipe tobacco of modification according to claim 1, it is characterized in that: the ratio of three kinds of raw materials is that PLA-1: PLA-2: PLA-3 is 15-80: 15-80: 5-50.
3. the PLA pipe tobacco of modification according to claim 1 and 2 is characterized in that: the PLA cigarette of modification is to be prepared from by following concrete grammar with silk:
(1) will tie PLA-1 and be dried to moisture less than 200ppm, 60～120 ℃ of baking temperatures, 4～8 hours drying times, PLA-2 is dried to moisture less than 200ppm, 50～60 ℃ of baking temperatures, are dried to moisture less than 200ppm with PLA-3 simultaneously at 8～16 hours drying times, 50～60 ℃ of baking temperatures, 8～16 hours drying times;
Send into spinning system after above-mentioned three kinds of polylactic resin heating and meltings mix, in 190～220 ℃ of meltings, filtration, quantitatively input filament spinning component through measuring pump; Melt is extruded through spinnerets; The spinnerets hole count is 8000～15000, and the spinneret orifice profile is three leaves (Y) types;
(3) adopting process air-conditioning cold radiator cooler carries out cooling forming to new spun tow, 10～20 ℃ of cooling wind-warm syndrome; By the finish oil disc that rotates, finish is coated in the tow surface to improve rear road machinability;
In being temporary in fiber barrel after under suitable coiling speed, tow being reeled, coiling speed is controlled at 300～1500m/min;
In the water-bath of uniform temperature, tow is carried out drawing-off, drawing temperature is 50～90 ℃, and the drawing-off multiplying power is 2～3.5 times;
Tow after drawing-off enters crimping machine and carries out curlingly, and curling temperature is 85～95 ℃;
Obtain PLA pipe tobacco of the present invention after tow drying and shaping after curling, the drying and shaping temperature is at 60～90 ℃, drying and shaping time 10～15min.
4. method of utilizing the described PLA pipe tobacco of claim 1 to prepare filter stick, it is characterized in that: the PLA tow is carried out moulding by filter-stick forming devices such as YL21, KDF-2, KDF-3 or KDF-4, tow is after shredding, apply triacetyl glycerine as the filter stick plasticizer, the plasticizer addition is the 4-12%wt of tow by weight percentage, and the filter stick of preparation is put under normal temperature namely curable.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310048812.9A CN103103633B (en) | 2013-02-07 | 2013-02-07 | Modified polylactic acid filament bundle and filter rod used for cigarette and preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310048812.9A CN103103633B (en) | 2013-02-07 | 2013-02-07 | Modified polylactic acid filament bundle and filter rod used for cigarette and preparation method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103103633A true CN103103633A (en) | 2013-05-15 |
| CN103103633B CN103103633B (en) | 2015-02-04 |
Family
ID=48311814
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310048812.9A Active CN103103633B (en) | 2013-02-07 | 2013-02-07 | Modified polylactic acid filament bundle and filter rod used for cigarette and preparation method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103103633B (en) |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2015164447A3 (en) * | 2014-04-22 | 2016-01-07 | Fiber Innovation Technology, Inc. | Fibers comprising an aliphatic polyester blend, and yarns, tows, and fabrics formed therefrom |
| CN105755575A (en) * | 2016-03-02 | 2016-07-13 | 云南瑞升烟草技术（集团）有限公司 | Preparation method of color polylactic acid tows for cigarette and filter stick |
| CN106906529A (en) * | 2017-04-08 | 2017-06-30 | 河南省龙都生物科技有限公司 | A kind of leaf profiled filament production method of PLA three |
| CN108703412A (en) * | 2018-06-03 | 2018-10-26 | 上海同巽环保科技有限公司 | A kind of filter stick of safety and environmental protection and preparation method thereof |
| CN109123768A (en) * | 2017-06-19 | 2019-01-04 | 贵州中烟工业有限责任公司 | A method of control releasing content of coke tar in cigarette stability |
| CN110326815A (en) * | 2019-07-18 | 2019-10-15 | 深圳市华远新材料有限公司 | A kind of cigarette filter tip materials and preparation method thereof of low resistance to suction and high filtration |
| WO2021037145A1 (en) * | 2019-08-28 | 2021-03-04 | 深圳市智叶科技有限公司 | Preparation method for filter for electronic cigarette |
| WO2021037144A1 (en) * | 2019-08-28 | 2021-03-04 | 深圳市智叶科技有限公司 | Non-woven cotton filter tip and manufacturing method therefor |
| WO2024060501A1 (en) * | 2022-09-23 | 2024-03-28 | 云南中烟工业有限责任公司 | Preparation method for knife-hitting-preventing polylactic acid fiber filter stick |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1961765A (en) * | 2006-11-30 | 2007-05-16 | 中国科学院长春应用化学研究所 | A cigarette filter filament and preparation method thereof |
| CN101023811A (en) * | 2007-02-05 | 2007-08-29 | 中国科学院长春应用化学研究所 | Filtering rod for cigarette and preparing method |
| CN101805937A (en) * | 2010-03-18 | 2010-08-18 | 上海同杰良生物材料有限公司 | Filament bundle for degrading cigarette, preparation method thereof, and preparation method of filter stick |
| CN102493003A (en) * | 2011-11-04 | 2012-06-13 | 马鞍山同杰良生物材料有限公司 | Method for preparing environment-friendly cigarette tows |
| CN102704030A (en) * | 2012-06-14 | 2012-10-03 | 中国烟草总公司郑州烟草研究院 | Tow with high crimp index for polylactic acid cigarette and preparation method for tow |
-
2013
- 2013-02-07 CN CN201310048812.9A patent/CN103103633B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1961765A (en) * | 2006-11-30 | 2007-05-16 | 中国科学院长春应用化学研究所 | A cigarette filter filament and preparation method thereof |
| CN101023811A (en) * | 2007-02-05 | 2007-08-29 | 中国科学院长春应用化学研究所 | Filtering rod for cigarette and preparing method |
| CN101805937A (en) * | 2010-03-18 | 2010-08-18 | 上海同杰良生物材料有限公司 | Filament bundle for degrading cigarette, preparation method thereof, and preparation method of filter stick |
| CN102493003A (en) * | 2011-11-04 | 2012-06-13 | 马鞍山同杰良生物材料有限公司 | Method for preparing environment-friendly cigarette tows |
| CN102704030A (en) * | 2012-06-14 | 2012-10-03 | 中国烟草总公司郑州烟草研究院 | Tow with high crimp index for polylactic acid cigarette and preparation method for tow |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2015164447A3 (en) * | 2014-04-22 | 2016-01-07 | Fiber Innovation Technology, Inc. | Fibers comprising an aliphatic polyester blend, and yarns, tows, and fabrics formed therefrom |
| CN106232882A (en) * | 2014-04-22 | 2016-12-14 | 纤维创新技术公司 | The fiber comprising aliphatic polyester blend and the yarn, tow and the fabric that are formed by it |
| CN105755575A (en) * | 2016-03-02 | 2016-07-13 | 云南瑞升烟草技术（集团）有限公司 | Preparation method of color polylactic acid tows for cigarette and filter stick |
| CN105755575B (en) * | 2016-03-02 | 2018-08-07 | 云南瑞升烟草技术（集团）有限公司 | A kind of preparation method of cigarette colored polylactic acid tow and filter stick |
| CN106906529A (en) * | 2017-04-08 | 2017-06-30 | 河南省龙都生物科技有限公司 | A kind of leaf profiled filament production method of PLA three |
| CN109123768A (en) * | 2017-06-19 | 2019-01-04 | 贵州中烟工业有限责任公司 | A method of control releasing content of coke tar in cigarette stability |
| CN109123768B (en) * | 2017-06-19 | 2021-03-23 | 贵州中烟工业有限责任公司 | Method for controlling stability of tar release amount of cigarette |
| CN108703412A (en) * | 2018-06-03 | 2018-10-26 | 上海同巽环保科技有限公司 | A kind of filter stick of safety and environmental protection and preparation method thereof |
| CN110326815A (en) * | 2019-07-18 | 2019-10-15 | 深圳市华远新材料有限公司 | A kind of cigarette filter tip materials and preparation method thereof of low resistance to suction and high filtration |
| WO2021037145A1 (en) * | 2019-08-28 | 2021-03-04 | 深圳市智叶科技有限公司 | Preparation method for filter for electronic cigarette |
| WO2021037144A1 (en) * | 2019-08-28 | 2021-03-04 | 深圳市智叶科技有限公司 | Non-woven cotton filter tip and manufacturing method therefor |
| WO2024060501A1 (en) * | 2022-09-23 | 2024-03-28 | 云南中烟工业有限责任公司 | Preparation method for knife-hitting-preventing polylactic acid fiber filter stick |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103103633B (en) | 2015-02-04 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103103633B (en) | Modified polylactic acid filament bundle and filter rod used for cigarette and preparation method | |
| CN103074716B (en) | Sheath-core polylactic acid tobacco tow and filter stick and preparation method thereof | |
| CN102691121B (en) | Polylactic acid/polypropylene cigarette composite tow with sheath-core structure and preparation method thereof | |
| CN102080275B (en) | Biodegradable cigarette fiber material and cigarette filter | |
| CN104532386B (en) | Polylactic acid filter stick paper element and manufacturing method thereof | |
| US9119419B2 (en) | Filter material for a filter element of a smoking article, and associated system and method | |
| CN101023811A (en) | Filtering rod for cigarette and preparing method | |
| CN102080278B (en) | Biodegradable cigarette fiber material and cigarette filter | |
| CN102080276B (en) | Biodegradable cigarette fiber material and cigarette filter tip | |
| CN108642601A (en) | Polylactic acid crimps compound pipe tobacco of autoadhesion and preparation method thereof certainly | |
| CN102392316B (en) | Cigarette filter tow and preparation method thereof | |
| CN102493003B (en) | Method for preparing environment-friendly cigarette tows | |
| CN102704030A (en) | Tow with high crimp index for polylactic acid cigarette and preparation method for tow | |
| CN102948924A (en) | Composite filament strand filter tip for cigarettes | |
| CN101889732A (en) | Preparation method of polylactic acid fiber cigarette tows | |
| CN102516728A (en) | Modified polyactic acid composition for cigarette filter stick and preparation method thereof | |
| CN102499478B (en) | Filter tip stick and preparation method thereof | |
| WO2024114026A1 (en) | Cigarette structure with composite filter stick | |
| CN102697180A (en) | Compound filter tip bar and compound filter tip cigarette | |
| CN101624729B (en) | Preparation method of fiber for hydrophile type porous cigarette filter tip | |
| CN108642602A (en) | A kind of two-component pipe tobacco and preparation method thereof | |
| CN111109651B (en) | Preparation method of biodegradable composite fiber glue-free hollow filter stick | |
| CN1817937A (en) | Use of lactide acid polymer | |
| CN102763897B (en) | Method for making polylactic acid fiber filter stick | |
| CN102771893B (en) | Tip rod adopting chitosan fiber beams as filter materials and preparation method of tip rod |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CP01 | Change in the name or title of a patent holder |
Address after: 450001 No. 2 Fengyang Street, Zhengzhou High-tech Zone, Henan Province Co-patentee after: Jiangsu Heji Tobacco Material Co., Ltd. Patentee after: Zhengzhou Tobacco Research Institute of CNTC Co-patentee after: Hongta Tobacco (Group) Co., Ltd. Address before: 450001 No. 2 Fengyang Street, Zhengzhou High-tech Zone, Henan Province Co-patentee before: Jiangsu Tianshengda Group Wuxi New Synthetic Fibre Co., Ltd. Patentee before: Zhengzhou Tobacco Research Institute of CNTC Co-patentee before: Hongta Tobacco (Group) Co., Ltd. |
|
| CP01 | Change in the name or title of a patent holder |