CN103233290A - Preparation method for cellulose carbamate fiber tow for cigarette - Google Patents

Preparation method for cellulose carbamate fiber tow for cigarette Download PDF

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Publication number
CN103233290A
CN103233290A CN2013101257441A CN201310125744A CN103233290A CN 103233290 A CN103233290 A CN 103233290A CN 2013101257441 A CN2013101257441 A CN 2013101257441A CN 201310125744 A CN201310125744 A CN 201310125744A CN 103233290 A CN103233290 A CN 103233290A
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cellulose carbamate
preparation
spinning
pipe tobacco
fibre pipe
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CN2013101257441A
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CN103233290B (en
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汤炼
王云波
李道喜
李雅明
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Yunnan Ji Ji Packing Technology Co ltd
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HUBEI TIANSI TECHNOLOGY Co Ltd
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Abstract

The present invention provides a preparation method for cellulose carbamate fiber tow for cigarette. According to the method, cellulose carbamate with a viscosity-average molecular weight of 48000-100,000 and a nitrogen content of 0.1wt%-7.0wt% is dissolved in a mixed aqueous solution of sodium hydroxide and zinc oxide to give a spinning solution with a certain concentration; and by using a wet spinning technique for spinning, and a mixed solution of sulfuric acid, sodium sulphate and zinc sulphate as a regeneration bath, the cellulose carbamate fiber tow for cigarette is obtained from the spinning solution through several processes of spinning -spinning oil applying- drafting- crimping-drying. The filter rod produced by using the tow of the invention has obvious filtering effect on harmful substances in smoke, and can be used in cigarette to replace cellulose acetate fiber tow and acrylic fiber tow.

Description

A kind of preparation method of cellulose carbamate fibre pipe tobacco
Invention field
The present invention relates to a kind of preparation method of cellulose carbamate fibre pipe tobacco.
Background technology
Cigarette filter has very big effect to lowering harm and decreasing coking, raising cigarette quality, is an indispensable part in the production of cigarettes.At present, the filter stick material of using on the domestic market mainly contains acetate silk and polypropylene fibre tow.Acetate fiber contains functional groups such as a large amount of acyl groups, ether, and its water imbibition and chemisorbed performance are good, more easily form space network in the filter tip forming process, and its physical adsorbability is also better.But acetate silk is that the cellulose acetate with the production of high-quality timber is raw material, and the forest reserves of China are limited, and lumber quality also is not suitable for producing cellulose acetate, needs a large amount of cellulose acetate of import and cellulose acetate tow every year.Along with the enhancing day by day of environmental consciousness in the world wide, high-quality timber producing countries such as Canada have begun to limit deforestation, thereby cause being becoming tight supply day of the interior cellulose acetate of world wide and cellulose acetate tow.
Supply falls short of demand at domestic cellulose acetate tow, software engineering researchers invent the has been arranged polypropylene tows that uses in low-grade cigarette.But, to compare with cellulose acetate tow, polypropylene tows has big shortcoming, its absorption property is relatively poor, and filter effect is bad, is unfavorable for the lowering harm and decreasing coking of flue gas in the cigarette, and it derives from the non-renewable resources oil, does not meet global sustainable development and domestic national conditions.
Cellulose carbamate has and the similar backbone structure of cellulose acetate, also has good absorption property, compares with cellulose acetate, and the used cellulose carbamate esterification degree of tow is lower, easier degraded, and its biological recyclability is better.And the used raw material of cellulose carbamate comprises the cotton pulp dregs of rice, bamboo pulp, wood pulps etc., and raw material sources are very extensive.The production process of cellulose carbamate is very environmental protection also, pollution-free generation.
Worldwide, cellulose carbamate fibre has had a large amount of research, Finland Neste company has developed the cellulose carbamate staple fibre the earliest, be used for textiles, its patent US 4923979 has set forth relevant production process among the US 4639535, with cellulose carbamate dissolving, spinning, oven dry, cut-out finally obtain weaving staple fibre Cella.Poland Lodz chemical fibre research institute, German zimmer company also carried out the research of cellulose carbamate fibre, document Use of Minerals in Papermaking, 1998,207 ~ 21 and patent DE 10040341 in cellulose carbamate and fiber thereof are set forth, the production process that it adopts and Finland Neste company are similar, and the tow that obtains is not have the cellulose carbamate long filament that curls.The Donghua University of China, Xinjiang physics and chemistry institute of the Chinese Academy of Sciences, University Of Tianjin etc. also carried out the research of cellulose carbamate long filament, patent ZL1775810A, CN100516326C etc. also introduce the civilian long filament of cellulose carbamate, its production process is mainly dissolving, spinning, oven dry, the tow that the nothing that finally obtains is curled.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of cellulose carbamate fibre pipe tobacco.
This invention provides a kind of preparation method of brand-new pipe tobacco, cellulose carbamate through dissolving, spinning, oil, drawing-off, curl, operation such as oven dry, obtain the cellulose carbamate fibre pipe tobacco.
For achieving the above object, technical scheme of the present invention is: cellulose carbamate is dissolved in the solvent, obtains certain density spinning solution; Adopt the wet spinning technology to carry out spinning, spinning solution process spinning ~ oil ~ drawing-off ~ curl ~ several procedures of drying and shaping prepare the carbamate fibre pipe tobacco; Its preparation method may further comprise the steps, and carries out successively:
(1) cellulose carbamate is dissolved in the mixed aqueous solution of NaOH and zinc oxide spinning solution;
(2) adopt wet spinning equipment to carry out spinning and get the spinning tow, adopt the mixed solution of sulfuric acid, sodium sulphate, zinc sulfate to do the regeneration bath;
(3) the spinning tow oils by the mixture of edible non-ionic surface active agent, edible oil and water;
(4) use drawing roller that tow is carried out drawing-off;
(5) tow through drawing-off curls;
(6) tow after curling carries out drying and shaping, obtains the carbamate fibre pipe tobacco.
In the method for the present invention, the viscosity average molecular weigh of described cellulose carbamate is 48000 ~ 100000, and nitrogen content is 0.1wt% ~ 7.5wt%.
In the described step 1), in the mixed aqueous solution component of the NaOH of dissolving cellulos carbamate and zinc oxide, concentration sodium hydroxide is 4wt% ~ 15wt%, and the oxidation zinc concentration is 0 ~ 2.5 wt%.
Described step 2) in, the mass concentration that sulfuric acid in the mixed solution is bathed in regeneration is 3% ~ 15%, and the mass concentration of sodium sulphate is 0 ~ 50%, and the mass concentration of zinc sulfate is 0 ~ 15%.
Described step 2) in, the temperature that regeneration is bathed is 10 ~ 60 ℃.
Described step 2) in, spinning tow total linear density is 2.0 ~ 6.0ktex.
The finish composition is the mixture of edible non-ionic surface active agent, edible oil and water in the described step 3), wherein the edible non-ionic surface active agent is one or more the mixture in methyl p-hydroxybenzoate, ethyl-para-hydroxybenzoate, the propylparaben, edible non-ionic surface active agent mass concentration is 0.1% ~ 2.5%, the mass concentration of edible oil is 0.1% ~ 6.0%, and the mass concentration of water is 91.5% ~ 99%.
In the described step 3), the temperature of finish is 5 ~ 95 ℃.
In the described step 4), drafting multiple is 0.5 ~ 1.2%, and total linear density is 3.0 ~ 5.0ktex after the drawing-off.
In the described step 5), the crimping machine temperature is 50 ~ 270 ℃, and crispation number is 15 ~ 30/25mm.
In the described step 6), the drying and shaping temperature is 50 ~ 200 ℃, and the time is 1 ~ 60 minute.
Gained cellulose carbamate fibre pipe tobacco of the present invention, its basic parameter index can reach the requirement of pipe tobacco, is fit to suitability for industrialized production.
The present invention compared with prior art has following advantage:
1) has a large amount of hydroxyls and amide groups in the cellulose carbamate fibre pipe tobacco molecular chemistry main chain, has good chemical adsorptivity, can adsorb a large amount of harmful substances in the flue gas, and its strainability is good, can substitutes acetate silk and polypropylene fibre tow.
2) cellulose carbamate fibre pipe tobacco raw material sources are very extensive, and the cotton pulp dregs of rice, bamboo pulp, wood pulps etc. can be used for preparing cellulose carbamate.
3) cellulose carbamate fibre pipe tobacco degradation property is good, and its esterification degree is lower than acetate fiber, and easier natural degradation is a kind of degradation material of green.
4) cellulose carbamate fibre pipe tobacco preparation flow is succinct, and technological requirement is simple, product price ratio height, industrialization easily.
The specific embodiment
In order to understand the present invention better, further illustrate content of the present invention below in conjunction with embodiment, but content of the present invention not only is confined to the following examples.
Embodiment 1
The preparation mass concentration is that 12% NaOH and mass concentration are 1.0% zinc oxide aqueous solution, the cellulose carbamate of getting viscosity average molecular weigh 60000, nitrogen content 1.5wt% places above-mentioned solution, mixture places subzero 10 ℃ of low temperature stirring and dissolving, obtain the transparency cellulose carbamate solution, with this solution filter, after the deaeration as spinning solution.
Spinning solution carries out spinning at the R535 wet-spinning frame, and the spinnerets hole count is 11000 holes, and spinneret orifice is trilobal cross, and the mixed liquor that adopts mass concentration 5% sulfuric acid, 15% sodium sulphate, 80% water is bathed in regeneration, 40 ℃ of regeneration bath temperatures; Deionized water is adopted in washing, and water temperature is 50 ℃; Finish adopts the mixed liquor of mass concentration 0.5% edible non-ionic surface active agent methyl p-hydroxybenzoate, mass concentration 5.0% edible oil, 94.5wt% water, 50 ℃ of oil bath temperatures; Drafting multiple 1.1.
After oiling, tow enters crimping machine, 80 ℃ of crimping machine temperature, crimping wheel pressure 0.2Mpa.Enter in the continous track dryness finalization machine after curling, setting temperature is 110 ℃, and the time is 5min.
The cellulose carbamate fibre tow monofilament linear density 2.9dtex that obtains, filament strength 1.6cN/dtex, total linear density are 3.19ktex, 25/25mm of crispation number.
Embodiment 2
The preparation mass concentration is that 8% NaOH and mass concentration are 0.3% zinc oxide aqueous solution, the cellulose carbamate of getting viscosity average molecular weigh 100000, nitrogen content 2.7wt% places above-mentioned solution, mixture places subzero 10 ℃ of low temperature stirring and dissolving, obtain the transparency cellulose carbamate solution, with this solution filter, after the deaeration as spinning solution.
Spinning solution carries out spinning at the R535 wet-spinning frame, and the spinnerets hole count is 11000 holes, and spinneret orifice is trilobal cross, and the mixed liquor that adopts mass concentration 8% sulfuric acid, mass concentration 10% sodium sulphate, 82wt% water is bathed in regeneration, 45 ℃ of regeneration bath temperatures; Deionized water is adopted in washing, and water temperature is 50 ℃; Finish adopts the mixed liquor of mass concentration 0.5% edible non-ionic surface active agent ethyl-para-hydroxybenzoate, mass concentration 6.0% edible oil, 93.5wt% water, 55 ℃ of oil bath temperatures; Drafting multiple 0.7.
After oiling, tow enters crimping machine, 80 ℃ of crimping machine temperature, crimping wheel pressure 0.2Mpa.Enter in the continous track dryness finalization machine after curling, setting temperature is 150 ℃, and the time is 3min.
The cellulose carbamate fibre tow monofilament linear density 3.1dtex that obtains, filament strength 1.8cN/dtex, total linear density are 3.41ktex, 26/25mm of crispation number.
Embodiment 3
The preparation mass concentration is that 13% NaOH and mass concentration are 0.1% zinc oxide aqueous solution, the cellulose carbamate of getting viscosity average molecular weigh 66000, nitrogen content 3.5wt% places above-mentioned solution, mixture places subzero 10 ℃ of low temperature stirring and dissolving, obtain the transparency cellulose carbamate solution, with this solution filter, after the deaeration as spinning solution.
Spinning solution carries out spinning at the R535 wet-spinning frame, the spinnerets hole count is 11000 holes, spinneret orifice is trilobal cross, and the mixed liquor that adopts mass concentration 10% sulfuric acid, mass concentration 3% sodium sulphate, mass concentration 1% zinc sulfate, 86wt% water is bathed in regeneration, 25 ℃ of regeneration bath temperatures; Deionized water is adopted in washing, and water temperature is 55 ℃; Finish adopts the mixed liquor of mass concentration 1.5% edible non-ionic surface active agent propylparaben, mass concentration 9.5% edible oil, 89wt% water, 52 ℃ of oil bath temperatures; Drafting multiple 1.0.
After oiling, tow enters crimping machine, 85 ℃ of crimping machine temperature, crimping wheel pressure 0.2Mpa.Enter in the continous track dryness finalization machine after curling, setting temperature is 75 ℃, and the time is 13min.
The cellulose carbamate fibre tow monofilament linear density 3.2dtex that obtains, filament strength 1.7cN/dtex, total linear density are 3.52ktex, 25/25mm of crispation number.
Embodiment 4
The preparation mass concentration is 12.5% sodium hydroxide solution, the cellulose carbamate of getting viscosity average molecular weigh 76000, nitrogen content 3.1wt% places above-mentioned solution, mixture places subzero 10 ℃ of low temperature stirring and dissolving, obtain the transparency cellulose carbamate solution, with this solution filter, after the deaeration as spinning solution.
Spinning solution carries out spinning at the R535 wet-spinning frame, and the spinnerets hole count is 11000 holes, and spinneret orifice is trilobal cross, and regeneration is bathed and adopted mass concentration 8% sulfuric acid solution, 25 ℃ of regeneration bath temperatures; Deionized water is adopted in washing, and water temperature is 55 ℃; The mixed liquor of the mixture of finish employing mass concentration 1.5% edible non-ionic surface active agent methyl p-hydroxybenzoate and ethyl-para-hydroxybenzoate, mass concentration 9.5% edible oil, 89wt% water, 52 ℃ of oil bath temperatures; Drafting multiple 1.0.
After oiling, tow enters crimping machine, 85 ℃ of crimping machine temperature, crimping wheel pressure 0.2Mpa.Enter in the continous track dryness finalization machine after curling, setting temperature is 75 ℃, and the time is 13min.
The cellulose carbamate fibre tow monofilament linear density 3.0dtex that obtains, filament strength 1.6cN/dtex, total linear density are 3.3ktex, 24/25mm of crispation number.

Claims (11)

1. the preparation method of a cellulose carbamate fibre pipe tobacco is characterized in that, may further comprise the steps, and carries out successively:
(1) cellulose carbamate is dissolved in the mixed aqueous solution of NaOH and zinc oxide spinning solution;
(2) adopt wet spinning equipment to carry out spinning and get the spinning tow, adopt the mixed solution of sulfuric acid, sodium sulphate, zinc sulfate to do the regeneration bath;
(3) the spinning tow oils by the mixture of edible non-ionic surface active agent, edible oil and water;
(4) use drawing roller that tow is carried out drawing-off;
(5) tow through drawing-off curls;
(6) tow after curling carries out drying and shaping, obtains the carbamate fibre pipe tobacco.
2. the preparation method of a kind of cellulose carbamate fibre pipe tobacco according to claim 1 is characterized in that, the viscosity average molecular weigh of described cellulose carbamate is 48000 ~ 100000, and nitrogen content is 0.1wt% ~ 7.5wt%.
3. the preparation method of a kind of cellulose carbamate fibre pipe tobacco according to claim 1, it is characterized in that, in the described step 1), in the mixed aqueous solution component of the NaOH of dissolving cellulos carbamate and zinc oxide, concentration sodium hydroxide is 4wt% ~ 15wt%, and the oxidation zinc concentration is 0 ~ 2.5 wt%.
4. the preparation method of a kind of cellulose carbamate fibre pipe tobacco according to claim 1, it is characterized in that described step 2) in, the mass concentration that sulfuric acid in the mixed solution is bathed in regeneration is 3% ~ 15%, the mass concentration of sodium sulphate is 0 ~ 50%, and the mass concentration of zinc sulfate is 0 ~ 15%.
5. the preparation method of a kind of cellulose carbamate fibre pipe tobacco according to claim 1 is characterized in that, described step 2) in, the temperature that regeneration is bathed is 10 ~ 60 ℃.
6. the preparation method of a kind of cellulose carbamate fibre pipe tobacco according to claim 1 is characterized in that, described step 2) in, spinning tow total linear density is 2.0 ~ 6.0ktex.
7. the preparation method of a kind of cellulose carbamate fibre pipe tobacco according to claim 1, it is characterized in that, the finish composition is the mixture of edible non-ionic surface active agent, edible oil and water in the described step 3), wherein the edible non-ionic surface active agent is one or more the mixture in methyl p-hydroxybenzoate, ethyl-para-hydroxybenzoate, the propylparaben, edible non-ionic surface active agent mass concentration is 0.1% ~ 2.5%, the mass concentration of edible oil is 0.1% ~ 6.0%, and the mass concentration of water is 91.5% ~ 99%.
8. the preparation method of a kind of cellulose carbamate fibre pipe tobacco according to claim 1 is characterized in that, in the described step 3), the temperature of finish is 5 ~ 95 ℃.
9. the preparation method of a kind of cellulose carbamate fibre pipe tobacco according to claim 1 is characterized in that, in the described step 4), drafting multiple is 0.5 ~ 1.2, and total linear density is 3.0 ~ 5.0ktex after the drawing-off.
10. the preparation method of a kind of cellulose carbamate fibre pipe tobacco according to claim 1 is characterized in that, in the described step 5), the crimping machine temperature is 50 ~ 270 ℃, and crispation number is 15 ~ 30/25mm.
11. the preparation method of a kind of cellulose carbamate fibre pipe tobacco according to claim 1 is characterized in that, in the described step 6), the drying and shaping temperature is 50 ~ 200 ℃, and the time is 1 ~ 60 minute.
CN201310125744.1A 2013-04-12 2013-04-12 Preparation method for cellulose carbamate fiber tow for cigarette Active CN103233290B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112390281A (en) * 2020-10-30 2021-02-23 冉国庆 Method for recovering zinc oxide from Cellulose Carbamate (CC) fiber coagulation bath and application

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101889732A (en) * 2010-07-19 2010-11-24 湖北金叶玉阳化纤有限公司 Preparation method of polylactic acid fiber cigarette tows
CN102134758A (en) * 2010-01-27 2011-07-27 大亚科技股份有限公司 Method for preparing tows for modified cigarettes
CN102691125A (en) * 2012-06-19 2012-09-26 武汉大学 Method for preparing regenerated cellulose fibers with cellulose carbamate

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102134758A (en) * 2010-01-27 2011-07-27 大亚科技股份有限公司 Method for preparing tows for modified cigarettes
CN101889732A (en) * 2010-07-19 2010-11-24 湖北金叶玉阳化纤有限公司 Preparation method of polylactic acid fiber cigarette tows
CN102691125A (en) * 2012-06-19 2012-09-26 武汉大学 Method for preparing regenerated cellulose fibers with cellulose carbamate

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112390281A (en) * 2020-10-30 2021-02-23 冉国庆 Method for recovering zinc oxide from Cellulose Carbamate (CC) fiber coagulation bath and application

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Effective date of registration: 20240425

Address after: 650400 Dongyuan Ecological Food Processing Park, Daying Street Office, Fumin County, Kunming City, Yunnan Province

Patentee after: Yunnan Ji Ji Packing Technology Co.,Ltd.

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Address before: No. 9 Fulong Road, Xiaonan Economic Development Zone, Xiaogan City, Hubei Province, 432100

Patentee before: Hubei Tiansi Technology Co.,Ltd.

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