CN104746374B - The cigarette preparation method and application of sugarcane refined cellulose - Google Patents

The cigarette preparation method and application of sugarcane refined cellulose Download PDF

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Publication number
CN104746374B
CN104746374B CN201510129190.1A CN201510129190A CN104746374B CN 104746374 B CN104746374 B CN 104746374B CN 201510129190 A CN201510129190 A CN 201510129190A CN 104746374 B CN104746374 B CN 104746374B
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cellulose
sugarcane
bagasse
prehydrolysis
reconstituted tobacco
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CN104746374A (en
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曾健
徐峻
赵瑞峰
李军
饶国华
刘熙
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South China University of Technology SCUT
China Tobacco Guangdong Industrial Co Ltd
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South China University of Technology SCUT
China Tobacco Guangdong Industrial Co Ltd
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    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21CPRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C3/00Pulping cellulose-containing materials
    • D21C3/02Pulping cellulose-containing materials with inorganic bases or alkaline reacting compounds, e.g. sulfate processes
    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21CPRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C1/00Pretreatment of the finely-divided materials before digesting
    • D21C1/04Pretreatment of the finely-divided materials before digesting with acid reacting compounds
    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21CPRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C9/00After-treatment of cellulose pulp, e.g. of wood pulp, or cotton linters ; Treatment of dilute or dewatered pulp or process improvement taking place after obtaining the raw cellulosic material and not provided for elsewhere
    • D21C9/10Bleaching ; Apparatus therefor
    • D21C9/12Bleaching ; Apparatus therefor with halogens or halogen-containing compounds
    • D21C9/123Bleaching ; Apparatus therefor with halogens or halogen-containing compounds with Cl2O
    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21CPRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C9/00After-treatment of cellulose pulp, e.g. of wood pulp, or cotton linters ; Treatment of dilute or dewatered pulp or process improvement taking place after obtaining the raw cellulosic material and not provided for elsewhere
    • D21C9/10Bleaching ; Apparatus therefor
    • D21C9/12Bleaching ; Apparatus therefor with halogens or halogen-containing compounds
    • D21C9/14Bleaching ; Apparatus therefor with halogens or halogen-containing compounds with ClO2 or chlorites
    • D21C9/144Bleaching ; Apparatus therefor with halogens or halogen-containing compounds with ClO2 or chlorites with ClO2/Cl2 and other bleaching agents in a multistage process

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  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Wood Science & Technology (AREA)
  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Paper (AREA)

Abstract

The invention discloses a kind of cigarette preparation method and application of sugarcane refined cellulose, with bagasse as raw material, prehydrolysis, soda cooking and bleaching are carried out after bagasse is ground, then processed by alkali refining, produced and obtain cellulose.The cellulose makes an addition to offal slurry and offal slurry is manufactured paper with pulp obtain reconstituted tobacco paper substrate best in quality together.The invention provides the integrated artistic of science, using " acid prehydrolysis+alkalescence boiling+tri-stage bleaching ", preparative separation obtains refined sugarcane fibre element of a content of cellulose more than 90%.The refined sugarcane fibre element of gained obtains good application effect in terms of the preparation of reconstituted tobacco, is all had a clear superiority using the overall texture and oral cavity comfort level of the reconstituted tobacco of the cellulose.

Description

The cigarette preparation method and application of sugarcane refined cellulose
Technical field
The invention belongs to technical field of cigarette production, more particularly, to the cigarette preparation method of sugarcane refined cellulose And application.
Background technology
China is tobacco big country, and the annual production of cigarette and consumption are sure to occupy the first in the world, and the demand of production of cigarettes raw material is non- Chang Ju great.Reconstituted tobacco is laggard using the cigarette leftover bits and pieces such as offal, crumbled tobacco and discarded tobacco leaf or tobacco waste formula combination A kind of raw material of cigarette that row restructuring reproduction process processing manufacture is obtained.Paper process be prepare reconstituted tobacco important method it One, reconstituted tobacco referred to as this area research that suitable fiber prepares high-quality is added in offal, crumbled tobacco and discarded tobacco leaf Emphasis.
Sugarcane is the important sugar crop of China, and this area is being applied to prepare reconstruction for the bagasse after sucrose is squeezed The existing related research of tobacco leaf aspect, in particular with reference to the processing method of the dead meals such as offal, offal, by bagasse after extraction Slurrying obtains the slurries such as sugarcane slurry and offal, offal and compares 5 according to oven dry weight:95~30:70 ratio carries out compound sheet Obtain reconstituted tobacco.
But, bagasse belongs to skin, medullary substance and mixes, complex structure, and contained various composition is to reconstruction cigarette in sugarcane fibre The quality of leaf has different degrees of influence.Currently without on refining research of the sugarcane fibre element in terms of reconstituted tobacco is prepared Report.
The content of the invention
The technical problem to be solved in the present invention overcomes existing tobacco leaf production technical field to utilize technology to sugarcane fibre It is not enough, there is provided a kind of cigarette preparation method of sugarcane refined cellulose.A- can successfully be prepared using the inventive method fine Refined cellulose of the dimension cellulose content more than 92%.
Another technical problem to be solved of the present invention is to provide the refined cellulose answering in terms of reconstituted tobacco is prepared With for preferred reconstituted tobacco non-tobacco fiber provides technical support.
The purpose of the present invention is achieved by following technical solution:
A kind of preparation method of cigarette with sugarcane refined cellulose is provided, with bagasse as raw material, bagasse is ground laggard Row prehydrolysis, soda cooking and ODEp tri-stage bleachings, are then processed by alkali refining, are produced and are obtained purity more than 90% Cellulose.
Preferably, the cigarette is comprised the following steps with the preparation method of sugarcane refined cellulose:
S1. bagasse raw material is selected, removal of impurities is air-dried, powder is milled to;
S2. prehydrolysis:By the powder equilibrium water conten of S1 steps gained bagasse, water and acid solution are added, carried out under air-proof condition Hydrolysis, bagasse and liquid after hydrolysis terminates, extruded and collect waste liquid and obtain prehydrolysis sample in the lump, and prehydrolysis sample is washed Wash clean;
S3. boiling is carried out in pre-hydrolyzed solution caustic soda addition S2 step process crossed;
S4. the pre-hydrolyzed solution that will be crossed through S3 step process is through D0EpD1Tri-stage bleaching treatment, at the D0EpD1 tri-stage bleachings The process conditions of reason are:
D0:ClO21.0%, slurry dense 10%, temperature 60 C, time 60min;
Ep:NaOH 1.5%, H2O20.5%, slurry dense 10%, 65 DEG C of temperature, time 90min;
D1:ClO20.4%, slurry dense 10%, temperature 70 C, time 90min.
S5. alkali refining treatment obtains refined cellulose.
Boiling described in S3 is addition steam and appropriate caustic lye of soda, sealing strip in the prehydrolysis sample that S2 step process is crossed Cooking reaction is carried out under part, after cooking reaction terminates, paper pulp and liquid is separated, and pulp washing is clean.
Preferably, bagasse described in S1 uses the slag of the sugarcane of new platform sugar ROC16 kinds.
It is further preferred that the bagasse produces the slag of the sugarcane of new platform sugar ROC16 kinds using Guangxi province.
Preferably, powder described in S1 is 40~60 mesh.
Preferably, the condition of hydrolysis described in S2 is:Heating-up time be 60~70min, hydrolysising reacting temperature be 155~ 160 DEG C, soaking time is 60min, and liquor ratio is 1:6, the mass percent concentration of acid solution is 0.50~1.00%.
It is further preferred that the condition of hydrolysis described in S2 is:Heating-up time is 60~70min, hydrolysising reacting temperature It it is 155 DEG C, soaking time is 60min, liquor ratio is 1:6, the mass percent concentration of acid solution is 0.50%.
Preferably, the acid solution is sulfuric acid solution.
Preferably, the addition of alkali described in S5 is relative to the 13~19% of prehydrolysis sample quality, it is further preferable that described The addition of alkali is 17~19%.
Present invention simultaneously provides the application of the refined cellulose, specifically gained refined cellulose is added by different proportion It is added in offal slurry and offal slurry, prepares reconstituted tobacco paper substrate.
The treatment of the offal slurry and offal slurry is prepared with reference to prior art, the fiber being refining to obtain according to the inventive method Element:Offal is starched:The mass ratio of offal slurry is 10~40%:40~10%:50~60% ratio is matched and manufactured paper with pulp, and is obtained Reconstituted tobacco paper substrate.
It is further preferred that the cellulose being refining to obtain according to the inventive method:Offal is starched:Offal slurry mass ratio be 20%:20%:60% ratio is matched and manufactured paper with pulp, and obtains reconstituted tobacco paper substrate.
The present invention also provides a kind of reconstituted tobacco, with above-mentioned reconstituted tobacco paper substrate applied coating solution drying, the painting Cloth liquid is the concentrate of offal leaching liquor.
The beneficial effects of the invention are as follows:
The present invention, by providing targetedly handling process, gives full play of its comprehensive fiber with new platform sugar ROC16 as raw material Element, the advantage that hemi-cellulose content is high, various extract contents are relatively low, produce refined cellulose and provide a kind of preferred original for separation Material.
The invention provides the integrated artistic of science, using " acid prehydrolysis+alkalescence boiling+tri-stage bleaching ", prepare and divide From obtaining, refined sugarcane fibre of the a- content of cellulose more than 90% is plain.System of the refined sugarcane fibre element of gained in reconstituted tobacco Standby aspect obtains very well application effect well, using the reconstituted tobacco of the cellulose overall texture and oral cavity comfort level all Have a clear superiority.
Brief description of the drawings
Influence of Fig. 1 acid consumptions to hydrolysis pH value and yield.
Relation between Fig. 2 prehydrolysis yield and poly-pentose removal efficiency.
Influence of Fig. 3 base amounts to physical property of pulp.
Specific embodiment
Below in conjunction with the accompanying drawings the present invention is further illustrated with specific embodiment.Unless stated otherwise, the examination that the present invention is used Agent and raw material are this area reagent and raw material routinely purchased in market.Unless stated otherwise, the percentage being related in the embodiment of the present invention It is mass percent.
The raw material of embodiment 1 is selected
Physicochemical characteristics analysis experiment of the present invention by producing sugarcane fibre raw material with different regions carries out raw material selection. To exempt to repeat, the present embodiment only produces bagasse and Guangxi that the bagasse of the kind of cloud sugarcane 03, Guangdong produce Guangdong 00 kind of sugar with Yunnan The bagasse of new platform sugar ROC16 kinds is produced for raw material is illustrated.
1.1 laboratory apparatus
Plant pulverizer, precision electronic balance, Muffle furnace, water-bath, air dry oven, vacuum pump using circulatory water, rapid water Divide analyzer, electric hot plate, DR5000 spectrophotometers, Soxhlet extractor and other conventional analysis glasswares.
1.2 raw materials and treatment
Bagasse Material is provided by Yunnan sugar refinery, Guangdong sugar refinery and Guangxi sugar refinery respectively, raw material mass dryness fraction about 50%; SWBQ0010 special fibres raw material is provided by cigarette in Guangdong.Representative Bagasse Material is taken at random, is sieved with 8 mesh sieves after air-drying Except fragment and dust, about 200 grams of sugarcane fibres are then taken using quartering, be then milled to powder, mistake with plant pulverizer After sieve, 40~60 mesh powder are collected, be stored in equilibrium water conten in sealed plastic bag, bagasse chemical composition is analyzed for subsequent measurements When use.
1.3 experimental results
The sugarcane fibre of the kind and the chemical constituent analysis result of SWBQ0010 special fibres are listed in the table below in 1.
As it can be seen from table 1 the content of ashes that sugarcane fibre is produced in Yunnan is 1.24%, the ash content that sugarcane fibre is produced in Guangxi contains It is 0.75% to measure, and in three major production areas sugarcane fibres, the content of ashes highest of sugarcane fibre is produced in Yunnan.Because ash content is main Composition is the inorganic matter such as calcium, potassium, sodium, magnesium, manganese and phosphorus, silica, needed for these elements are plant growth nutrition, potassium ion It is relative benign to tobacco product that content is higher, and the increase of preservative water preperation can strengthen the firepower of holding of tobacco leaf, promote cigarette Cigarette is burnt, and then reduces cigarette tar content, improves the security of cigarette.In YC/T 16.3-2003《Reconstituted tobacco the 3rd Point:Paper process》In, also using potassium content as one of its characteristic index, therefore ash content to sugarcane fibre in reconstituted tobacco should With not constituting negative effect.But, content of ashes especially metal ion content too high sample high, the color of ashes after burning Obfuscation;In addition, ash content is high and can cause fiber separation subtractive process pipeline scale and cause difficulty to devil liquor recovery.Therefore, from ash Divided by it is poor with respect to Guangxi, Guangdong product sugarcane fibre that sugarcane fibre is produced in Yunnan.
The chemical constituent of the Yunnan Province of table 1 representativeness sugarcane fibre raw material
From the point of view of the content of the big component fibre element of 1 sugarcane fibre of table three, hemicellulose and lignin, it is comprehensive that sugarcane fibre is produced in Yunnan Cellulose, hemicellulose, the content of total lignin are respectively 70.24%, 25.56%, 19.86%, and its holocellulose content is three Minimum among person, hemicellulose level is then highest among three, shows that the content of cellulose of sugarcane fibre is produced most in Yunnan It is few.If using sugarcane fibre separation and purification sugarcane fibre element, yield is relatively low, and production cost is of a relatively high.Hemicellulose splits Solution can produce irritating heat-decomposing compound (for example producing more low-grade aldehydes), and irritating choking can be caused when burning and sucking Cough, thus the low raw material of hemicellulose level, its quality is preferable.As can be seen here, from economy point and product quality angle, cloud Produce sugarcane fibre and produce sugarcane fibre not as good as Guangxi, Guangdong in south.In addition, as can also be seen from Table 1, the hot water of sugarcane fibre is produced in Yunnan Extract content is that 25.62%, 1%NaOH extracts are that 40.61%, alcohol-benzene extractive content is 1.85%;Each extract Content is above Guangdong, Guangxi and produces sugarcane fibre.These components, during cellulose is separated, the overwhelming majority can all degrade Dissolution.The chemicals consumption of sugarcane fibre subtractive process, therefore the low original of extract content can be increased due to the presence of which Material, quality is preferable, namely the inferior quality of sugarcane fibre is produced in Yunnan.Therefore, chemically for composition analysis result, Yunnan is produced sweet The quality of sugarcane fiber is lower than Guangdong, Guangxi product sugarcane fibre quality.
As can also be seen from Table 1, Sugarcane in Guangdong fiber holocellulose content, hemicellulose, acid-insoluble lignin, total lignin Content is respectively 77.20%, 23.30%, 20.27% and 21.56%, wherein the content of hemicellulose and acid-insoluble lignin, total Lignin content (including acid soluble lignin) is above Guangxi sugarcane fibre.Hemicellulose and the low raw material of lignin content, its quality compared with Get well, namely the quality of Sugarcane in Guangdong fiber is poor compared with Guangxi sugarcane fibre.
As can also be seen from Table 1, hot water extract's content of Sugarcane in Guangdong fiber is that 16.96%, 1%NaOH extracts are 37.02%th, alcohol-benzene extractive content is 1.35%;The content of each extract is above Guangxi sugarcane fibre.These components, are dividing During cellulose, most dissolutions that can all degrade.Because the presence of which can increase sugarcane fibre subtractive process Chemicals is consumed, therefore the low raw material of extract content, quality preferably, namely Sugarcane in Guangdong fiber quality compared with Guangxi sugarcane Fiber is poor.
In sum, chemically for composition analysis result, the quality that sugarcane fibre is produced in Guangxi is produced than Guangdong and Yunnan Sugarcane fibre quality is high.
The sugarcane fibre of embodiment 2 is plain to be refined
S2. prehydrolysis
1. laboratory apparatus
ZT1-00 type 15L electric cooking pots (match somebody with somebody 4 1L canisters), accurate pH meter, electronic balance, water-bath, forced air drying Case, vacuum pump using circulatory water, fast tester for water content, electric hot plate, DR5000 spectrophotometers, Soxhlet extractor and other routines point Analysis glassware.
2. raw material and treatment
The wet feed after 100 grams of equilibrium water contens of over dry is weighed, then water or acid solution needed for being added by the process conditions of table 2 fill Enter canister, be transferred in digester after sealing, then reacted with a temperature of in the heating curve for setting.After reaction terminates, by sugarcane Slag and liquid are moved into 200 mesh Nylon Bags in the lump, extrude and collect waste liquid, then will hydrolyze sample washes clean, are used for analysis.
The bagasse clear water of table 2/weak acid pre-hydrolysis technique condition
Note:Heating-up time is 60~70min.
3. experimental result
3.1 hydrolysis sample chemical constituent analyses
Hydrolysis sample is processed by preceding method, the sample chemical constituent that is hydrolyzed analysis, experimental results are listed in table 3 and table 4 In.
The different hydrolysis process gained hydrolysis sample yield of table 3, pH value and ash content
Note:Absolute magnitude is actual content of the component in sample is hydrolyzed;
Relative quantity=absolute magnitude × hydrolysis yield;
Relative quantity/the component of extrusion rate=1- components content in the feed
Can be seen that sour consumption is higher from table 3 and Fig. 1, the pH of hydrolytic process is lower, hydrolysis yield is lower;Hydrolysis temperature Higher, the pH of the hydrolytic process under the same terms is lower, hydrolysis yield is also lower.But from the point of view of comparing, difference is not very bright It is aobvious.
From the point of view of the change of ash content, with the increase of sour consumption, ash content abjection is taken the lead in slightly increasing, and then reduces, and acidity is got over By force, ash content extrusion rate is lower;And hydrolysis temperature abjection ratio higher is bigger.This influence of explanation temperature to ash content is greater than acid The influence of catalysis, and acidity is stronger, the abjection to ash content is on the contrary unfavorable.
From table 4, it can be seen that in the case of other experiment condition identicals, with the increase of acid concentration, hydrolyzing sample poly- penta The removal efficiency of sugar is significantly improved, and cellulose loss rate increases, hydrolysis yield reduction.(the experiment number 1 under conditions of not acid adding With experiment number 4), because under high-temperature and high-pressure conditions, water can dissociate H+And OH-, destroy hemicellulose oxy-acetyl and furfural acid Substituent, generates organic acid, and then promotes the degraded dissolution of hemicellulose by self-catalyzed reaction.But contrast experiment number 1 and reality The number of testing 2, is hydrolyzed using anacidity self-catalysis, and experiment poly-pentose extrusion rate is low, and only 21.80%, and after the acid of addition 0.5%, Poly-pentose extrusion rate, up to 85.25%, is the former 3.9 times in experiment;This shows that in pre-hydrolysis process acid is to hemicellulose Dissolution serves catalytic action.Because hemicellulose molecule contains free hydroxyl group, it is a kind of polar group, with hydrophilic Property, thus it is soluble in water.Its degree of polymerization is relatively low, and generally without crystal structure, arrangement is loose, is easily hydrolyzed under acid environment. When being hydrolyzed using dilute sulfuric acid, the H that acid is dissociated in water+H can be combined into water3O+, glucosides in hemicellulose molecule can be made The oxygen atom protonation of key, forms conjugate acid, and be broken because bond energy weakens.The carbonium ion of end can produce matter again after fracture Son, proton reacts with water, generates new water and hydrogen ion, participates in new hydrolysis.Therefore, it is acid-hydrolyzed to hemicellulose Solute effect is hydrolyzed more than self-catalysis.But the increase of acid concentration, helps little to the extrusion rate of poly-pentose, such as acid concentration from 0.5% brings up to 1.0%, and the poly-pentose extrusion rate of experiment number 3 only improves 0.66%, the poly-pentose of experiment number 6 than experiment number 2 Extrusion rate only improves 0.29% than experiment number 2.
Influence of the different hydrolysis process of table 4 to hydrolysis sample carbohydrate
In addition, as can also be seen from Table 4, in the case of other experiment condition identicals, with the raising of temperature, hydrolyzing sample Poly-pentose removal efficiency slightly has raising, but hydrolysis yield is then significantly reduced, and holocellulose loss late is dramatically increased.Such as in temperature 155 DEG C, sulfuric acid concentration 0.5% when, poly-pentose removal efficiency be 85.52%, prehydrolysis yield, holocellulose loss late are respectively 66.09% and 36.09%.Under similarity condition, temperature lifting to 160 DEG C, hydrolysis sample poly-pentose removal efficiency improve only 3.62%, but its hydrolysis yield then have dropped 4.87%, and holocellulose loss late increased 4.71%, exceed poly-pentose Extrusion rate.This is because under higher temperature, prehydrolysis reaction aggravates, and carbohydrate is drastically degraded, and makees in inorganic acid Under, the activation energy reduction of glucoside bond causes cellulose dissolution rate to be accelerated.
Accompanying drawing 2 shows the relation of prehydrolysis yield and poly-pentose clearance.From accompanying drawing 2, the yield of prehydrolysis with The increase of poly-pentose clearance and reduce.But according to the difference of its amplitude for reducing, 2 intervals can be divided into.Poly-pentose is removed Rate is interval A 0~85%.This interval yield can use linear equation Y=98.0096- with the relation of poly-pentose removal efficiency 0.373X is represented.Herein in interval, yield declines more slow, poly-pentose removing about 85%, and yield only reduces about 25%.Poly- penta Sugared removal efficiency is interval B 85%~90%.Herein in interval.Yield can use linear equation with the relation of poly-pentose removal efficiency Y=176.145-1.291X represents that its slope is 3.46 times of interval A.This explanation in interval 2, prehydrolysis yield decline compared with Hurry up, the removing of poly-pentose is extremely difficult, it is necessary to sacrifice yield as cost.Herein in interval, poly-pentose removal efficiency is not enough 4%, and yield reduces about 5%.As the above analysis, interval A slopes are smaller, are the optimum interval of pretreatment.To sum up institute State, the preferred process condition that choice experiment 2 is processed as bagasse prehydrolysis.Now, prehydrolysis yield is 66.09%, poly-pentose Removal efficiency is 85.25%.
Influence of the different hydrolysis process of table 5 to hydrolysis sample trees cellulose content
As can be seen from Table 5, lignin there occurs different degrees of degraded dissolution in pre-hydrolysis process.For sour insoluble wood Element, acid stronger, temperature is higher, and the lignin of dissolution is more;For acid soluble lignin, then a large amount of dissolutions, it is left that extrusion rate reaches 50% The right side, because whether self-catalysis or acid-catalyzed hydrolysis, the pH of pre-hydrolysis process is in acid (being shown in Table 3).
3rd, the new platform sugar ROC16 sugarcane fibres hydrolysis sample in Guangxi province separates the research experiment of cellulose
1. laboratory apparatus
Horizontal rotates boiling vessel KRK 2611 (volume is 4L), oscillatory type flat screen, Mark V1 type PFI defibrinations Machine, Xiao's Bai Shi Schooper-Riegler beating degree testers, paper sheet formation system and equipment, L&W062 tensile strength testers, L&W180 bursting strength instrument, L& W09 tearability instrument, YQ-Z-48B whiteness instrument, pH meter, electric mixer, small-sized wet pulp dissociation device, stopwatch, electronic balance, experiment Commonly use general glassware in room.
2. experimental raw and treatment
Soda cooking and D0EpD1 tri-stage bleachings are carried out to amplification test gained prehydrolysis sample, then gained slurry is entered Row mashing, handsheet, then determine the strength character of page.
3. experimental result
3.1 hydrolysis sample soda pulping processes
Slurrying is carried out according to the technique of table 6, acquired results and characteristics of pulp are shown in Table 6 and table 6.
Influence of the base amount of table 6 to prehydrolysis sugarcane fibre pulpability
* with respect to yield=paper pulp yield × hydrolysis yield;
Other techniques:160 DEG C of temperature, intensification 60min is incubated 60min, liquor ratio 1:4.
As can be seen from Table 6, paper pulp yield is reduced with the increase of alkali charge, such as when base amount is 13% and 19% Paper pulp yield is respectively 50.63% and 46.44%, reduces 8.28%;But 30.68% then is down to from 33.45% with respect to yield, Reduce about 2.8%;At the same time pulp hardness (Kappa number) is then down to 10.63% from 92.21.From black liquor pH value and black liquor From the point of view of solid content, alkali charge is crossed, and the pH value of black liquor is higher, and solid content is also higher, and this reflects that base amount is bigger, The material of dissolution is more, and this is also the reason for yield is gradually reduced.From the point of view of pulp brightness, alkali charge is higher, and whiteness is higher.When Alkali charge is less than 15%, and pulp brightness is no more than 30%ISO;When alkali charge reaches 17%, now pulp brightness reaches 35.5% ISO, continues to increase base amount to 19%, and whiteness is further increased to 43.3%ISO.Beating degree has reacted the wire-dividing broom purification of slurry Degree, as can be seen from Table 6, base amount is bigger, and the swollen of slurry, wire-dividing broom purification are more obvious, shows as the rising of beating degree.
The brown stock physical property of table 7
For paper grade pulp, tensile index is higher, paper pulp intensity is better.But for reconstituted tobacco (YC/T16.3- 2003), its tensile strength requirement is no more than 1.0kN/m.Therefore, want the ratio of paper pulp in raising reconstituted tobacco, reduce additional The tensile strength of paper pulp is one of necessary means.From table 7 from the point of view of physical property, preprocessed repulping gained brown stock intensity It is relatively low, by quantitative 110g/m2Calculate, between 2.75~3.30kN/m, this is very beneficial for improving the tensile strength of brown stock Its adding proportion in reconstituted tobacco.
Accompanying drawing 3 is described without under base amount, the variation tendency of physical property of pulp.From accompanying drawing 3 as can be seen that alkali is used Amount improves 15% from 13%, and each intensity index of paper pulp has a raising;Continue to improve base amount to 17%, each intensity index Then it is remarkably decreased, then continues to increase base amount, each index then changes unobvious.
Comprehensive analysis, base amount is proper between 17~19%.
The bleaching characteristic of 3.2 hydrolysis sample alkaline pulps
Choose 4#Sample carries out D by following techniques0EpD1Tri-stage bleaching, gained bleached cellulose pulp characteristic is listed in Table 8 below.
Bleaching process:
D0:ClO21.0%, slurry dense 10%, temperature 60 C, time 60min;
Ep:NaOH 1.5%, H2O20.5%, slurry dense 10%, 65 DEG C of temperature, time 90min;
D1:ClO20.4%, slurry dense 10%, temperature 70 C, time 90min.
The bleached cellulose pulp characteristic of table 8
From the point of view of the characteristic of the bleached cellulose pulp of table 8, through bleaching, pulp brightness reaches 85.9%ISO, with commodity Bleached wood pulp whiteness is close.Every intensity index of paper pulp slightly has improvement, this removal for being mainly due to fiber fines and fiber The brooming of element.From the point of view of viscosity, bleaching viscosity has declined.From the point of view of a- content of cellulose, by pretreatment, brown stock Slightly improved after being above 90%, and bleaching with the cellulose purity of bleached pulp.
All in all, using " acid prehydrolysis+alkalescence boiling+ECF is bleached ", can be existed with isolated a- content of cellulose 90~92% or more refined cellulose.
Embodiment 3 refine sugarcane fibre element with copy experiment and sensory evaluating smoking experiment
1. laboratory apparatus
Horizontal rotates boiling vessel KRK 2611 (volume is 4L), oscillatory type flat screen, thermostat water bath, BBS types Quick kayser method handshcet former, YQ-Z-48B whiteness instrument, general glassware is commonly used in electric mixer, electronic balance, laboratory.
2. experimental raw and treatment
According to the inventive method, with Guangxi sugarcane fibre as raw material, prehydrolysis-soda cooking and three sections of drifts are carried out to it In vain, then processed by alkali refining, produce cellulose of the purity more than 92%.Then it is added to cigarette by different proportion In stalk, offal, reconstituted tobacco paper substrate is prepared, send Guangdong China Tobacco Industry Co., Ltd technique center to carry out sensory evaluating smoking.
3. experimental result
Offal, the treatment of offal are prepared with reference to other item optimization techniques, the sugarcane fibre of different cellulose purities First it is beaten to 32~35 ° of SR with other paper pulp fibers, then the proportioning of according to the form below 9 carries out reconstituted tobacco paper substrate and manufactures paper with pulp.
The reconstituted tobacco paper substrate sample fiber of table 9 matches table
Sample number into spectrum Plus fiber Addition/% Offal addition/% Offal addition/%
A Needlebush pulp 6 65.8 28.2
B Bamboo pulp 6 65.8 28.2
C Poplar is starched 6 65.8 28.2
D Bagasse pulp 6 65.8 28.2
E Bagasse pulp 8 64.4 27.6
F Refined sugarcane fibre element 6 65.8 28.2
G Bagasse pulp 100 0 0
H Bagasse pulp 100 0 0
Control sample GD-125 paper substrates
To above-mentioned sample, organizes expert carries out experiment of smokeing panel test, and smoking result is as follows:
A:Flue gas concentration is higher, and the texture of flue gas is general, and wooden breath is heavier, and the calcination in oral cavity, stimulation are larger, and drying is bright Aobvious, comfort level is poor.
B:Flue gas concentration is higher, and the texture of flue gas is general, and slightly, the peppery sense of lingual surface thorn is obvious for miscellaneous gas, dries and residual compares Substantially, comfort level is poor.
C:Flue gas concentration is higher, and the texture of flue gas is poor, and miscellaneous gas is more apparent, and the stimulation in nasal cavity and oral cavity is more apparent, comfortably Degree is poor.
D:Flue gas concentration is moderate, and flue gas entirety texture E is more or less the same, and oral cavity slightly stimulates and dry sensation.
E:Flue gas concentration is moderate, and flue gas entirety texture is slightly inferior to F, and the muddiness of flue gas is more obvious than F, and the burning sensation in oral cavity compares F Greatly.
F:Flue gas concentration is moderate, and the texture of flue gas is relatively preferable, Wei You xylon gas, and oral cavity is micro- sweet sense, and comfort level is relative Preferably, oral stimulation and dry sensation are little.
G:Flue gas concentration is higher, and the texture of flue gas is poor, and the stimulation in oral cavity and residual are more apparent.
H:Flue gas concentration is (being slightly decreased with respect to G) higher, and the texture of flue gas is poor, and the stimulation in oral cavity and residual are more apparent.
GD-125 paper substrates:Flue gas concentration is in a slight decrease, and still, wooden miscellaneous gas relatively appears the texture of flue gas, and lingual surface is micro- hardship Taste, peppery sense, the stimulation in oral cavity and dry sensation are larger.
In general, sugarcane fibre is added in reconstituted tobacco paper substrate (E, F) as plus fiber, than needlebush (A), wealthy Ye Mu (C), bamboo pulp (B) are added in reconstituted tobacco paper substrate as plus fiber, the overall texture of sugarcane fibre sample and oral cavity Comfort level all has a clear superiority;Compared with GD-125 paper substrates simultaneously, lifting of the sugarcane fibre reconstituted tobacco sample in flue gas texture Miscellaneous gas aspect is also advantageous with reducing.The sample overall quality of the refined sugarcane fibre element of the addition present invention is significantly improved.
Embodiment 4 refine sugarcane fibre element with copy experiment and sensory evaluating smoking experiment
1. laboratory apparatus
Horizontal rotates boiling vessel KRK 2611 (volume is 4L), oscillatory type flat screen, thermostat water bath, BBS types Quick kayser method handshcet former, YQ-Z-48B whiteness instrument, general glassware is commonly used in electric mixer, electronic balance, laboratory.
2. experimental raw and treatment
According to the inventive method, with Guangxi sugarcane fibre as raw material, prehydrolysis-soda cooking and three sections of drifts are carried out to it In vain, then processed by alkali refining, produce cellulose of the purity more than 92%.Then it is added to cigarette by different proportion In stalk, offal, reconstituted tobacco paper substrate is prepared, send Guangdong Tobacco Company to carry out sensory evaluating smoking.
3. experimental result
The ratio of offal and offal is adjusted to 5:5, refined sugarcane fibre element is mainly used in substituting tobacco stalk fibre.Coating fluid is The extraction concentrate of gained after offal and offal extraction, spreading rate is about 35%.The reconstituted tobacco paper substrate sample of according to the form below 10 is fine Dimension proportioning, carries out the preparation of reconstituted tobacco paper substrate and dip-coating sample, then carries out sensory evaluating smoking.
The reconstituted tobacco paper substrate sample fiber of table 10 matches table
To above-mentioned sample, organizes expert carries out endoplasm and smokes panel test, and smoking result is as follows:
(1) reconstituted tobacco paper substrate sample
A-w (control sample):Flue gas concentration is moderate, and still, wooden miscellaneous gas is slightly obvious, oral cavity, the thorn of lingual surface for the texture of flue gas Swash slightly, global comfort is fine.
B-w:Flue gas concentration has lifting compared with the texture that control sample has lifting, flue gas compared with control sample, and wooden miscellaneous gas is smaller, oral cavity Micro- to have sweet sense, nasal cavity stimulates slightly, and global comfort is fine.
C-w:The upper sample of flue gas concentration is micro- lifting, and preferably, wooden miscellaneous gas is smaller, the sweet sense in oral cavity for the texture of flue gas More apparent, slightly, global comfort is fine for drying, the stimulation in oral cavity.
E-w:Flue gas concentration is higher, and still, sugarcane fibre breath slightly appears the texture of flue gas, and slightly, oral cavity is micro- to be had miscellaneous gas Sweet sense, the drying in oral cavity, stimulation are more apparent, and global comfort is slightly worse.
G-w:Flue gas concentration is moderate, and the texture of flue gas is slightly worse, and sugarcane fibre breath is more apparent, and miscellaneous gas is larger, oral cavity it is dry Dry, stimulation is more apparent, and global comfort is slightly worse.
H-w:Flue gas concentration is fitted, and the texture of flue gas has lifting compared with control sample, and wooden miscellaneous gas is smaller, and the sweet sense in oral cavity is more apparent, The stimulation in oral cavity is smaller, and drying is more apparent, and global comfort is fine.
(2) reconstituted tobacco sample
A-t (control sample):Flue gas concentration is moderate, and still, perfume quantity is medium for the texture of flue gas, and smoke behavior is preferably, wooden Miscellaneous gas is smaller, and dried-up miscellaneous gas is more apparent, and slightly, global comfort is fine for drying, the stimulation in oral cavity.
B-t:Flue gas concentration is moderate, and the texture of flue gas has lifting compared with control sample, and perfume quantity is medium, and smoke behavior is preferably, miscellaneous Gas is smaller, and somewhat there is sweet sense in oral cavity, and nasal cavity stimulates more apparent, and global comfort is slightly worse.
C-t:Flue gas concentration has lifting compared with control sample, and preferably, perfume quantity is medium on the upper side for the texture of flue gas, the softer silk floss of flue gas, Exquisiteness, wooden miscellaneous gas is smaller, and the sweet sense in oral cavity is more apparent, and the drying in oral cavity, stimulation are smaller, and global comfort is preferable.
E-t:Flue gas concentration is moderate, and still, perfume quantity is medium for the texture of flue gas, smoke behavior preferably, wooden miscellaneous gas slightly, Dried-up miscellaneous gas is micro- to be had, and the drying of oral cavity and nasal cavity, stimulation are more apparent, and global comfort is slightly worse.
G-t:Flue gas concentration is medium on the upper side, and still, perfume quantity is medium for the texture of flue gas, and smoke behavior is preferable, wooden miscellaneous gas Larger, the drying in oral cavity, stimulation are larger, and global comfort is poor.
H-t:Flue gas concentration is higher, and preferably, perfume quantity is medium on the upper side for the texture of flue gas, and smoke behavior is preferable, wooden miscellaneous gas Larger, the drying in oral cavity, stimulation are larger, and global comfort is poor.
From the point of view of above-mentioned smoking result, sugarcane refined cellulose replaces tobacco stalk fibre as plus fiber, is replaced with 20% Generation amount is preferable, and sensory evaluating smoking's effect of reconstituted tobacco paper substrate and reconstituted tobacco is preferable.

Claims (3)

1. application of a kind of sugarcane refined cellulose in terms of reconstituted tobacco, it is characterised in that be by refined cellulose:Offal Slurry:Offal slurry is 20% according to mass ratio:20%:60% ratio is matched and manufactured paper with pulp, and prepares reconstituted tobacco paper substrate;It is described Refined cellulose is prepared by following steps:
S1. bagasse raw material is selected, removal of impurities is air-dried, powder is milled to;
S2. prehydrolysis:By the powder equilibrium water conten of S1 steps gained bagasse, water and acid solution are added, be hydrolyzed under air-proof condition Reaction, bagasse and liquid after hydrolysis terminates, extruded and collect waste liquid and obtain prehydrolysis sample in the lump, and the washing of prehydrolysis sample is dry Only;
S3. boiling is carried out in caustic soda being added into pre-hydrolyzed solution;
S4. the pre-hydrolyzed solution that will be crossed through S3 step process is through D0EpD1Tri-stage bleaching treatment, the D0EpD1Tri-stage bleaching treatment Process conditions are:
D0:ClO21.0%, slurry dense 10%, temperature 60 C, time 60min;
Ep:NaOH 1.5%, H2O20.5%, slurry dense 10%, 65 DEG C of temperature, time 90min;
D1:ClO20.4%, slurry dense 10%, temperature 70 C, time 90min;
S5. alkali refining treatment obtains refined cellulose;
The condition of hydrolysis described in S2 is:Heating-up time is 60~70min, and hydrolysising reacting temperature is 155~160 DEG C, insulation Time is 60min, and liquor ratio is 1:6, the mass percent concentration of acid solution is 0.50~1.00%;
The acid solution is sulfuric acid solution;
The bagasse uses the slag of the sugarcane of the new platform sugar ROC16 kinds of Guangxi province;
The addition of caustic soda described in S3 steps is relative to the 13~19% of prehydrolysis sample quality.
2. application according to claim 1, it is characterised in that hydrolysising reacting temperature described in step S2 is 155 DEG C, acid solution Mass percent concentration is 0.50%.
3. application according to claim 1, it is characterised in that the addition of caustic soda described in step S3 is 17~19%.
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