CN104746374A - Preparation method and application of sugarcane refined cellulose for tobaccos - Google Patents

Preparation method and application of sugarcane refined cellulose for tobaccos Download PDF

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Publication number
CN104746374A
CN104746374A CN201510129190.1A CN201510129190A CN104746374A CN 104746374 A CN104746374 A CN 104746374A CN 201510129190 A CN201510129190 A CN 201510129190A CN 104746374 A CN104746374 A CN 104746374A
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sugarcane
cellulose
offal
refined cellulose
preparation
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CN104746374B (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 preparation method and application of sugarcane refined cellulose of tobaccos. The preparation method takes begasse as raw materials; the begasse is crushed and then pre-hydrolyzed, cooked with a caustic soda method and bleaching; and the materials are subjected to alkali refining treatment to prepare the cellulose. The cellulose is added into tobacco stem pulp and waste tobacco pulp, and then the mixture is used for making paper to obtain a regenerated tobacco leaf paper base with good quality. A scientific whole process is provided and a process including acid prehydrolysis, alkaline cooking and three-section bleaching is adopted to prepare the refined sugarcane cellulose with the content of alpha-cellulose of more than 90% in a separation manner. The obtained refined sugarcane cellulose has a good application effect in the aspect of the preparation of regenerated tobacco leaves and the whole quality and oral cavity comfort of the regenerated tobacco leaves adopting the cellulose have obvious advantages.

Description

The cigarette preparation method of sugarcane refined cellulose and application
Technical field
The invention belongs to technical field of cigarette production, more specifically, relate to preparation method and the application of cigarette sugarcane refined cellulose.
Background technology
China is tobacco big country, and annual production and the consumption of cigarette are sure to occupy the first in the world, and the demand of production of cigarettes raw material is very huge.Reconstituted tobacco to carry out after utilizing the cigarette leftover bits and pieces such as offal, crumbled tobacco and discarded tobacco leaf or tobacco waste formula combination recombinating a kind of raw material of cigarette that the manufacture of reproduction process processing obtains.Paper process is one of important method preparing reconstituted tobacco, adds the reconstituted tobacco that suitable fiber prepares high-quality and be called the emphasis that this area is studied in offal, crumbled tobacco and discarded tobacco leaf.
Sugarcane is the important sugar crop of China, this area has relevant research for squeezing the bagasse after sucrose being applied to prepare in reconstituted tobacco, specifically with reference to the processing method of the dead meal such as offal, offal, bagasse slurrying after lixiviate is obtained sugarcane slurry and carry out compound sheet according to oven dry weight than the ratio of 5:95 ~ 30:70 with the slurry such as offal, offal and obtain reconstituted tobacco.
But bagasse belongs to skin, medullary substance mixing, and complex structure, the quality of various compositions on reconstituted tobacco contained in sugarcane fibre has impact in various degree.Do not preparing the report of the research in reconstituted tobacco about refining sugarcane fibre element at present.
Summary of the invention
The technical problem to be solved in the present invention overcomes existing tobacco leaf production technical field utilizes technology deficiency to sugarcane fibre, provides a kind of cigarette preparation method of sugarcane refined cellulose.Adopt the inventive method successfully can prepare the refined cellulose of a-content of cellulose more than 92%.
Another technical problem that will solve of the present invention is to provide described refined cellulose and is preparing the application in reconstituted tobacco, for preferred reconstituted tobacco non-tobacco fiber provides technical support.
Object of the present invention is achieved by following technical solution:
Thering is provided a kind of cigarette preparation method of sugarcane refined cellulose, take bagasse as raw material, carries out prehydrolysis, soda cooking and ODEp tri-stage bleaching after being ground by bagasse, then by alkali refining process, produces and obtains the cellulose of purity more than 90%.
Preferably, the described cigarette preparation method of sugarcane refined cellulose comprises the following steps:
S1. select bagasse raw material, air-dry removal of impurities, is milled to powder;
S2. prehydrolysis: by the powder equilibrium water conten of S1 step gained bagasse, add water and acid solution, be hydrolyzed under air-proof condition reaction, after hydrolysis terminates, bagasse and liquid extruded in the lump and collect waste liquid and obtain prehydrolysis sample, by prehydrolysis sample washes clean;
S3. caustic soda is added in the pre-hydrolyzed solution that S2 step process crosses and carry out boiling;
S4. by the pre-hydrolyzed solution crossed through S3 step process through D 0epD 1tri-stage bleaching process, the process conditions of described D0EpD1 tri-stage bleaching process are:
D 0: ClO 21.0%, starch dense 10%, temperature 60 C, time 60min;
Ep:NaOH 1.5%, H 2o 20.5%, starch dense 10%, temperature 65 DEG C, time 90min;
D 1: ClO 20.4%, starch dense 10%, temperature 70 C, time 90min.
S5. alkali refining process obtains refined cellulose.
Boiling described in S3 adds steam and appropriate caustic lye of soda in the prehydrolysis sample crossed in S2 step process, carries out cooking reaction under air-proof condition, after cooking reaction terminates, by paper pulp and fluid separation applications, and pulp washing is clean.
Preferably, bagasse described in S1 adopts the slag of the sugarcane of new platform sugar ROC16 kind.
Further preferably, described bagasse adopts Guangxi province to produce the slag of the sugarcane of new platform sugar ROC16 kind.
Preferably, powder described in S1 is 40 ~ 60 orders.
Preferably, the condition of hydrolysis described in S2 is: the heating-up time is 60 ~ 70min, and hydrolysising reacting temperature is 155 ~ 160 DEG C, and temperature retention time is 60min, and liquor ratio is 1:6, and the mass percent concentration of acid solution is 0.50 ~ 1.00%.
Further preferably, the condition of hydrolysis described in S2 is: the heating-up time is 60 ~ 70min, and hydrolysising reacting temperature is 155 DEG C, and temperature retention time is 60min, and liquor ratio is 1:6, and the mass percent concentration of acid solution is 0.50%.
Preferably, described acid solution is sulfuric acid solution.
Preferably, the addition of alkali described in S5 is relative to prehydrolysis sample quality 13 ~ 19%, and more preferably, the addition of described alkali is 17 ~ 19%.
The present invention provides the application of described refined cellulose simultaneously, specifically gained refined cellulose is added in offal slurry and offal slurry by different proportion, prepares reconstituted tobacco paper substrate.
The process of described offal slurry and offal slurry is with reference to prior art preparation, the cellulose obtained is refined: offal is starched: the mass ratio that offal is starched is that the ratio of 10 ~ 40%:40 ~ 10%:50 ~ 60% is carried out proportioning and manufactures paper with pulp, and obtains reconstituted tobacco paper substrate according to the inventive method.
Further preferably, refine the cellulose obtained according to the inventive method: offal is starched: the mass ratio that offal is starched is that the ratio of 20%:20%:60% is carried out proportioning and manufactures paper with pulp, and obtains reconstituted tobacco paper substrate.
The present invention also provides a kind of reconstituted tobacco, and dry with above-mentioned reconstituted tobacco paper substrate applied coating solution and get final product, described coating fluid is the concentrate of offal leaching liquor.
The invention has the beneficial effects as follows:
The present invention for raw material, by providing treatment process targetedly, gives full play of its holocellulose, advantage that high, the various extract content of hemi-cellulose content is lower with new platform sugar ROC16, produces refined cellulose provide a kind of preferred raw material for being separated.
The invention provides the integrated artistic of science, adopt " acid prehydrolysis+alkaline boiling+tri-stage bleaching ", preparative separation obtains the refining sugarcane fibre element of a-content of cellulose more than 90%.Gained is refined sugarcane fibre element in the preparation of reconstituted tobacco, is obtained very well well effect, and overall texture and the oral cavity comfort level of applying described cellulosic reconstituted tobacco all have a clear superiority in.
Accompanying drawing explanation
Fig. 1 acid consumption is on the impact of hydrolyzed PH value and yield.
Relation between Fig. 2 prehydrolysis yield and poly-pentose removal efficiency.
Fig. 3 alkali consumption is on the impact of physical property of pulp.
Detailed description of the invention
The present invention is further illustrated below in conjunction with the drawings and specific embodiments.Unless stated otherwise, the reagent that adopts of the present invention and raw material are the conventional commercial reagent in this area and raw material.Unless stated otherwise, the percentage related in the embodiment of the present invention is mass percent.
Embodiment 1 raw material is selected
The present invention carries out raw material selection by the physicochemical characteristics analysis design mothod producing sugarcane fibre raw material with different regions.For exempting to repeat, the present embodiment only produces the bagasse that produces new platform sugar ROC16 kind in the bagasse of cloud sugarcane 03 kind, the bagasse of product Guangdong, Guangdong sugar 00 kind and Guangxi for raw material and is described with Yunnan.
1.1 laboratory apparatus
Plant pulverizer, precision electronic balance, Muffle furnace, water-bath, air dry oven, vacuum pump using circulatory water, fast tester for water content, electric hot plate, DR5000 spectrophotometer, Soxhlet extractor and other conventional analysis glassware.
1.2 raw materials and process
Bagasse Material is provided by sugar refinery, Yunnan, sugar refinery, Guangdong and sugar refinery, Guangxi respectively, raw material mass dryness fraction about 50%; SWBQ0010 special fibre raw material is provided by cigarette in Guangdong.Get representative Bagasse Material at random, air-dry rear use 8 mesh sieve screens out fragment and dust, then quartering is adopted to get about 200 grams of sugarcane fibres, then powder is milled to plant pulverizer, after sieving, collect 40 ~ 60 order powder, be stored in equilibrium water conten in sealed plastic bag, when analyzing bagasse chemical composition for subsequent measurements.
1.3 experimental result
The sugarcane fibre of described kind and the chemical constituent analysis result of SWBQ0010 special fibre are listed in the table below in 1.
As can be seen from Table 1, the content of ashes that sugarcane fibre is produced in Yunnan is 1.24%, and the content of ashes that sugarcane fibre is produced in Guangxi is 0.75%, and in three major production areas sugarcane fibres, the content of ashes that sugarcane fibre is produced in Yunnan is the highest.Because ash content main component is calcium, potassium, sodium, magnesium, manganese and the inorganic matter such as phosphorus, silica, these elements are all needed for plant growth nutrition, potassium content is higher is relative benign to tobacco product, what the increase of preservative water preperation can strengthen tobacco leaf holds firepower, promote Cigarette burning, and then reduction cigarette tar content, improve the security of cigarette.In YC/T 16.3-2003 " reconstituted tobacco the 3rd part: paper process ", also using potassium content as one of its characteristic index, therefore ash content does not form negative effect to the application of sugarcane fibre in reconstituted tobacco.But, the sample that the too high especially metal ion content of content of ashes is high, after burning, ashes is a bit darkish in color; In addition, ash content height can cause fiber separation subtractive process pipeline scale and cause difficulty to devil liquor recovery.Therefore, assign to from ash, it is poor relative to Guangxi, Guangdong product sugarcane fibre that sugarcane fibre is produced in Yunnan.
The chemical constituent of the representative sugarcane fibre raw material in table 1 Yunnan Province
From the content of the large component fibre element of table 1 sugarcane fibre three, hemicellulose and lignin, sugarcane fibre holocellulose is produced in Yunnan, hemicellulose, the always content of lignin are respectively 70.24%, 25.56%, 19.86%, its holocellulose content is minimum among three, hemicellulose level is then the highest among three, and the content of cellulose demonstrating Yunnan product sugarcane fibre is minimum.If utilize this sugarcane fibre separation and purification sugarcane fibre element, then yield is on the low side, and production cost is relatively high.Hemicellulose cracking can produce irritating heat-decomposing compound (such as producing more low-grade aldehydes), and irritating choking can be caused to cough when burning and sucking, the raw material that thus hemicellulose level is low, its quality is better.As can be seen here, from economy point and product quality angle, Yunnan is produced sugarcane fibre and is produced sugarcane fibre not as good as Guangxi, Guangdong.In addition, as can also be seen from Table 1, Yunnan produces that hot water extract's content of sugarcane fibre is 25.62%, 1%NaOH extract is 40.61%, alcohol-benzene extractive content is 1.85%; The content of each extract all produces sugarcane fibre higher than Guangdong, Guangxi.These components, in the process of defibre element, the overwhelming majority all can be degraded stripping.Existence due to them can increase the chemicals consumption of sugarcane fibre subtractive process, the raw material that therefore extract content is low, and quality is better, and also namely the inferior quality of sugarcane fibre is produced in Yunnan.Therefore, chemically composition analysis result, the quality that sugarcane fibre is produced in Yunnan is lower than Guangdong, Guangxi product sugarcane fibre quality.
As can also be seen from Table 1, the content of Sugarcane in Guangdong fiber holocellulose content, hemicellulose, acid-insoluble lignin, total lignin is respectively 77.20%, 23.30%, 20.27% and 21.56%, and wherein content, the always lignin content (comprising acid soluble lignin) of hemicellulose and acid-insoluble lignin are all higher than Guangxi sugarcane fibre.Hemicellulose and the low raw material of lignin content, its quality is better, and comparatively Guangxi sugarcane fibre is poor for the quality of also i.e. Sugarcane in Guangdong fiber.
As can also be seen from Table 1, hot water extract's content of Sugarcane in Guangdong fiber is 16.96%, 1%NaOH extract is 37.02%, alcohol-benzene extractive content is 1.35%; The content of each extract is all higher than Guangxi sugarcane fibre.These components, in the process of defibre element, the overwhelming majority all can be degraded stripping.Existence due to them can increase the chemicals consumption of sugarcane fibre subtractive process, the raw material that therefore extract content is low, and quality is better, and comparatively Guangxi sugarcane fibre is poor for the quality of also i.e. Sugarcane in Guangdong fiber.
In sum, chemically composition analysis result, it is high that the Guangxi quality of producing sugarcane fibre produces sugarcane fibre quality than Guangdong and Yunnan.
Refining of embodiment 2 sugarcane fibre element
S2. prehydrolysis
1. laboratory apparatus
ZT1-00 type 15L electric cooking pot (joining 4 1L canisters), accurate pH meter, electronic balance, water-bath, air dry oven, vacuum pump using circulatory water, fast tester for water content, electric hot plate, DR5000 spectrophotometer, Soxhlet extractor and other conventional analysis glassware.
2. raw material and process
Take the wet feed after over dry 100 grams of equilibrium water contens, add required water or acid solution by table 2 process conditions, then load canister, proceed in digester after sealing, then react under the heating curve and temperature of setting.After reaction terminates, bagasse and liquid are moved in 200 order Nylon Bags in the lump, extrudes and collect waste liquid, then will be hydrolyzed sample washes clean, for analysis.
Table 2 bagasse clear water/weak acid pre-hydrolysis technique condition
Note: the heating-up time is 60 ~ 70min.
3. experimental result
3.1 hydrolysis sample chemical constituent is analyzed
By preceding method process hydrolysis sample, the sample chemical constituent that is hydrolyzed analysis, experimental results is listed in table 3 and table 4.
Table 3 different hydrolysis process gained hydrolysis sample yield, pH value and ash content
Note: absolute magnitude is the actual content of component in hydrolysis sample;
Relative quantity=absolute magnitude × hydrolysis yield;
Relative quantity/component content in the feed of extrusion rate=1-component
As can be seen from table 3 and Fig. 1, sour consumption is higher, and the pH of hydrolytic process is lower, and hydrolysis yield is lower; Hydrolysis temperature is higher, and the pH of the hydrolytic process under the same terms is lower, hydrolysis yield is also lower.But relatively, difference is not clearly.
From the change of ash content, along with the increase of sour consumption, ash content is deviate to take the lead in slightly to increase, and then reduce, acidity is stronger, and ash content extrusion rate is lower; And hydrolysis temperature higher deviate from ratio larger.This illustrates that the impact of temperature on ash content is greater than acid catalyzed impact, and acidity is stronger, is disadvantageous on the contrary to deviating from of ash content.
As can be seen from Table 4, when other experiment conditions are identical, along with the increase of acid concentration, the removal efficiency of hydrolysis sample poly-pentose is significantly improved, and cellulose loss rate increases, and hydrolysis yield reduces.Under the condition of not acid adding (experiment number 1 and experiment number 4), due under high-temperature and high-pressure conditions, water dissociation can go out H +and OH -, destroy hemicellulose oxy-acetyl and furfural acid substituent, generate organic acid, and then promote the degraded stripping of hemicellulose by self-catalyzed reaction.But contrast experiment number 1 and experiment numbers 2, adopt anacidity self-catalysis hydrolysis, experiment poly-pentose extrusion rate is low, be only 21.80%, and after adding the acid of 0.5%, in experiment, poly-pentose extrusion rate reaches 85.25%, is the former 3.9 times; This shows in pre-hydrolysis process, and acid half-and-half cellulosic stripping serves catalytic action.This is because hemicellulose molecule contains free hydroxyl group, be a kind of polar group, there is hydrophily, thus soluble in water.Its degree of polymerization is lower, is generally without crystal structure, arranges loose, is easily hydrolyzed under acid environment.When using dilute sulfuric acid to be hydrolyzed, the H that acid is dissociated in water +meeting and water are combined into H 3o +, the oxygen atom of glycosidic bond in hemicellulose molecule can be made protonated, form conjugate acid, and rupture because bond energy weakens.After fracture, the carbonium ion of end can produce proton again, and proton and water react, and generate new water and hydrogen ion, participate in new hydrolysis.Therefore, acid-hydrolyzed half-and-half cellulosic solute effect is hydrolyzed more than self-catalysis.But the increase of acid concentration, helps little to the extrusion rate of poly-pentose, as acid concentration brings up to 1.0% from 0.5%, the poly-pentose extrusion rate of experiment numbers 3 only improves 0.66% than experiment numbers 2, and the poly-pentose extrusion rate of experiment numbers 6 only improves 0.29% than experiment numbers 2.
The different hydrolysis process of table 4 is on the impact of hydrolysis sample carbohydrate
In addition, as can also be seen from Table 4, when other experiment conditions are identical, along with the raising of temperature, hydrolysis sample poly-pentose removal efficiency slightly improves, but hydrolysis yield then significantly reduces, and holocellulose loss late significantly increases.As when temperature 155 DEG C, sulfuric acid concentration 0.5%, poly-pentose removal efficiency is 85.52%, and prehydrolysis yield, holocellulose loss late are respectively 66.09% and 36.09%.Under similarity condition, temperature increase 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 adds 4.71%, has all exceeded the extrusion rate of poly-pentose.This is due under higher temperature, prehydrolysis reaction aggravation, and carbohydrate is sharply degraded, and under inorganic acid effect, the activation energy of glucoside bond reduces, and causes cellulose dissolution rate to accelerate.
Figure 2 shows the relation of prehydrolysis yield and poly-pentose clearance.From accompanying drawing 2, the yield of prehydrolysis reduces along with the increase of poly-pentose clearance.But according to the difference of the amplitude that it reduces, 2 intervals can be divided into.Poly-pentose removal efficiency is interval A 0 ~ 85%.The relation of this interval yield and poly-pentose removal efficiency can represent with linear equation Y=98.0096-0.373X.In this interval, yield declines comparatively slow, and poly-pentose removes about 85%, and yield only reduces about 25%.Poly-pentose removal efficiency is interval B 85% ~ 90%.In this interval.The relation of yield and poly-pentose removal efficiency can represent with linear equation Y=176.145-1.291X, and its slope is 3.46 times of interval A.This illustrates that, in interval 2, prehydrolysis yield declines very fast, and removing of poly-pentose is very difficult, needs to sacrifice yield for cost.In this interval, poly-pentose removal efficiency is less than 4%, and yield reduces about 5%.As the above analysis, interval A slope is less, is pretreated optimum interval.In sum, choice experiment 2 is as the preferred process condition of bagasse prehydrolysis process.Now, prehydrolysis yield is 66.09%, and poly-pentose removal efficiency is 85.25%.
The different hydrolysis process of table 5 is on the impact of hydrolysis sample trees cellulose content
As can be seen from Table 5, lignin there occurs degraded stripping in various degree at pre-hydrolysis process.For acid-insoluble lignin, acidity is stronger, temperature is higher, and the lignin of stripping is more; For acid soluble lignin, then a large amount of stripping, extrusion rate reaches about 50%, no matter this is because be self-catalysis or acid-catalyzed hydrolysis, the pH of pre-hydrolysis process is acid (being shown in Table 3).
Three, the research experiment of the new platform sugar in Guangxi province ROC16 sugarcane fibre hydrolysis sample defibre element
1. laboratory apparatus
Horizontal rotates boiling vessel KRK 2611 (volume is 4L), oscillatory type flat screen, Mark V1 type PFI fiberizer, Xiao Bai Shi Schooper-Riegler beating degree tester, paper sheet formation system and equipment, L & W062 tensile strength tester, 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, general glassware is commonly used in laboratory.
2. experimental raw and process
Soda cooking and D0EpD1 tri-stage bleaching are carried out to amplification test gained prehydrolysis sample, then gained slurry are pulled an oar, handsheet, then measure the strength character of page.
3. experimental result
3.1 hydrolysis sample soda pulping processes
Carry out slurrying according to table 6 technique, acquired results and characteristics of pulp are in table 6 and table 6.
Table 6 alkali consumption is on the impact of prehydrolysis sugarcane fibre pulpability
* relative yield=paper pulp yield × hydrolysis yield;
Other technique: temperature 160 DEG C, intensification 60min, insulation 60min, liquor ratio 1:4.
As can be seen from Table 6, paper pulp yield reduces along with the increase of alkali charge, and when such as alkali consumption is 13% and 19%, paper pulp yield is respectively 50.63% and 46.44%, reduces 8.28%; But yield is then down to 30.68% from 33.45% relatively, reduces about 2.8%; Meanwhile pulp hardness (Kappa number) is then down to 10.63% from 92.21.Solid content from black liquor pH value and black liquor, alkali charge is crossed, and the pH value of black liquor is higher, and solid content is also higher, and this reflects that alkali consumption is larger, and the material of stripping is more, and this is also the reason that yield declines gradually.From pulp brightness, alkali charge is higher, and whiteness is higher.When alkali charge is lower than 15%, pulp brightness is no more than 30%ISO; When alkali charge reaches 17%, now pulp brightness reaches 35.5%ISO, and continuing increases alkali consumption to 19%, and whiteness brings up to 43.3%ISO further.Beating degree has reacted the wire-dividing broom purification degree of slurry, and as can be seen from Table 6, alkali consumption is larger, and swollen, the wire-dividing broom purification of slurry are more obvious, show as the rising of beating degree.
Table 7 brown stock physical property
For paper grade pulp, tensile index is higher, the intensity of paper pulp is better.But for reconstituted tobacco (YC/T16.3-2003), its tensile strength requires to be no more than 1.0kN/m.Therefore, want the ratio improving paper pulp in reconstituted tobacco, the tensile strength reducing additional paper pulp is one of necessary means.Physical property from table 7, through preliminary treatment, slurrying gained brown stock intensity is lower again, by quantitative 110g/m 2calculate, the tensile strength of brown stock is between 2.75 ~ 3.30kN/m, and this is very beneficial for improving its adding proportion in reconstituted tobacco.
Accompanying drawing 3 describes without under alkali consumption, the variation tendency of physical property of pulp.As can be seen from accompanying drawing 3, alkali consumption improves 15% from 13%, and each intensity index of paper pulp all has a raising; Continue to improve alkali consumption to 17%, each intensity index then significantly declines, and then continue to increase alkali consumption, each index then changes not obvious.
Comprehensive analysis, alkali consumption is proper between 17 ~ 19%.
The bleaching characteristic of 3.2 hydrolysis sample alkaline pulps
Choose 4 #sample carries out D by following technique 0epD 1tri-stage bleaching, gained bleached cellulose pulp characteristic is listed in table 8.
Bleaching process:
D 0: ClO 21.0%, starch dense 10%, temperature 60 C, time 60min;
Ep:NaOH 1.5%, H 2o 20.5%, starch dense 10%, temperature 65 DEG C, time 90min;
D 1: ClO 20.4%, starch dense 10%, temperature 70 C, time 90min.
Table 8 bleached cellulose pulp characteristic
From the characteristic of table 8 bleached cellulose pulp, through bleaching, pulp brightness reaches 85.9%ISO, close with commodity bleached wood pulp whiteness.Every intensity index of paper pulp is slightly improved, and this is mainly owing to removal and the cellulosic brooming of fiber fines.From viscosity, bleaching viscosity declines to some extent.From a-content of cellulose, by preliminary treatment, the cellulose purity of brown stock and bleached pulp all more than 90%, and slightly improves after bleaching.
All in all, adopt " acid prehydrolysis+alkaline boiling+ECF bleaches ", can be separated obtain a-content of cellulose 90 ~ 92% or more refined cellulose.
Embodiment 3 refine sugarcane fibre element join copy experiment and sensory evaluating smoking experiment
1. laboratory apparatus
Horizontal rotates boiling vessel KRK 2611 (volume is 4L), and oscillatory type flat screen, thermostat water bath, BBS type quick kayser method handshcet former, YQ-Z-48B whiteness instrument, electric mixer, electronic balance, general glassware is commonly used in laboratory.
2. experimental raw and process
According to the inventive method, with Guangxi sugarcane fibre for raw material, prehydrolysis-soda cooking and tri-stage bleaching are carried out to it, then by alkali refining process, produce the cellulose of purity more than 92%.Then it is added in offal, offal by different proportion, prepare reconstituted tobacco paper substrate, send Guangdong China Tobacco Industry Co., Ltd technique center to carry out sensory evaluating smoking.
3. experimental result
The process of offal, offal is prepared with reference to other item optimization technique, and the sugarcane fibre of different cellulose purity and other paper pulp fiber are first pulled an oar to 32 ~ 35 ° of SR, and then the proportioning of according to the form below 9 is carried out reconstituted tobacco paper substrate and manufactured paper with pulp.
Table 9 reconstituted tobacco paper substrate sample fiber proportioning 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 Refining 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 substrate
To above-mentioned sample, organize expert to carry out experiment of smokeing panel test, smoking result is as follows:
A: flue gas concentration is higher, the texture of flue gas is general, and wooden breath is heavier, and calcination, the stimulation in oral cavity are comparatively large, and obviously dry, comfort level is poor.
B: flue gas concentration is higher, the texture of flue gas is general, and slightly, it is obvious that lingual surface stings peppery sense to assorted gas, and dry and residual obvious, comfort level is poor.
C: flue gas concentration is higher, the texture of flue gas is poor, and assorted gas is comparatively obvious, and the stimulation in nasal cavity and oral cavity is comparatively obvious, and comfort level is poor.
D: flue gas concentration is moderate, the overall texture E of flue gas is more or less the same, and oral cavity slightly stimulates and dry sensation.
E: flue gas concentration is moderate, the overall texture of flue gas is slightly inferior to F, and the muddiness of flue gas is more obvious than F, and the burning sensation in oral cavity is larger than F.
F: flue gas concentration is moderate, the texture of flue gas is relatively better, Wei You xylon gas, and oral cavity is micro-sweet sense, and comfort level is relatively better, oral stimulation and dry sensation little.
G: flue gas concentration is higher, the texture of flue gas is poor, the stimulation in oral cavity and residual more obvious.
H: flue gas concentration higher (relative G slightly declines), the texture of flue gas is poor, the stimulation in oral cavity and residual more obvious.
GD-125 paper substrate: flue gas concentration is in a slight decrease, the texture of flue gas still can, wooden assorted gas comparatively appears, and lingual surface is micro-bitter taste, peppery sense, and stimulation and the dry sensation in oral cavity are larger.
In general, sugarcane fibre joins in reconstituted tobacco paper substrate (E, F) as plus fiber, join in reconstituted tobacco paper substrate than needlebush (A), leaf wood (C), bamboo pulp (B) as plus fiber, overall texture and the oral cavity comfort level of sugarcane fibre sample all have a clear superiority in; Compare with GD-125 paper substrate, sugarcane fibre reconstituted tobacco sample also has superiority in the lifting and the assorted gas of minimizing of flue gas texture simultaneously.The sample overall quality that interpolation the present invention refines sugarcane fibre element is significantly improved.
Embodiment 4 refine sugarcane fibre element join copy experiment and sensory evaluating smoking experiment
1. laboratory apparatus
Horizontal rotates boiling vessel KRK 2611 (volume is 4L), and oscillatory type flat screen, thermostat water bath, BBS type quick kayser method handshcet former, YQ-Z-48B whiteness instrument, electric mixer, electronic balance, general glassware is commonly used in laboratory.
2. experimental raw and process
According to the inventive method, with Guangxi sugarcane fibre for raw material, prehydrolysis-soda cooking and tri-stage bleaching are carried out to it, then by alkali refining process, produce the cellulose of purity more than 92%.Then it is added in offal, offal by different proportion, prepare reconstituted tobacco paper substrate, send Guangdong Tobacco Company to carry out sensory evaluating smoking.
3. experimental result
The ratio of offal and offal is adjusted to 5:5, and refining sugarcane fibre element is mainly used in alternative tobacco stalk fibre.Coating fluid is the extraction concentrate of gained after offal and offal extract, and spreading rate is about 35%.According to the form below 10 reconstituted tobacco paper substrate sample fiber proportioning, carries out the preparation of reconstituted tobacco paper substrate and dip-coating sample, then carries out sensory evaluating smoking.
Table 10 reconstituted tobacco paper substrate sample fiber proportioning table
To above-mentioned sample, organize expert to carry out endoplasm and smoke panel test, smoking result is as follows:
(1) reconstituted tobacco paper substrate sample
A-w (control sample): flue gas concentration is moderate, the texture of flue gas still can, wooden assorted gas is slightly obvious, and slightly, global comfort still can in the stimulation of oral cavity, lingual surface.
B-w: flue gas concentration comparatively control sample has lifting, the texture of flue gas comparatively control sample has lifting, and wooden assorted gas is less, and oral cavity is micro-sweet sense, and nasal cavity stimulates slightly, and global comfort still can.
C-w: the upper sample of flue gas concentration is micro-lifting, the texture of flue gas is better, and wooden assorted gas is less, and the sweet sense in oral cavity is comparatively obvious, the drying in oral cavity, stimulates slightly, and global comfort still can.
E-w: flue gas concentration is higher, the texture of flue gas still can, sugarcane fibre breath slightly appears, and slightly, oral cavity is micro-sweet sense to assorted gas, the drying in oral cavity, stimulates comparatively obvious, and global comfort is slightly poor.
G-w: flue gas concentration is moderate, the texture of flue gas is slightly poor, and sugarcane fibre breath is comparatively obvious, and assorted gas is comparatively large, and drying, the stimulation in oral cavity are comparatively obvious, and global comfort is slightly poor.
H-w: flue gas concentration is fitted, the texture of flue gas comparatively control sample has lifting, and wooden assorted gas is less, and the sweet sense in oral cavity is comparatively obvious, and the stimulation in oral cavity is less, and drying is comparatively obvious, and global comfort still can.
(2) reconstituted tobacco sample
A-t (control sample): flue gas concentration is moderate, the texture of flue gas still can, perfume quantity is medium, and smoke behavior is better, and wooden assorted gas is less, and dried-up assorted gas is comparatively obvious, the drying in oral cavity, stimulates slightly, and global comfort still can.
B-t: flue gas concentration is moderate, the texture of flue gas comparatively control sample has lifting, and perfume quantity is medium, and smoke behavior is better, and assorted gas is less, and oral cavity has sweet sense a little, and nasal cavity stimulates comparatively obvious, and global comfort is slightly poor.
C-t: flue gas concentration comparatively control sample has lifting, the texture of flue gas is better, and perfume quantity is medium on the upper side, the softer silk floss of flue gas, exquisiteness, and wooden assorted gas is less, and the sweet sense in oral cavity is comparatively obvious, and drying, the stimulation in oral cavity are less, and global comfort is better.
E-t: flue gas concentration is moderate, the texture of flue gas still can, perfume quantity is medium, and smoke behavior is better, and slightly, dried-up assorted gas is micro-to be had wooden assorted gas, the drying of oral cavity and nasal cavity, stimulates comparatively obvious, and global comfort is slightly poor.
G-t: flue gas concentration is medium on the upper side, the texture of flue gas still can, perfume quantity is medium, and smoke behavior is better, and wooden assorted gas is comparatively large, the drying in oral cavity, stimulates comparatively large, and global comfort is poor.
H-t: flue gas concentration is higher, the texture of flue gas is better, and perfume quantity is medium on the upper side, and smoke behavior is better, and wooden assorted gas is comparatively large, and drying, the stimulation in oral cavity are comparatively large, and global comfort is poor.
From above-mentioned smoking result, sugarcane refined cellulose replaces tobacco stalk fibre as plus fiber, and substitute amount with 20% better, sensory evaluating smoking's effect of reconstituted tobacco paper substrate and reconstituted tobacco is better.

Claims (9)

1. a cigarette preparation method for sugarcane refined cellulose, is characterized in that, comprise the following steps:
S1. select bagasse raw material, air-dry removal of impurities, is milled to powder;
S2. prehydrolysis: by the powder equilibrium water conten of S1 step gained bagasse, add water and acid solution, be hydrolyzed under air-proof condition reaction, after hydrolysis terminates, bagasse and liquid extruded in the lump and collect waste liquid and obtain prehydrolysis sample, by prehydrolysis sample washes clean;
S3. caustic soda is added in pre-hydrolyzed solution and carry out boiling;
S4. by the pre-hydrolyzed solution crossed through S3 step process through D 0epD 1tri-stage bleaching process, described D 0epD 1the process conditions of tri-stage bleaching process are:
D 0: ClO 21.0%, starch dense 10%, temperature 60 C, time 60min;
Ep:NaOH 1.5%, H 2o 20.5%, starch dense 10%, temperature 65 DEG C, time 90min;
D 1: ClO 20.4%, starch dense 10%, temperature 70 C, time 90min;
S5. alkali refining process obtains refined cellulose.
2. the cigarette preparation method of sugarcane refined cellulose according to claim 1, is characterized in that, described bagasse adopts the slag of the sugarcane of the new platform sugar ROC16 kind of Guangxi province.
3. the cigarette preparation method of sugarcane refined cellulose according to claim 1, it is characterized in that, the condition of hydrolysis described in S2 is: the heating-up time is 60 ~ 70min, hydrolysising reacting temperature is 155 ~ 160 DEG C, temperature retention time is 60min, liquor ratio is 1:6, and the mass percent concentration of acid solution is 0.50 ~ 1.00%.
4. the cigarette preparation method of sugarcane refined cellulose according to claim 3, it is characterized in that, described hydrolysising reacting temperature is 155 DEG C, and the mass percent concentration of acid solution is 0.50%.
5. the cigarette preparation method of sugarcane refined cellulose according to claim 3 or 4, is characterized in that, described acid solution is sulfuric acid solution.
6. the cigarette preparation method of sugarcane refined cellulose according to claim 1, it is characterized in that, the addition of caustic soda described in S3 step is 13 ~ 19% relative to prehydrolysis sample quality.
7. the cigarette preparation method of sugarcane refined cellulose according to claim 6, it is characterized in that, described in S3 step, the addition of caustic soda is 17 ~ 19%.
8. the application of refined cellulose for preparing of any one of claim 1 to 7 preparation method, it is characterized in that gained refined cellulose to add to during offal slurry and offal starch by different proportion, prepares reconstituted tobacco paper substrate.
9. application according to claim 8, it is characterized in that, the cellulose obtained is refined: offal is starched: the mass ratio that offal is starched is that the ratio of 10 ~ 40%:40 ~ 10%:50 ~ 60% is carried out proportioning and manufactures paper with pulp according to the inventive method, obtain reconstituted tobacco paper substrate, preferably refine the cellulose obtained according to the inventive method: offal is starched: the mass ratio that offal is starched is that the ratio of 20%:20%:60% is carried out proportioning and manufactures paper with pulp, and obtains reconstituted tobacco paper substrate.
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