CN104109978B - A kind of method preparing cotton linter dissolving pulp - Google Patents
A kind of method preparing cotton linter dissolving pulp Download PDFInfo
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Abstract
The present invention relates to a kind of method producing dissolving pulp, prepare the clean preparation method of qualified dissolving pulp particularly to a kind of cotton linter。The method is that the cotton linter raw material after getting the raw materials ready is carried out carbamide pretreatment, drops poly-then through enzyme, then adds liquid at the bottom of steaming and decocting under certain pressure and temperature and hydrogen peroxide steams drift and processes, eventually pass acid treatment and finally give qualified dissolving pulp。Compared with traditional high temperature, high pressure, Qiang Zheng, weight bleaching process, present invention reduces technological process, reduce energy consumption, improve product yield, production cost is made to significantly reduce, and the contaminated wastewater load of generation is little in production process, nontoxic, just can be directly used for crop irrigation or for producing fertilizer through simple process。
Description
Technical field
The present invention relates to pulping technique field, be specifically related to a kind of method preparing cotton linter dissolving pulp。
Background technology
Cotton linter, also known as cotton linters, is by after the effect of cotton gin, fiber that a part in Semen Gossypii surface attachment is short and intensive and fine hair。China abounds with Cotton Gossypii, and cotton linter resource is very abundant, and after all the Semen Gossypii of cotton ginning is shelled floss, obtained short flannel quantity is approximately equivalent to the 15% of gined cotton total output, is a fibre resources that can not be ignored。With regard to its chemical composition, the content of cellulose of cotton linter is up to 90%(mass fraction, lower same), additionally contain the materials such as a small amount of pectin (about 1%), waxiness (about 2%), lignin (2% ~ 3%), ash (about 1%), wherein most just can remove under the conditions of cooking relatively relaxed, but owing to being mixed into cotton seed hull, boll hull (it is mainly composed of lignin) in cotton linter in cotton ginning process, thus resulting in pulp-making of cotton linter difficulty increases。
Dissolving pulp prepared by cotton linter, and mainly one removes lignin therein, waxiness and hemicellulose, and along with the process that the gossypin degree of polymerization reduces。Traditional pulp-making of cotton linter method is the technique of first steaming and decocting after bleaching " heavily steaming light drift ", steaming and decocting generally carries out in rotary spherical digester, by high temperature, high pressure, high alkaline boiling, dissolved lignin, hemicellulose, reduce the cellulosic degree of polymerization, and remove the impurity such as boll hull, cotton seed hull。Traditional preparation flow is as follows:
(1) get the raw materials ready: cotton linter opener dry slag disposal device blower fan cyclone separator；
(2) slurrying: pressafiner rotary spherical digester spraying pot HC Cleaner jordan refiner vaccum pulp absorbing unit intermediate pool desander wash engine reserve pit blender static mixer chlorination tower wash engine double roller mixer alkalization tower double roller mixer bleaching tower wash engine dechlorinator；
(3) post processing: wash engine reserve pit reserve pit gravity disc thickener pulp machine。
THE TECHNICS IN PULPMAKING OF COTTON LINTER adopts the method to produce dissolving pulp, there is following problem: 1) mixing of cooking liquor and cotton linter, permeate uneven, cooking effect is poor。2) in order to reduce the degree of polymerization and improve reactivity worth, fiber primary cell wall being sufficiently destroyed, adopt process conditions fiercer, basic hydrolysis and peeling reaction are strong, cause that cotton linter consumption is higher, and yield is relatively low。3) dissolved with the Organic substances such as lignin, hemicellulose, waxiness, its COD higher (30000-40000mg/l) in waste liquid, liquid waste processing is difficult, relatively costly。4) adopt chlorine or chloride bleaching, containing chlorine in waste water, add the difficulty of liquid waste processing。5) complex manufacturing, equipment is more, and production cost puts into bigger。
In order to reduce pollution, alkali-hydrogen peroxide process starts expanded application。Document (Tang Jifu, Li Fengzhu. pulp-making of cotton linter new technology [J]. paper and papermaking 2005 (1): 42-43) in describe this method in detail。This method hydrogen peroxide replaces the chlorine such as chlorine, chlorine dioxide system bleach, it is possible to reduce the pollutant in waste liquid, and becomes pulp yield and whiteness higher。But this method there is also hydrogen peroxide can only bleached fiber top layer, not easily infiltration, can not effectively remove oils and fats and waxiness, the easy decomposition of hydrogen peroxide, steam the problems such as drift effect haves much room for improvement。
Summary of the invention
For prior art Problems existing, the present invention proposes a kind of preparation method polluting cotton linter dissolving pulp little, that waste liquid is easy to be recycled, product yield is high, steaming drift is effective, production cost is low。
For reaching above-mentioned purpose, the present invention adopts the following technical scheme that with the cotton linter after getting the raw materials ready for raw material, successively add carbamide and it is processed by enzyme, it is then added into filling in the pressure vessel of liquid at the bottom of steaming and decocting, and add hydrogen peroxide carry out steam drift, finally gained slurry is carried out acid treatment, after being then passed through post-processing step, obtain qualified dissolving pulp。
It concretely comprises the following steps:
1) to liquor ratio, (weight ratio of over dry cotton linter and liquid, fluid density presses 1g/cm in carbamide pretreatment3) 1:7 ~ 15 get the raw materials ready cotton linter and water system in add carbamide, under 90 DEG C ~ 170 DEG C conditions, prehydrolysis process 30 ~ 180min；
2) ferment treatment sulphuric acid regulates above-mentioned system pH to 7 ~ 8, enzyme is added in system, described enzyme is feruloyl esterase or cellulase or lipase, the amount adding enzyme is 20 ~ 200U/g oven dry stock, under 40 DEG C ~ 80 DEG C conditions, process 2 ~ 48h, be then discharged out treatment fluid, obtaining slurry I, its water content is at 70wt% ~ 80wt%；
3) steam drift process and be sequentially added into liquid at the bottom of slurry I and steaming and decocting in steaming drift container, its mass ratio is 1:0.4 ~ 0.6, being warming up to 85 DEG C ~ 100 DEG C, add 27.5wt% hydrogen peroxide, the mass percent of the relative over dry cotton linter of its addition is 5% ~ 20%, and add water regulation system liquor ratio, make its liquor ratio in the scope of 1:8 ~ 9, be continuously heating to 120 DEG C ~ 170 DEG C, steam drift and process 1 ~ 3h, pressure release, whole process carries out under agitation；
4) acid treatment is when temperature is 50 DEG C ~ 90 DEG C, adds acid, regulation system pH to 3 ~ 5, processes 0.5 ~ 3h。
Getting the raw materials ready as step is prior art, it is therefore an objective to the foreign material such as the sand and dust removed in cotton linter how, boll hull, Semen Gossypii of trying one's best。After getting the raw materials ready, first it is in the cotton linter system got the raw materials ready, add carbamide carry out prehydrolysis。The basic character of carbamide plays infiltration and profit rises effect, it is possible to remove the wax fat on cotton linter surface；Select carbamide reason also reside in, on the one hand, carbamide action temperature and, the cutting action of fiber is little, decrease the loss of cotton linter raw material, be conducive to improve yield；On the other hand, carbamide is as a kind of conventional fertilizer, and environment is not only constituted pollution by the waste liquid containing carbamide, produces waste liquid and is also used as Fertilizer application after treatment。Cotton linter after Urea treatment can the contact area of increased fiber and enzyme and other chemical reagent, raising accessibility, thus accelerating response speed, reduce the consumption of following enzyme。The mass percent of the relative over dry cotton linter of optimum amount of carbamide is 6% ~ 12%, at 90 ~ 170 DEG C, and pretreatment 30 ~ 180min。
Enzyme is added again in system。Ferment treatment not only pollutes little but also has very strong selectivity and specific aim, the present invention relates to three kinds of common enzymes in slurrying field: the ester bond in feruloyl esterase energy Polysaccharides ferulic acid ester, ferulic acid is dissociated out, it can cut off the crosslinking between polysaccharide-polysaccharide in cell wall, polysaccharide-lignin, is conducive to the release of cellulosic degraded and lignin in cell wall substance；Lipase and cellulase can the glycosidic bond of cut staple element, effectively reduce the cellulosic degree of polymerization。In order to provide a suitable environment to enzyme, with sulphuric acid regulation system pH to 7 ~ 8, controlling temperature between 40 ~ 80 DEG C, then select 1 ~ 3 kind in these three enzyme, the amount ranges of enzyme is 20 ~ 200U/g oven dry stock, drops poly-process 2 ~ 48h。After dropping poly-process by enzyme, the degree of polymerization of cotton linter can be substantially reduced, it is ensured that next step steams the effect of drift。After ferment treatment, discharge treatment fluid, make slurry water content 70% ~ 80%。
Being sequentially added into liquid at the bottom of slurry I and steaming and decocting to steaming in drift container, its mass ratio is 1:0.4 ~ 0.6。The component of liquid at the bottom of steaming and decocting is: cellulose penetrating agent: 0.5% ~ 1%, potassium hydroxide 10% ~ 25%, surfactant 0.1% ~ 1%, magnesium sulfate 0.2% ~ 0.5%, EDTA0.5% ~ 3%, and described surfactant is the built agent of dodecylbenzene sodium sulfonate, Polyethylene Glycol。
In the component of liquid at the bottom of heretofore described steaming and decocting, cellulose penetrating agent can make other chemical reagent contact with cotton linter fiber better, improves its functioning efficiency。Potassium hydroxide replaces traditional sodium hydroxide, containing potassium ion in such waste liquid, is conducive to waste liquid as the application of fertilizer。The effect of surfactant mainly has acceleration steaming and decocting infiltration, improves bleaching effect etc.。Adding and the effect of EDTA chelate heavy metals of magnesium sulfate, decrease and add the decomposition of hydrogen peroxide after hydrogen peroxide, thus improving hydrogen peroxide bleaching effect。
Above-mentioned mixed system is heated, when temperature rises to 85 DEG C ~ 100 DEG C, adds hydrogen peroxide, the addition of hydrogen peroxide can most of Organic substance in oxidation Decomposition waste liquid, strengthen cooking effect, increase pulp brightness。Find that adding hydrogen peroxide at such a temperature can obtain optimum efficiency, because it so can be made quickly to discharge hydroxyl radical free radical, reduces decomposition in practice。The mass percent of the relative over dry cotton linter of addition is 5% ~ 20%, and adds water adjustment liquor ratio in right amount so that it is in the scope of 1:8 ~ 9, it is ensured that it can normally stir, and has the steaming drift effect of the best。Being continuously heating to 120 DEG C ~ 170 DEG C, steam drift and process 1 ~ 3h, pressure release discharge, whole process carries out under agitation。
Finally, add acid to process, purpose is to improve the whiteness of pulp, reduce ash, improve the reactivity worth of pulp, pulp is finally made to reach the quality standard (FZ/T51001-2009) of short rayon fiber Wesy Cotton Pulp Grade A, what add in hydrochloric acid, sulphuric acid, acetic acid is any, regulation system pH to 3 ~ 5, processes 0.5 ~ 3h。
The technique using the present invention prepares dissolving pulp, and product yield and whiteness all increase than traditional handicraft。The waste liquid produced can discharge after simply slagging-off, sedimentation, tune pH, moreover it can be used to field irrigation and organic fertilizer, in waste liquid, COD is reduced to≤14000mg/L from the 40000mg/L of prior art。
The invention have the benefit that the technological process shortening tradition alkali liquor steaming and decocting, reduce energy consumption, product yield and quality are all significantly improved, and make production cost significantly reduce。It addition, the pollutant load in production waste liquid reduces, namely waste liquid can be used for field irrigation through simple process or does organic fertilizer。
Detailed description of the invention
Embodiment 1
Cotton linter used in embodiment is the three class one-level flosss being commercially available。
Idiographic flow is as follows:
Get the raw materials ready: cotton linter opener dry slag disposal device blower fan cyclone separator；
Slurrying: carbamide pretreatment ferment treatment steams drift and processes acid treatment；
Post processing: slagging-off wash engine reserve pit reserve pit gravity disc thickener pulp machine。
In embodiment get the raw materials ready and last handling process be traditional handicraft, be not repeated in following example introduce。
Pulping process is as follows:
The first step: carbamide pretreatment
In rustless steel stirred tank vessel, add 1Kg(oven-dry weight) cotton linter of getting the raw materials ready, regulating liquor ratio (ratio of dry solids and total liquid, lower with) is 1:7, adds carbamide 80g, is warming up to 90 DEG C, is incubated 180min；
Second step: ferment treatment
Use 9mol L-1Sulfuric acid solution, adjust system pH to 7, temperature is reduced to 40 DEG C, and adding feruloyl esterase and cellulase mass ratio is 1:1, and consumption is 200U/g oven dry stock, and isothermal holding 48h is then discharged out treatment fluid, makes slurry water content at 70wt%；
3rd step: steam drift and process
Steam drift process to carry out in the stainless steel pressure reactor with stirring, outside reactor, have chuck can pass into steam heating。1:0.4 adds liquid at the bottom of pretreatment slurry and steaming and decocting in reactor in mass ratio, then at the logical steam of interlayer, when making slurry be warming up to 85 DEG C, adding hydrogen peroxide 50g, adds 50 DEG C of warm water, adjustment liquor ratio is to 1:8 then closed reactor, continue heating, make temperature rise to 120 DEG C, be incubated 3h blowing；
Steaming liquid at the bottom of the steaming and decocting that relates in drift processing procedure is fiber pervasion agent, potassium hydroxide, surfactant, magnesium sulfate, EDTA mixed liquor, consumption is as follows: penetrating agent: 5g, potassium hydroxide 100g, surfactant 1g, magnesium sulfate 2g, EDTA5g；
In whole steaming drift process, one heads straight for stirring, speed of agitator 200r/min；
4th step: acid treatment
In feed liquid, add sulphuric acid, at adjusting pH to 3,50 DEG C, be incubated 3h；
Carry out post processing after acid treatment, be prior art and repeat no more。
The final cotton linter dissolving pulp obtained, yield is up to 86.5%, and has carried out product quality detecting (product quality data see attached list one), all reaches short rayon fiber Wesy Cotton Pulp Grade A quality standard (FZ/T51001-2009)。Yield and Related product mass parameter all measure according to national standard。
Embodiment 2
Cotton linter used in embodiment is the three class floss one-level flosss being commercially available。
Cotton linter used is through getting the raw materials ready。
Pulping process is as follows:
The first step: carbamide pretreatment
In rustless steel stirred tank vessel add 1Kg(oven-dry weight) cotton linter of getting the raw materials ready, adjustments liquor ratio is 1:10, add carbamide 150g, be warming up to 170 DEG C, insulation 180min；
Second step: ferment treatment
Use 9mol L-1Sulfuric acid solution, adjust system pH to 8, temperature is reduced to 80 DEG C, add feruloyl esterase, consumption is 100U/g oven dry stock, and isothermal holding 48h is then discharged out treatment fluid, makes slurry water content at 75wt%；
3rd step: steam drift and process
Steam drift process to carry out in the stainless steel pressure reactor with stirring, outside reactor, have chuck can pass into steam heating。In mass ratio 1:0.5 process to addition in reactor after liquid at the bottom of feed liquid and steaming and decocting, then at the logical steam of interlayer, when making slurry be warming up to 85 DEG C, adding hydrogen peroxide 20%, adds 100 DEG C of hot water, adjustment liquor ratio is to 1:10 then closed reactor, continue heating, make temperature rise to 120 DEG C, be incubated 3h blowing；
Steaming liquid at the bottom of the steaming and decocting that relates in drift processing procedure is penetrating agent, potassium hydroxide, surfactant, magnesium sulfate, EDTA mixed liquor, addition is as follows: penetrating agent: 10g, potassium hydroxide 250g, surfactant 10g, magnesium sulfate 5g, EDTA30g；
In whole steaming drift process, one heads straight for stirring, speed of agitator 200r/min；
4th step: acid treatment
Acid used is hydrochloric acid, and the temperature of acid treatment is 95 DEG C, adjusts pH to 5, and the acid treatment time is 0.5h。
Carry out post processing after acid treatment, be prior art and repeat no more。
The final cotton linter dissolving pulp obtained, yield is up to 85.1%, and has carried out product quality detecting (product quality data see attached list one), all reaches short rayon fiber Wesy Cotton Pulp Grade A quality standard (FZ/T51001-2009)。Yield and Related product mass parameter all measure according to national standard。
Embodiment 3
Cotton linter used in embodiment is the three class floss one-levels being commercially available。
Cotton linter used is through getting the raw materials ready。
Pulping process is as follows:
The first step: carbamide pretreatment
In rustless steel stirred tank vessel add 1Kg(oven-dry weight) cotton linter of getting the raw materials ready, regulate liquor ratio 1:15, add carbamide 100g, be warming up to 130 DEG C, be incubated 120min；
Second step: ferment treatment
Use 9mol L-1Sulfuric acid solution, adjust system pH to 7.5, temperature is reduced to 60 DEG C, adds feruloyl esterase, cellulase, lipase mass ratio are 1:1:1, and consumption is 20U/g oven dry stock, and isothermal holding 12h is then discharged out treatment fluid, makes slurry water content 70% ~ 80%。PH value is to regulate with tap water and potassium hydroxide solution；
3rd step: steam drift and process
Steam drift process to carry out in the stainless steel pressure reactor with stirring, outside reactor, have chuck can pass into steam heating。In mass ratio 1:0.6 process to addition in reactor after liquid at the bottom of feed liquid and steaming and decocting, then at the logical steam of interlayer, when making slurry be warming up to 95 DEG C, adding hydrogen peroxide 150g, adds 80 DEG C of warm water, adjustment liquor ratio is to 1:9 then closed reactor, continue heating, make temperature rise to 150 DEG C, be incubated 2h blowing；
Steaming liquid at the bottom of the steaming and decocting that relates in drift processing procedure is penetrating agent, potassium hydroxide, surfactant, magnesium sulfate, EDTA mixed liquor, addition is as follows: penetrating agent: 8g, potassium hydroxide 200g, surfactant 5g, magnesium sulfate 3g, EDTA20g；
In whole steaming drift process, one heads straight for stirring, speed of agitator 200r/min；
4th step: acid treatment
Acid used is acetic acid, and the temperature of acid treatment is 70 DEG C, pH to 4, and the acid treatment time is 2.5h；
Carry out post processing after acid treatment, be prior art and repeat no more。
The final cotton linter dissolving pulp obtained, yield is up to 86.9%, and has carried out product quality detecting (product quality data see attached list one), all reaches short rayon fiber Wesy Cotton Pulp Grade A quality standard (FZ/T51001-2009)。Yield and Related product mass parameter all measure according to national standard。
Embodiment 4
Cotton linter used in embodiment is the three class floss one-levels being commercially available。
Cotton linter used is through getting the raw materials ready。
Pulping process is as follows:
The first step: carbamide pretreatment
In rustless steel stirred tank vessel add 1Kg(oven-dry weight) cotton linter of getting the raw materials ready, regulate liquor ratio 1:10, add carbamide 120g, be warming up to 140 DEG C, be incubated 120min；
Second step: ferment treatment
Use 9mol L-1Sulfuric acid solution, adjust system pH to 7.5, temperature is reduced to 60 DEG C, and adding cellulase, lipase mass ratio is 1:1, and consumption is 150U/g oven dry stock, and isothermal holding 12h is then discharged out treatment fluid, makes slurry water content 70% ~ 80%；
3rd step: steam drift and process
Steam drift process to carry out in the stainless steel pressure reactor with stirring, outside reactor, have chuck can pass into steam heating。In mass ratio 1:0.5 process to addition in reactor after liquid at the bottom of feed liquid and steaming and decocting, then at the logical steam of interlayer, when making slurry be warming up to 100 DEG C, adding hydrogen peroxide 150g, adds 80 DEG C of warm water, adjustment liquor ratio is to 1:9 then closed reactor, continue heating, make temperature rise to 150 DEG C, be incubated 2h blowing；
Steaming liquid at the bottom of the steaming and decocting that relates in drift processing procedure is penetrating agent, potassium hydroxide, surfactant, magnesium sulfate, EDTA mixed liquor, addition is as follows: penetrating agent: 8g, potassium hydroxide 200g, surfactant 5g, magnesium sulfate 3g, EDTA20g；
In whole steaming drift process, one heads straight for stirring, speed of agitator 200r/min；
4th step: acid treatment
Acid used is acetic acid, and the temperature of acid treatment is 70 DEG C, pH to 4, and the acid treatment time is 2.5h。
Carry out post processing after acid treatment, be prior art and repeat no more。
The final cotton linter dissolving pulp obtained, yield is up to 85.9%, and has carried out product quality detecting (product quality data see attached list one), all reaches short rayon fiber Wesy Cotton Pulp Grade A quality standard (FZ/T51001-2009)。Yield and Related product mass parameter all measure according to national standard。
The product index of subordinate list one embodiment
Subordinate list two short rayon fiber Wesy's Cotton Pulp Grade A quality standard (FZ/T51001-2009)
Claims (3)
1. the method preparing cotton linter dissolving pulp, it is characterized in that: with the cotton linter after getting the raw materials ready for raw material, successively add carbamide and it is processed by enzyme, it is then added into filling in the pressure vessel of liquid at the bottom of steaming and decocting, add hydrogen peroxide to carry out steaming drift process, finally gained slurry is carried out acid treatment, after being then passed through post-processing step, obtain qualified dissolving pulp；
It concretely comprises the following steps:
1) carbamide pretreatment adds carbamide in the mixed system of get the raw materials ready cotton linter and the water of liquor ratio 1:7～15, and under 90 DEG C～170 DEG C conditions, prehydrolysis processes 30～180min；
2) ferment treatment sulphuric acid regulates above-mentioned system pH to 7～8, enzyme is added in system, described enzyme is feruloyl esterase or cellulase or lipase, the amount adding enzyme is 20～200U/g oven dry stock, under 40 DEG C～80 DEG C conditions, process 2～48h, be then discharged out treatment fluid, obtaining slurry I, its water content is at 70wt%～80wt%；
3) steam drift process and be sequentially added into liquid at the bottom of slurry I and steaming and decocting in steaming drift container, its mass ratio is 1:0.4～0.6, being warming up to 85 DEG C～100 DEG C, add 27.5wt% hydrogen peroxide, the mass percent of the relative over dry cotton linter of its addition is 5%～20%, and add water regulation system liquor ratio, make its liquor ratio in the scope of 1:8～9, be continuously heating to 120 DEG C～170 DEG C, steam drift and process 1～3h, pressure release, whole process carries out under agitation；
4) acid treatment is when temperature is 50 DEG C～90 DEG C, adds acid, regulation system pH to 3～5, processes 0.5～3h, and reaction completes, and enters post-processing step；
Wherein step 1) in add carbamide measure relative over dry cotton linter mass percent be 8%～15%；
Step 3) in the component of liquid at the bottom of steaming and decocting include cellulose penetrating agent, potassium hydroxide, surfactant, magnesium sulfate, EDTA；Its addition is as follows relative to the mass percent of over dry cotton linter: cellulose penetrating agent 0.5%～1%, potassium hydroxide 10%～25%, surfactant 0.1%～1%, magnesium sulfate 0.2%～0.5%, EDTA0.5%～3%。
2. a kind of method preparing cotton linter dissolving pulp according to claim 1, it is characterised in that: step 4) in the acid that adds be any one in hydrochloric acid, acetic acid, sulphuric acid。
3. a kind of method preparing cotton linter dissolving pulp according to claim 1, it is characterised in that: described surfactant is the built agent of dodecylbenzene sodium sulfonate, Polyethylene Glycol, and its compound proportion is 1:1～10。
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| CN105484084B (en) * | 2015-11-24 | 2018-05-01 | 黄河三角洲京博化工研究院有限公司 | A kind of method that cotton linter prepares dissolving pulp |
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