CN102182086B - Method for preparing bamboo pulp by full-liquid-phase prehydrolysis sulfate displacement cooking process - Google Patents
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Abstract
The invention discloses a method for preparing bamboo pulp by a full-liquid-phase prehydrolysis sulfate displacement cooking process, which comprises the following steps: preparing materials, washing the materials, prehydrolysizing, cooking, washing, screening, bleaching, regulating polymerization degree, dechlorinating and conducting acid treatment. According to the preparation method, after the cooking is finished, for the obtained pulp, the content of alpha cellulose is more than or equal to 95%, the pepentosan is more than or equal to 4%, and the average polymerization degree is 550-650; after the acid treatment is finished, for the obtained pulp, the content of alpha cellulose is more than or equal to 94%, the pentosan is less than or equal to 3.0%, the average polymerization degree is 400-500, and the white degree is 86-89%. The method has the following advantages: the whole set of technology of full-liquid-phase prehydrolysis, full-liquid-phase cooking, hydrolyzate recovering and recovered black liquid displacement cooking, not only is the waste water pollution degree is alleviated, the temperature rising time and steam amount are saved, the trebling effects of energy saving, emission reduction and yield increasing are achieved, and the problems that the waste water pollution is serious, the energy consumption is high and the output is low in the pulp prepared by the current prehydrolisis sulfate method.
Description
Technical field
The invention belongs to chemical fiber field, be specifically related to the method that a kind of full liquid phase prehydrolysis sulfate displacement cooking prepares bamboo pulp.
Background technology
In recent years, along with becoming increasingly conspicuous of global energy problem in short supply, the non-renewable resources prices such as coal, oil rose steadily, and caused that the price of petrochemical industry class synthetic fiber is soaring, and therefore, seeking renewable fibrid becomes following new trend.Although cotton class natural fabric has good spinnability and reproducibility, limited because of its production capacity, price still rises steadily, and does not satisfy the huge fiber market demand far away.Therefore, another kind of renewable fiber--viscose is a dark horse, and becomes the main flow of regenerated fiber class.
In the viscose class, pass through the viscose that the dissolving spinning technology produces take wood pulps and bamboo pulp as raw material and consisted of market nominative office.Wherein, the bamboo fibre take bamboo pulp as raw material production has good anti-microbial property, anti-ultraviolet function and drapability, and made bamboo fiber towel, bamboo fibre bath towel, bamboo fibre daily necessities more and more are subject to people's favor and pursue.So, constantly appreciating in cotton, petrochemical industry class synthetic fiber production capacity constantly limits, the special performance of bamboo fibre is constantly found by people and like under this background, has formed the new situation of this bamboo pulp market contention in several years.
The bamboo pulp raw materials for production are bamboo wood, on China Sichuan, Guangxi, Guizhou and other places very abundant bamboo resource are arranged.Bamboo wood is from planting to the 2-3 of becoming a useful person, and output is at 2 tons about every mu.Wherein, cizu is most popular, and it is the good raw material of papermaking, also is the good raw material of bamboo pulp.
Pulp has another name called dissolving pulp, and production method the earliest is to adopt sulphite process, and because of its system complex, huge existing domestic the employing seldom of investment, this method is generally for the production of the senior dissolving pulp of special type.Afterwards, develop prehydrolysis sulphate cook technique, comprised acid hydrolysis sulphate cook technique, decatize hydrolysis sulphate cook technique and the prehydrolysis sulphate cook technique take water as medium.Acid hydrolysis sulphate cook technique is owing to use a large amount of acid solutions, and the acid solution recovery system is complicated, and is large to equipment corrosion, and the water consumption is high, operating cost is also higher, and this method is seldom used.Decatize hydrolysis sulphate cook technique uses steam to be hydrolyzed, and hydrolysis efficiency is higher, but since steam enter steamer after temperature can't evenly control, it is relatively poor to cause being hydrolyzed uniformity, product quality is stable not, this method is not all adopted in general large production.Prehydrolysis sulphate cook technique take water as medium is the more method that adopts both at home and abroad at present, and this method investment is little, and operating cost is low, and product quality is comparatively stable, is applicable to produce medium-to-high grade viscose pulp.But the prehydrolytic sulfate process that adopts both at home and abroad at present uses semi-liquid phase hydrolysis and boiling, thereby the uniformity of hydrolysis and boiling is still not bery desirable, and hydrolyzate directly effluxes processing, a large amount of heat energy and water resource have been wasted, heating-up time is longer, so have still that energy consumption is higher, hydrolytically unstable, discharge liquid pollute the outstanding problem large, that production capacity is low, so the production capacity of bamboo pulp is restricted to a certain extent.
Summary of the invention
The purpose of this invention is to provide the method that a kind of full liquid phase prehydrolysis sulfate displacement cooking prepares bamboo pulp.
The present invention is achieved in that the method that adopts a kind of full liquid phase prehydrolysis sulfate displacement cooking to prepare bamboo pulp, comprise get the raw materials ready, wash material, prehydrolysis, boiling, wash material, screen, bleach, telomerize right, dechlorination, acid treatment, it is characterized in that:
(1), get the raw materials ready: bamboo wood is cut into long 20-50mm, the rectangle bamboo chip of wide 10-20 mm, for subsequent use;
(2), wash material: the bamboo chip that cuts is washed first, remove after the washing surface impurity, for subsequent use;
(3), prehydrolysis: bamboo chip carries out first the prehydrolysis step before carrying out sulphate cook after the washing; Described prehydrolysis is carried out in digester, mix as hydrolysis medium in the 9:1-4:1 ratio with clear water and reuse hydrolyzate, the hydrolyzate complete bamboo chip in the submergence digester just in digester during hydrolysis, be full liquid-phase hydrolysis, hydrolysis pressure is 0.6-0.75MPa, dwell time is 120-300 minute, and the hydrolyzate of generation carries out the part reuse; " hydrolyzate of reuse " is a kind of acidic liquid that contains a large amount of organic acids and a small amount of hemicellulose, according to 200-220kg/m
3Dress pot density fill pot and can improve single pot of production capacity, reduce solid-to-liquid ratio, the concentration of acid when increasing hydrolysis, thereby improve hydrolysis speed, save hydrolysis time.
(4), boiling: described boiling is carried out in digester, adopts the full liquid phase displacement cooking of sulfate technology, the black liquor part reuse that boiling produces, technological parameter is: the alkali mass fraction accounts for over dry bamboo chip weight 18-30%(with Na
2The O meter), sulphidity is 15-25%(Na
2The O meter), protected 120-300 minute at 0.6-0.75MPa, the gained slurry is removed impurity after washing and screening;
(5), bleaching: in oxygen floats tower, chlorine dioxide upwelling and down-welling tower, caustic tower, carry out employing O-D0-EOP-D1 bleaching process, bleaching time 60-240 minute, bleaching temperature 60-100 ℃;
(6), telomerize right: in the hypochlorite treating column, carry out, add the clorox of 0.1-0.3%, processed 40-70 minute at 35-40 ℃;
(7), dechlorination: slurry does not wash after right through telomerizing, and directly carries out dechlorination between acid treatment and hypochlorite are processed, and used antichlor is sodium thiosulfate, consumption be residual chlorine dose in the slurry 1.2-1.4 doubly;
(8), acid treatment: in acid accumulator treatment tower, carry out, and add a small amount of chelating agent 25-45 ℃ of processing 40-60 minute.
Prepare the method for bamboo pulp according to full liquid phase prehydrolysis sulfate displacement cooking of the present invention, it is characterized in that the cooking liquor in the described boiling step is NaOH and Na
2S presses the mass ratio of 1:3-1:5.6 (with Na
2The O meter) mixed liquor.
According to above-mentioned preparation method, after described steaming stage finishes, the content of alphacellulose of gained slurry 〉=95%, pentosan≤4%, average degree of polymerization are 550-650; After described acid treatment finishes, the content of alphacellulose of gained slurry 〉=94%, pentosan≤3.0%, average degree of polymerization are 400-500, whiteness 86-89%.
The utility model has the advantage of: the method adopts full liquid-phase hydrolysis, full liquid phase cooking, hydrolyzate reuse and reuse black liquor displacement cooking technological package, both greatly alleviated contaminated wastewater, heating-up time and steam have been saved again, reached triple effects energy-conservation, that reduce discharging, increase production, efficiently solved current prehydrolytic sulfate process and produce the problem that pulp waste water pollutes greatly, energy consumption is high, production capacity is low.
The specific embodiment
Now to the detailed description of the invention:
Embodiment 1
Get the raw materials ready: bamboo wood is cut into the long rectangle bamboo chip of 20-50mm through bamboo cutter, requires qualification rate to reach more than 80%.
Washing: bamboo chip enters digester through flush away surface impurity behind the rinsing machine and after removing excessive moisture.
Prehydrolysis: after bamboo chip installs pot by the dress pot density of 200kg/m3 after the washing, heat up after being full of hydrolyzate in the digester, be raised to 160 ℃ in 30 minutes to protect 180 minutes, after hydrolysis is finished with hydrolyzate suction hydrolyzate storagetank as next pot hydrolysis medium.
Boiling: adopt the full liquid phase displacement cooking of sulfate.To over dry bamboo chip weight 22%, sulphidity is with Na to alkali charge in Na2O
2The O meter was raised to 145 ℃ in 25%, 90 minute, protected 30 minutes, was raised to 160 ℃ in 60 minutes again and protected 120 minutes, and blowing after the terminal point displacement is finished gets slurry yield rate 40%, content of alphacellulose 95.1%, pentosan 4%, Kappa number 14, iron part 40ppm.
Bleaching: adopt O-D0-EOP-D1 technique, oxygen floats 95 ℃ of temperature, pressure 0.5MPa, 60 minutes time; D0 section ClO2 is to oven dry stock consumption 1%, temperature 60 C, 120 minutes time; EOP section alkali is to oven dry stock consumption 2.5%, and hydrogen peroxide is to oven dry stock consumption 0.07%, and oxygen is pressed 0.1MPa, temperature 70 C, 120 minutes time; D1 section ClO2 is to oven dry stock consumption 0.5%, temperature 60 C, 120 minutes time.
Telomerize right: add the clorox of 0.1-0.3%, processed 40 minutes for 35 ℃.
Dechlorination: the sodium thiosulfate consumption is 1.2-1.4 times of residual chlorine dose in the slurry.
Acid treatment: added at normal temperatures the salt acid treatment 40 minutes.
Manufacture paper with pulp: the slurry after the acid treatment send the oven dry of manufacturing paper with pulp of pulpboard workshop after washing, cuts at last metering and packs.By present embodiment gained bamboo pulp for cellulose viscose, content of alphacellulose 93%, pentosan 3%, whiteness 88, iron part 10ppm, ash content 0.11%.
Embodiment 2
Get the raw materials ready: bamboo wood is cut into the long rectangle bamboo chip of 20-50mm through bamboo cutter, requires qualification rate to reach more than 80%.
Washing: bamboo chip enters digester through flush away surface impurity behind the rinsing machine and after removing excessive moisture.
Prehydrolysis: after bamboo chip installs pot by the dress pot density of 200kg/m3 after the washing, heat up after being full of hydrolyzate in the digester, be raised to 165 ℃ in 50 minutes to protect 180 minutes, after hydrolysis is finished with hydrolyzate suction hydrolyzate storagetank as next pot hydrolysis medium.
Boiling: adopt the full liquid phase displacement cooking of sulfate.Alkali charge in Na2O to over dry bamboo chip weight 22%, sulphidity is in Na2O 25%, be raised to 145 ℃ in 90 minutes, protected 30 minutes, be raised to again 160 ℃ in 60 minutes and protected 140 minutes, blowing after the terminal point displacement is finished, get slurry yield rate 39%, content of alphacellulose 96%, pentosan 3.6%, Kappa number 10, iron part 30ppm.
Bleaching: adopt O-D0-EOP-D1 technique, oxygen floats 98 ℃ of temperature, pressure 0.5MPa, 60 minutes time; D0 section ClO2 is to oven dry stock consumption 1%, 65 ℃ of temperature, 120 minutes time; EOP section alkali is to oven dry stock consumption 2.0%, and hydrogen peroxide is to oven dry stock consumption 0.07%, and oxygen is pressed 0.1MPa, temperature 70 C, 120 minutes time; D1 section ClO2 is to oven dry stock consumption 0.5%, temperature 60 C, 120 minutes time.
Telomerize right: add the clorox of 0.1-0.3%, processed 40 minutes for 38 ℃.
Dechlorination: the sodium thiosulfate consumption is 1.2-1.4 times of residual chlorine dose in the slurry.
Acid treatment: added at normal temperatures the salt acid treatment 60 minutes.
Manufacture paper with pulp: the slurry after the acid treatment send the oven dry of manufacturing paper with pulp of pulpboard workshop after washing, cuts at last metering and packs.By present embodiment gained bamboo pulp for cellulose viscose, content of alphacellulose 94%, pentosan 2.8%, whiteness 88, iron part 9ppm, ash content 0.12%.
Embodiment 3
Get the raw materials ready: bamboo wood is cut into the long rectangle bamboo chip of 20-50mm through bamboo cutter, requires qualification rate to reach more than 80%.
Washing: bamboo chip enters digester through flush away surface impurity behind the rinsing machine and after removing excessive moisture.
Prehydrolysis: after bamboo chip installs pot by the dress pot density of 200kg/m3 after the washing, heat up after being full of hydrolyzate in the digester, be raised to 165 ℃ in 60 minutes to protect 200 minutes, after hydrolysis is finished with hydrolyzate suction hydrolyzate storagetank as next pot hydrolysis medium.
Boiling: adopt the full liquid phase displacement cooking of sulfate.Alkali charge in Na2O to over dry bamboo chip weight 22%, sulphidity is in Na2O 25%, be raised to 140 ℃ in 40 minutes, protected 20 minutes, be raised to again 160 ℃ in 80 minutes and protected 180 minutes, blowing after the terminal point displacement is finished, get slurry yield rate 38.2%, content of alphacellulose 96.5%, pentosan 3%, Kappa number 9, iron part 25ppm.
Bleaching: adopt O-D0-EOP-D1 technique, oxygen floats 100 ℃ of temperature, pressure 0.5MPa, 60 minutes time; D0 section ClO2 is to oven dry stock consumption 1%, 65 ℃ of temperature, 120 minutes time; EOP section alkali is to oven dry stock consumption 2.5%, and hydrogen peroxide is to oven dry stock consumption 0.07%, and oxygen is pressed 0.1MPa, temperature 70 C, 120 minutes time; D1 section ClO2 is to oven dry stock consumption 0.5%, 65 ℃ of temperature, 120 minutes time.
Telomerize right: add the clorox of 0.1-0.3%, processed 60 minutes for 38 ℃.
Dechlorination: the sodium thiosulfate consumption is 1.2-1.4 times of residual chlorine dose in the slurry.
Acid treatment: added at normal temperatures the salt acid treatment 60 minutes.
Manufacture paper with pulp: the slurry after the acid treatment send the oven dry of manufacturing paper with pulp of pulpboard workshop after washing, cuts at last metering and packs.By present embodiment gained bamboo pulp for cellulose viscose, content of alphacellulose 94.5%, pentosan 2.2%, whiteness 89, iron part 5ppm, ash content 0.10%.
Embodiment 4
Get the raw materials ready: bamboo wood is cut into the long rectangle bamboo chip of 20-50mm through bamboo cutter, requires qualification rate to reach more than 80%.
Washing: bamboo chip enters digester through flush away surface impurity behind the rinsing machine and after removing excessive moisture.
Prehydrolysis: after bamboo chip installs pot by the dress pot density of 200kg/m3 after the washing, heat up after being full of hydrolyzate in the digester, be raised to 160 ℃ in 180 minutes to protect 180 minutes, after hydrolysis is finished with hydrolyzate suction hydrolyzate storagetank as next pot hydrolysis medium.
Boiling: adopt the full liquid phase displacement cooking of sulfate.To over dry bamboo chip weight 20%, sulphidity is warmed up to 162 ℃ and protected 150 minutes in Na2O 20% alkali charge in Na2O, terminal point displacement finishes that laggard row is cold to be spurted, and gets slurry yield rate 40%, content of alphacellulose 96.5%, pentosan 2.7%, Kappa number 9, iron part 32ppm.
Bleaching: adopt O-D0-EOP-D1 technique, oxygen floats 105 ℃ of temperature, pressure 0.5MPa, 60 minutes time; D0 section ClO2 is to oven dry stock consumption 1%, 65 ℃ of temperature, 120 minutes time; EOP section alkali is to oven dry stock consumption 2.5%, and hydrogen peroxide is to oven dry stock consumption 0.07%, and oxygen is pressed 0.1MPa, temperature 70 C, 120 minutes time; D1 section ClO2 is to oven dry stock consumption 0.5%, 65 ℃ of temperature, 120 minutes time.
Telomerize right: add the clorox of 0.1-0.3%, processed 60 minutes for 40 ℃.
Dechlorination: the sodium thiosulfate consumption is 1.2-1.4 times of residual chlorine dose in the slurry.
Acid treatment: 40 ℃ of lower adding salt acid treatment 60 minutes.
Manufacture paper with pulp: the slurry after the acid treatment send the oven dry of manufacturing paper with pulp of pulpboard workshop after washing, cuts at last metering and packs.By present embodiment gained bamboo pulp for cellulose viscose, content of alphacellulose 95.7%, pentosan 2.0%, whiteness 89, iron part 3ppm, ash content 0.09%.
Claims (2)
1. a full liquid phase prehydrolysis sulfate displacement cooking prepares the method for bamboo pulp, comprise get the raw materials ready, wash material, prehydrolysis, boiling, wash material, screen, bleach, telomerize right, dechlorination, acid treatment, it is characterized in that:
(1), get the raw materials ready: bamboo wood is cut into long 20-50mm, the rectangle bamboo chip of wide 10-20 mm, for subsequent use;
(2), wash material: the bamboo chip that cuts is washed first, remove after the washing surface impurity, for subsequent use;
(3), prehydrolysis: bamboo chip carries out first the prehydrolysis step before carrying out sulphate cook after the washing; Described prehydrolysis is carried out in digester, mix as hydrolysis medium in the 9:1-4:1 ratio with clear water and reuse hydrolyzate, the hydrolyzate complete bamboo chip in the submergence digester just in digester during hydrolysis, be full liquid-phase hydrolysis, hydrolysis pressure is 0.6-0.75MPa, dwell time is 120-300 minute, and the hydrolyzate of generation carries out the part reuse;
(4), boiling: described boiling is carried out in digester, adopts the full liquid phase displacement cooking of sulfate technology, the black liquor part reuse that boiling produces, technological parameter is: the alkali mass fraction accounts for the 18-30% of over dry bamboo chip weight, with Na
2The O meter; Sulphidity is 15-25%, with Na
2The O meter; Protected 120-300 minute at 0.6-0.75MPa, the gained slurry is removed impurity after washing the material screen choosing;
(5), bleaching: in oxygen floats tower, chlorine dioxide upwelling and down-welling tower, caustic tower, carry out employing O-D0-EOP-D1 bleaching process, bleaching time 60-240 minute, bleaching temperature 60-100 ℃;
(6), telomerize right: in the hypochlorite treating column, carry out, add the clorox of 0.1-0.3%, processed 40-70 minute at 35-40 ℃;
(7), dechlorination: slurry does not wash after right through telomerizing, and directly carries out dechlorination between acid treatment and hypochlorite are processed, and used antichlor is sodium thiosulfate, consumption be residual chlorine dose in the slurry 1.2-1.4 doubly;
(8), acid treatment: in acid accumulator treatment tower, carry out, and add a small amount of chelating agent 25-45 ℃ of processing 40-60 minute.
2. full liquid phase prehydrolysis sulfate displacement cooking according to claim 1 prepares the method for bamboo pulp, it is characterized in that, adopts NaOH and Na in the described boiling step
2S is with Na
2The O meter is cooking liquor by the mixed liquor of the mass ratio of 1:3-1:5.6.
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| CN102321990A (en) * | 2011-09-16 | 2012-01-18 | 四川永丰纸业股份有限公司 | Method for preparing bamboo pulp with full liquid phase pre-hydrolytic sulfate rapid displacement cooking |
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| CN114960248A (en) * | 2022-06-30 | 2022-08-30 | 泰盛科技（集团）股份有限公司 | Preparation method of bamboo pulp for Lyocell fiber and product thereof |
| CN116145457B (en) * | 2022-11-24 | 2024-06-14 | 泰盛科技（集团）股份有限公司 | Preparation method of bleached bamboo pulp |
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