CN102321990A - Method for preparing bamboo pulp with full liquid phase pre-hydrolytic sulfate rapid displacement cooking - Google Patents
Method for preparing bamboo pulp with full liquid phase pre-hydrolytic sulfate rapid displacement cooking Download PDFInfo
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Abstract
The invention discloses a method for preparing bamboo pulp with full liquid phase pre-hydrolytic sulfate rapid displacement cooking. The method comprises the following steps of preparing for materials, washing the materials, pre-hydrolyzing, cooking, washing, selecting, bleaching, regulating the polymerization degree, dechlorinating and acid-treating. According to the method, after the cooking stage is finished, the obtained pulp has alpha cellulose content of not less than 95%, pentosan of not more than 4% and average polymerization degree of 550-700; and after the acid treating is finished, the obtained pulp has alpha cellulose content of not less than 93%, pentosan content of not more than 4.0%, average polymerization degree of 500-650 and whiteness of 82-86%. The processes of full liquid phase hydrolysis, full liquid phase cooking, hydrolysate recycling, recycled black liquor displacement cooking and chlorine dioxide clean bleaching are adopted in the method disclosed by the invention. The method has the characteristics of high whiteness, low viscosity and high polymerization degree of products, thus wastewater pollution is greatly reduced, the temperature rise time and steam are saved, the triple effects of energy saving, emission reduction and production increasing are achieved, and the problems of large wastewater pollution, high energy consumption and low capacity existing in the traditional pre-hydrolytic sulfate method for preparing pulp.
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, 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.Though cotton class natural fabric has good spinnability and reproducibility, limited because of its production capacity, price still rises steadily, and has satisfied not 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, be that raw material passes through the viscose that dissolving spinning technology produces and constituted market nominative office with wood pulps and bamboo pulp.Wherein, be that the bamboo fibre of raw material production has good anti-microbial property, anti-ultraviolet function and drapability with the bamboo pulp, made bamboo fiber towel, bamboo fibre bath towel, bamboo fibre daily necessities more and more receive 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, and very abundant bamboo resource is all arranged on China Sichuan, Guangxi, Guizhou and other places.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 to use the most widely, 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 generally is used to produce extraordinary senior dissolving pulp.Afterwards, developed prehydrolysis sulphate cook technology, and comprised acid hydrolysis sulphate cook technology, decatize hydrolysis sulphate cook technology and be the prehydrolysis sulphate cook technology of medium with water.Acid hydrolysis sulphate cook technology is owing to use a large amount of acid solutions, and the acid solution recovery system is complicated, and is big to equipment corrosion, and the water consumption is high, operating cost is also higher, and this method is seldom used.Decatize hydrolysis sulphate cook technology uses steam to be hydrolyzed, and hydrolysis efficiency is higher, but owing to temperature behind the steam entering steamer can't evenly be controlled, causes the hydrolysis uniformity relatively poor, and product quality is stable inadequately, and this method is not all adopted in general big production.The prehydrolysis sulphate cook technology that with water is 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 that producing medium-to-high grade viscose uses 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 really desirable; And hydrolyzate directly effluxes processing, has wasted great amount of heat energy and water resource, and the heating-up time is longer; So have still that energy consumption is higher, hydrolytically unstable, discharge liquor pollute the outstanding problem big, 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 realizes like this; Adopt a kind of full liquid phase prehydrolysis sulfate displacement cooking to prepare the method for bamboo pulp, method comprises down step: get the raw materials ready, wash material, prehydrolysis, boiling, washing, screening, 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, subsequent use;
(2), wash material: with the bamboo chip that cuts washing earlier, remove the impurity on surface after the washing, subsequent use;
(3), prehydrolysis: bamboo chip carries out the prehydrolysis step earlier before carrying out sulphate cook after washing; Said prehydrolysis is carried out in digester; Hydrolysis medium is the mixed liquor of clear water and hydrolyzate, and hydrolyzate shared volume parts in mixed liquor is 10-50%, the bamboo chip in the just complete submergence digester of hydrolyzate in digester during hydrolysis; Be full liquid-phase hydrolysis; Hydrolysis temperature is 164-174 ℃, and temperature retention 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 cooking technology of sulfate, the black liquor part reuse that boiling produces, technological parameter is: alkali charge is that 18-30% is (with Na
2The O meter), sulphidity is that 15-25% is (with Na
2The O meter), protected 120-300 minute at 164-174 ℃, the gained slurry is removed impurity after washing and screening;
(5), bleaching: in chlorine dioxide upwelling and down-welling tower, caustic tower, carry out employing D0-E-D1 bleaching process, bleaching time 60-240 minute, bleaching temperature 60-100 ℃ in advance after the acid treatment;
(6), telomerize right: in the hypochlorite treating column, carry out, add the clorox of 0.1-1%, handled 40-70 minute at 35-40 ℃;
(7), dechlorination: slurry does not wash after right through telomerizing, and directly between acid treatment and hypochlorite are handled, carries out dechlorination, and used antichlor is a 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, handled 40-60 minute at 35-70 ℃.
Prepare the method for bamboo pulp according to above-mentioned full liquid phase prehydrolysis sulfate displacement cooking, it is characterized in that the cooking liquor in the said boiling step is NaOH and Na
2The mixed liquor of S.
According to above-mentioned preparation method, after said steaming stage finishes, alpha cellulose content>=95% of gained slurry, pentosan≤4%, average degree of polymerization are 550-700; After said acid treatment finishes, alpha cellulose content>=93% of gained slurry, pentosan≤4.0%, average degree of polymerization are 500-650, whiteness 82-86%.
The invention has the advantages that: this method adopts full liquid-phase hydrolysis, full liquid phase cooking, hydrolyzate reuse, reuse black liquor displacement cooking and ClO 2 bleaching technology; Product viscosity is suitable, the degree of polymerization is high, whiteness is high; Both alleviated contaminated wastewater greatly; Saved heating-up time and steam 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 the present invention is made detailed explanation: the present invention implements in such a way;
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 gets into digester through flush away surface impurity behind the rinsing machine and after removing excessive moisture.
Prehydrolysis: after washing back bamboo chip installs pot by the dress pot density of 200kg/m3; In digester, charge into hydrolysis medium; Long-pending 10% of the hydrolysis medium cumulative volume that accounts for of the acidic hydrolysis liquid of reuse; After heat up, be raised to 165 ℃ and protected 180 minutes, after hydrolysis is accomplished with hydrolyzate suction hydrolyzate storagetank as next pot hydrolysis medium.
Boiling: adopt the full liquid phase cooking of sulfate.Alkali charge is with Na
2The O meter is to over dry bamboo chip weight 22%, and sulphidity is with Na
2O meter 25% is raised to 160 ℃ and protected 120 fens, and blowing after the terminal point displacement is accomplished gets slurry yield rate 34%, alpha cellulose content 95.1%, Kappa number 11, iron part 40ppm.
Bleaching: in advance D0-E-D1 technology is adopted in the acid back, and D0 section ClO2 is to oven dry stock consumption 1%, 60 ℃ of temperature, 120 minutes time; E section alkali is to oven dry stock consumption 2.5%, 70 ℃ of temperature, 120 minutes time; D1 section ClO2 is to oven dry stock consumption 0.5%, 60 ℃ of temperature, 240 minutes time.
Telomerize right: add the clorox of 0.1-0.3%, handled 40 minutes for 35 ℃.
Dechlorination: the sodium thiosulfate consumption is 1.2-1.4 a times of residual chlorine dose in the slurry.
Acid treatment: added the salt acid treatment at normal temperatures 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 metering at last and packs.By present embodiment gained bamboo pulp for cellulose viscose, alpha cellulose content 93%, whiteness 85%, iron part 20ppm, 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 gets into digester through flush away surface impurity behind the rinsing machine and after removing excessive moisture.
Prehydrolysis: after washing back bamboo chip installs pot by the dress pot density of 200kg/m3; Heat up after in digester, being full of hydrolysis medium; Long-pending 20% of the hydrolysis medium cumulative volume that accounts for of the acidic hydrolysis liquid of reuse; Be raised to 165 ℃ and protected 180 minutes, after hydrolysis is accomplished with hydrolyzate suction hydrolyzate storagetank as next pot hydrolysis medium.
Boiling: adopt the full liquid phase cooking of sulfate.Alkali charge is with Na
2The O meter is to over dry bamboo chip weight 22%, and sulphidity is with Na
2O meter 25% is raised to 165 ℃ and protected 140 fens, and blowing after the terminal point displacement is accomplished gets slurry yield rate 33%, alpha cellulose content 96%, Kappa number 10, iron part 38ppm.
Bleaching: in advance D0-E-D1 technology is adopted in the acid back, and 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%, 70 ℃ of temperature, 120 minutes time; D1 section ClO2 is to oven dry stock consumption 0.5%, 70 ℃ of temperature, 240 minutes time.
Telomerize right: add the clorox of 0.1-0.3%, handled 40 minutes for 38 ℃.
Dechlorination: the sodium thiosulfate consumption is 1.2-1.4 a times of residual chlorine dose in the slurry.
Acid treatment: added the salt acid treatment at normal temperatures 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 metering at last and packs.By present embodiment gained bamboo pulp for cellulose viscose, alpha cellulose content 94.2%, pentosan 3.6%, whiteness 85.5%, iron part 18ppm, 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 gets into digester through flush away surface impurity behind the rinsing machine and after removing excessive moisture.
Prehydrolysis: after washing back bamboo chip installs pot by the dress pot density of 200kg/m3; Heat up after in digester, being full of hydrolysis medium; Long-pending 20% of the hydrolysis medium cumulative volume that accounts for of the acidic hydrolysis liquid of reuse; Be raised to 170 ℃ and protected 120 fens, after hydrolysis is accomplished with hydrolyzate suction hydrolyzate storagetank as next pot hydrolysis medium.
Boiling: adopt the full liquid phase cooking of sulfate.Alkali charge is with Na
2The O meter is to over dry bamboo chip weight 20%, and sulphidity is with Na
2O meter 20% is raised to 170 ℃ and protected 120 fens, and blowing after the terminal point displacement is accomplished gets slurry yield rate 34.2%, alpha cellulose content 95.5%, Kappa number 8, iron part 45ppm.
Bleaching: in advance D0-E-D1 technology is adopted in the acid back, and 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%, 80 ℃ of temperature, 120 minutes time; D1 section ClO2 is to oven dry stock consumption 0.4%, 75 ℃ of temperature, 240 minutes time.
Telomerize right: add the clorox of 0.1-0.3%, handled 60 minutes for 38 ℃.
Dechlorination: the sodium thiosulfate consumption is 1.2-1.4 a times of residual chlorine dose in the slurry.
Acid treatment: add hydrochloric acid and handled 60 minutes down at 50 ℃.
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 metering at last and packs.By present embodiment gained bamboo pulp for cellulose viscose, alpha cellulose content 94.5%, pentosan 3.5%, whiteness 86%, iron part 15ppm, 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 gets into digester through flush away surface impurity behind the rinsing machine and after removing excessive moisture.
Prehydrolysis: after washing back bamboo chip installs pot by the dress pot density of 200kg/m3; Heat up after in digester, being full of hydrolysis medium; Long-pending 50% of the hydrolysis medium cumulative volume that accounts for of the acidic hydrolysis liquid of reuse; Be raised to 168 ℃ and protected 210 fens, after hydrolysis is accomplished with hydrolyzate suction hydrolyzate storagetank as next pot hydrolysis medium.
Boiling: adopt the full liquid phase cooking of sulfate.Alkali charge is with Na
2The O meter is to over dry bamboo chip weight 21%, and sulphidity is with Na
2O meter 20% is warmed up to 168 ℃ and protected 120 fens, and blowing after the terminal point displacement is accomplished gets slurry yield rate 33%, alpha cellulose content 95.5%, Kappa number 7.3, iron part 40ppm.
Bleaching: in advance D0-E-D1 technology is adopted in the acid back, and 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%, 70 ℃ of temperature, 120 minutes time; D1 section ClO2 is to oven dry stock consumption 0.5%, 75 ℃ of temperature, 240 minutes time.
Telomerize right: add the clorox of 0.1-0.3%, handled 60 minutes for 40 ℃.
Dechlorination: the sodium thiosulfate consumption is 1.2-1.4 a times of residual chlorine dose in the slurry.
Acid treatment: add salt acid treatment 40 minutes down at 70 ℃.
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 metering at last and packs.By present embodiment gained bamboo pulp for cellulose viscose, alpha cellulose content 94.7%, pentosan 3.3%, whiteness 85%, iron part 12ppm, ash content 0.09%.
Claims (2)
1. a full liquid phase prehydrolysis sulfate displacement cooking prepares the method for bamboo pulp, comprises getting the raw materials ready, washing material, prehydrolysis, boiling, wash material, screen, bleach, telomerize right, dechlorination and acid treatment, it is characterized in that:
(1), get the raw materials ready: bamboo wood is cut into the rectangle bamboo chip of long 20-50mm, wide 10-20 mm, subsequent use;
(2), wash material: with the bamboo chip that cuts washing earlier, remove the impurity on surface after the washing, subsequent use;
(3), prehydrolysis: bamboo chip carries out the prehydrolysis step earlier before carrying out sulphate cook after washing; Said prehydrolysis is carried out in digester; Hydrolysis medium is the mixed liquor of clear water and hydrolyzate, and hydrolyzate shared volume parts in mixed liquor is 10-50%, the bamboo chip in the just complete submergence digester of hydrolyzate in digester during hydrolysis; Be full liquid-phase hydrolysis; Hydrolysis temperature is 164 ℃-174 ℃, and temperature retention 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 cooking technology of sulfate, the black liquor part reuse that boiling produces, technological parameter is: with Na
2The O meter, the alkali mass fraction accounts for over dry bamboo chip weight 18-30%, Na
2The O meter, sulphidity is 15-25%, protects 120-300 minute at 164 ℃-174 ℃, the gained slurry is removed impurity after washing and screening;
(5), bleaching: through in chlorine dioxide upwelling and down-welling tower, caustic tower, carrying out employing D0-E-D1 bleaching process, bleaching time 60-240 minute, bleaching temperature 60-100 ℃ in advance after the acid treatment;
(6), telomerize right: in the hypochlorite treating column, carry out, add the clorox of 0.1-1%, handled 40-70 minute at 35-40 ℃;
(7), dechlorination: slurry does not wash after right through telomerizing, and directly between acid treatment and hypochlorite are handled, carries out dechlorination, and used antichlor is a 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, handled 40-60 minute at 35-70 ℃.
2. full liquid phase prehydrolysis sulfate displacement cooking according to claim 1 prepares the method for bamboo pulp, it is characterized in that, with Na
2The O meter, the cooking liquor in the said boiling step is Na
2S and NaOH press the mixed liquor of the mass ratio of 1:3-1:5.6.
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Cited By (7)
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| CN102888773A (en) * | 2012-10-17 | 2013-01-23 | 四川永丰纸业股份有限公司 | Technique for preparing bamboo pulp by cooking to two-grade full-liquid-phase sulphate |
| CN102888772A (en) * | 2012-10-17 | 2013-01-23 | 四川永丰纸业股份有限公司 | Method for preparing bamboo pulp by replacing cooking sulfate with steaming sulfate |
| CN103628341A (en) * | 2013-12-16 | 2014-03-12 | 广西大学 | Dissolving-grade bamboo pulp chlorine dioxide bleaching method |
| CN106702799A (en) * | 2016-12-02 | 2017-05-24 | 山东银鹰股份有限公司 | Method for preparing dissolving wood pulp for viscose fibers by modifying papermaking-grade wood pulp |
| CN107447588A (en) * | 2017-09-11 | 2017-12-08 | 四川唤初新材料有限公司 | The preparation technology of the instant lavatory paper of the full bamboo fibre of true qualities |
| CN107988835A (en) * | 2017-10-16 | 2018-05-04 | 四川永丰纸业股份有限公司 | A kind of method that low temperature displacement dipping produces high yield pulp1 true qualities bamboo pulp |
| CN116145457A (en) * | 2022-11-24 | 2023-05-23 | 泰盛科技（集团）股份有限公司 | Preparation method of bleached bamboo pulp |
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| CN102888773A (en) * | 2012-10-17 | 2013-01-23 | 四川永丰纸业股份有限公司 | Technique for preparing bamboo pulp by cooking to two-grade full-liquid-phase sulphate |
| CN102888772A (en) * | 2012-10-17 | 2013-01-23 | 四川永丰纸业股份有限公司 | Method for preparing bamboo pulp by replacing cooking sulfate with steaming sulfate |
| CN102888773B (en) * | 2012-10-17 | 2014-12-17 | 四川永丰纸业股份有限公司 | Technique for preparing bamboo pulp by cooking to two-grade full-liquid-phase sulphate |
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| CN103628341A (en) * | 2013-12-16 | 2014-03-12 | 广西大学 | Dissolving-grade bamboo pulp chlorine dioxide bleaching method |
| CN103628341B (en) * | 2013-12-16 | 2016-01-13 | 广西大学 | A kind of dissolving grade bamboo pulp ClO 2 bleaching method |
| CN106702799A (en) * | 2016-12-02 | 2017-05-24 | 山东银鹰股份有限公司 | Method for preparing dissolving wood pulp for viscose fibers by modifying papermaking-grade wood pulp |
| CN107447588A (en) * | 2017-09-11 | 2017-12-08 | 四川唤初新材料有限公司 | The preparation technology of the instant lavatory paper of the full bamboo fibre of true qualities |
| CN107988835A (en) * | 2017-10-16 | 2018-05-04 | 四川永丰纸业股份有限公司 | A kind of method that low temperature displacement dipping produces high yield pulp1 true qualities bamboo pulp |
| CN116145457A (en) * | 2022-11-24 | 2023-05-23 | 泰盛科技（集团）股份有限公司 | Preparation method of bleached bamboo pulp |
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Application publication date: 20120118 |