Background technology
Pulp has another name called dissolving pulp, the method that adopts both at home and abroad at present is more, there is hydrolysis to join alkaline cooking technique, kraft cooking technique is joined in hydrolysis, digesting technoloy is changed in the hydrolysis configuration, also have steam prehydrolysis to join kraft cooking technique, and external comparatively advanced person's is to adopt steam prehydrolysis configuration to change digesting technoloy.But this technique has only obtained successful Application in the timber dissolving pulp at present.Steam prehydrolysis configuration change digesting technoloy at steam saving, enhancing productivity and solving all has very outstanding advantage aspect contaminated wastewater and the atmosphere pollution.Bamboo wood produce the viscose glue pulp at present ripe technique be that Hydrolyze method is joined the traditional batch boiling, but this to improve production capacity, steam saving, effectively to solve discharge of wastewater and atmosphere pollution very difficult.Therefore, grafting steam prehydrolysis replacing and digesting technoloy has important economic worth and social value in the production of bamboo wood pulp.
At present, existing enterprise is adopting decatize displacement cooking technology to produce bamboo pulp, obtaining breakthrough aspect energy-saving and emission-reduction and the increase production capacity, but there is the poor problem of reactivity worth in prepared bamboo pulp after using, the opposite bamboo pulp reactivity worth of using the liquid phase water solution to produce is far better, the bamboo pulp that the liquid phase water solution is produced adds 11ml carbon disulfide can both be passed through, and the decatize replacement technique with identical physical and chemical index is produced bamboo pulp and is added 11ml carbon disulfide and can not pass through, and be added to 15ml could pass through substantially.So, virtually increased production cost to down-stream enterprise, also increased simultaneously ambient pollution burden, and this series products can't use separately, can only allocate in the wood pulp in a small amount of ratio and use, greatly reduce the exclusive advantage of bamboo fibre, limited bamboo pulp and used the field, its added value does not obtain excavating.
Cause that decatize bamboo pulp reactivity worth is bad two reasons: the one, bamboo fibre self molecular structure factor, the 2nd, preparation technology is not in place.Because Steaming does not have acid solution extractive process in the liquid-phase hydrolysis technique, cause fully being opened in prehydrolysis process bamboo fibre structure, and the impurity such as the lignin of association on fiber, hemicellulose only have the soda boiling of dependence to remove, and this is the maximum difference of Steaming and liquid-phase hydrolysis technique.In the currently used decatize replacement technique, without the acid discharge process, with the white liquid neutralization of heat, cause alkali lye consumption in antacid process, reduced lignin and the hemicellulose ability of removing, the white liquid neutralization of heat makes the very fast swollen of fiber, causes later stage alkali lye can not enter smoothly fibrous inside, the course of reaction delignification is not thorough, and it is comprehensive easily to produce lignin.Use hot black liquor to fill in the present decatize replacement technique and displace neutralizer, when carrying out this step, the low alkali state of high temperature can appear in tablet in the pot, adds the excessive swollen of tablet in early stage, alkali lye in the hot black liquor can not enter tablet inside smoothly, causes half steaming even.For this reason, the bamboo pulp quality of doing corresponding improvement production for present decatize replacement technique is more even, has better reactivity worth.
Summary of the invention
The object of the present invention is to provide a kind of preparation method with bamboo pulp of better reactivity worth.
The present invention is achieved in that by a kind of
Decatize sulfate displacement cooking prepares the method for bamboo pulp, comprise and get the raw materials ready, wash material, steam dress pot, steam prehydrolysis, acid discharge, white liquid neutralization, pre-boiling, soda boiling, time retractable pot, washing, bleaching, acid treatment and manufacture paper with pulp, 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, for subsequent use;
(2) wash material: the bamboo chip that cuts is washed first, removed the impurity on surface after the washing, for subsequent use;
(3) steam dress pot: in pot, pass into low-pressure steam in described (2) when bamboo chip enters digester, limit dress pot limit preheating;
(4) steam prehydrolysis: carry out the prehydrolysis step after the dress pot is finished; Described prehydrolysis is carried out in digester, and steam is lower filter plate and the adding of digester lower cone bottom from steamer, and steam prehydrolysis temperature is 160 ℃-175 ℃, temperature retention time 30-180 minute;
(5) acid discharge: prehydrolysis is drained the acid solution that condensation in the pot produces latter stage;
(6) white liquid neutralization: after decatize meets the requirements of the P factor, in digester, inject a certain amount of white liquid, in and the outer condensed water of tablet and the sour molten hemicellulose in the tablet, make pot an interior bamboo chip transfer rapidly strong basicity to, termination prehydrolysis is reacted;
(7) pre-boiling: and then inject simultaneously hot black liquor and Re Bai liquid after with white liquid injecting neutralization, the white liquid layer after the neutralization is pushed into pot mouthful until be full of hot black liquor in the pot from the bottom of a pan, stop feed liquor after filling with black liquor in pot, beat circulation 0-30 minute;
(8) soda boiling: after finishing pre-boiling, continue in steamer, to inject simultaneously the white liquid of heat and hot black liquor and the black liquor of described step (7) is all ejected, with Na
2The O meter, white liquid quality is 8-16% to over dry tablet quality, sulphidity 15-25% is warmed up to 160-170 ℃ and protected 30-180 minute;
(9) reclaim: soda boiling reaches after the H factor of regulation beginning and injects washing in the pot and float the rare black liquor of low temperature, and the displacement interior hot black liquor that takes the dish out of the pot is stored for subsequent use to hot black liquor groove and warm black liquor slot heat recovery in the pot;
(10) put pot: treat that kettle temperature drops to below 100 ℃, begin to take out slurry and put pot;
(11) washing: adopt closed screening, squeezing washing to carry out the adverse current pulp washing with the vacuum displacement washing mode of combining;
(12) bleaching: adopt O-D0-E
P-D1 bleaching process, oxygen take off (O) section condition: use alkali 2-4%, and hydrogen peroxide 0.1-2%, oxygen is pressed 0.5MPa, temperature 90-120 ℃, time 60-90 minute; D0 section condition is: ClO
2Consumption 0.8-1.5%, pH value 2-4, temperature 50-80 ℃, time 90-180 minute; E
PThe section condition is: use alkali 1-3%, hydrogen peroxide 0.5-2%, chelating agent: 0.05-0.2%, temperature 70-90 ℃, time 90-180 minute; D1 section condition is: ClO
2Consumption 0.2-0.7%, chelating agent: 0.05-0.2%, pH value 3-5, temperature 60-90 ℃, time 120-240 minute;
(13) acid treatment: chelating agent 0.05-0.2%, pH value 2-4 processed 40-90 minute at 30-60 ℃;
(14) 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.
Prepare the method for bamboo pulp according to decatize solution sulfate displacement cooking of the present invention, it is characterized in that, the hot black liquor in the described step (7) (8) is black liquor in the hot black liquor groove that reclaims in the step (9), and its residual alkali content is with Na
2O counts 10-40g/l.
Prepare the method for bamboo pulp according to decatize solution sulfate displacement cooking of the present invention, it is characterized in that the white liquid temp in the described step (6) is 70-120 ℃.
According to above-mentioned preparation method, after described steaming stage finishes, the content of alphacellulose of gained slurry 〉=95%, pentosan≤5%, average degree of polymerization are 600-800; After described acid treatment finishes, the content of alphacellulose of gained slurry 〉=95%, pentosan≤4.5%, average degree of polymerization are 450-550, whiteness 82-88%.
The present invention is with respect to present decatize replacement technique, and its advantage is: 1, adopt steam dress pot mode to make tablet shift to an earlier date preheating, improved production efficiency, tablet is to a certain degree softening simultaneously, can improve dress pot amount.2, the mode by the many places admission has overcome that present steam prehydrolysis is inhomogeneous, the problem of the too high generation cellulose degradation of local temperature.3, decatize process multiplex low-pressure steam has to greatest extent reduced the degree of injury of decatize to fiber, and is fine beneficial to improving first.4, increased the acid discharge process, made alkali lye obtain more effective utilization.5, the white liquid lower temperature of neutralization has increased later stage alkali lye osmotic effect, has improved the uniformity of boiling.6, adopt twice soda boiling mode after the prehydrolysis, guaranteed the residual alkali concn that final stage of cooking is high, make delignification more thorough, boiling is more even, has overcome the deficiency of Steaming.By above-mentioned measure, prepared bamboo pulp adds 11ml carbon disulfide can both be passed through substantially, and reactivity worth is greatly improved.
The specific embodiment
Now the present invention is further made detailed explanation: the present invention implements in such a way;
Embodiment 1
(1) get the raw materials ready: bamboo wood is cut into the rectangle bamboo chip of long 20-50mm, wide 10-20 mm, for subsequent use.
(2) wash material: the bamboo chip that cuts is washed first, removed the impurity on surface after the washing, for subsequent use.
(3) steam dress pot: in pot, pass into low-pressure steam, limit dress pot limit preheating.
(4) steam prehydrolysis: bamboo chip carries out first steaming step before carrying out sulphate cook after the washing; Described decatize is carried out in digester, and steam circulates and the adding of digester lower cone bottom under the bottom of a pan, and steam prehydrolysis temperature is 160 ℃, temperature retention time 180 minutes.
(5) acid discharge: prehydrolysis is drained the acid solution that condensation in the pot produces latter stage.
(6) neutralization: after decatize meets the requirements of the P factor, in digester, inject 120 ℃ white liquid, make in the whole pot to transfer rapidly strong basicity to, stop the prehydrolysis reaction.
(7) pre-boiling: injecting neutralization hot black liquor and Re Bai liquid that and then to inject 150 ℃ of residual alkali after with white liquid be 15g/l, will neutralize white liquid layer from the bottom of a pan be pushed into the pot mouth until pot in be full of this hot black liquor.Then play circulation 15 minutes.
(8) soda boiling: after finishing pre-boiling, continue in steamer, to inject simultaneously the hot black liquor of the white liquid of heat and step (9), with Na
2The O meter, white liquid quality is 10% to over dry tablet quality, sulphidity 25% was protected 180 minutes at 160 ℃.
(9) reclaim: soda boiling reaches after the H factor of regulation beginning and injects washing in the pot and float the rare black liquor of low temperature, and the displacement interior hot black liquor that takes the dish out of the pot is stored for subsequent use to hot black liquor groove and warm black liquor slot heat recovery in the pot.
(10) put pot: treat that kettle temperature drops to 95 ℃, begin to take out slurry and put pot.
(11) washing: adopt closed screening, squeezing washing to carry out the adverse current pulp washing with the vacuum displacement washing mode of combining
(12) bleaching: oxygen takes off (O) section condition and is: with alkali 2%, oxygen is pressed 0.5MPa, 100 ℃ of temperature, 60 minutes time.D0 section condition is: ClO
2Consumption 1%, pH value 2.5, temperature 60 C, 120 minutes time.E
PThe section condition is: with alkali 1.5%, hydrogen peroxide 1%, and chelating agent: 0.05%, temperature 70 C, 90 minutes time.D1 section condition is: ClO
2Consumption 0.3%, chelating agent: 0.05%, pH value 3, temperature 60 C, 150 minutes time.
(13) acid treatment: chelating agent 0.1%, pH value 2 was processed 40 minutes at 38 ℃.
Slurry after the acid treatment send the oven dry of manufacturing paper with pulp of pulpboard workshop after washing, cut at last metering and pack.By present embodiment gained bamboo pulp for cellulose viscose, content of alphacellulose 95%, whiteness 85%, iron part 20ppm, ash content 0.11%, 4 seconds/11ml of reactivity worth.
Embodiment 2
(1) get the raw materials ready: bamboo wood is cut into the rectangle bamboo chip of long 20-50mm, wide 10-20 mm, for subsequent use.
(2) wash material: the bamboo chip that cuts is washed first, removed the impurity on surface after the washing, for subsequent use.
(3) steam dress pot: in pot, pass into low-pressure steam, limit dress pot limit preheating.
(4) steam prehydrolysis: bamboo chip carries out first steaming step before carrying out sulphate cook after the washing; Described decatize is carried out in digester, and steam circulates and the adding of digester lower cone bottom under the bottom of a pan, and steam prehydrolysis temperature is 168 ℃, temperature retention time 75 minutes.
(5) acid discharge: prehydrolysis is drained the acid solution that condensation in the pot produces latter stage.
(6) neutralization: after decatize meets the requirements of the P factor, in digester, inject 100 ℃ white liquid, make in the whole pot to transfer rapidly strong basicity to, stop the prehydrolysis reaction.
(7) pre-boiling: injecting neutralization hot black liquor and Re Bai liquid that and then to inject 155 ℃ of residual alkali after with white liquid be 20g/l, will neutralize white liquid layer from the bottom of a pan be pushed into the pot mouth until pot in be full of this hot black liquor.Then play circulation 20 minutes.
(8) soda boiling: after finishing pre-boiling, continue in steamer, to inject simultaneously the hot black liquor of the white liquid of heat and step (9), with Na
2The O meter, white liquid quality is 13% to over dry tablet quality, sulphidity 23% was protected 100 minutes at 163 ℃.
(9) reclaim: soda boiling reaches after the H factor of regulation beginning and injects washing in the pot and float the rare black liquor of low temperature, and the displacement interior hot black liquor that takes the dish out of the pot is stored for subsequent use to hot black liquor groove and warm black liquor slot heat recovery in the pot.
(10) put pot: treat that kettle temperature drops to 95 ℃, begin to take out slurry and put pot.
(11) washing: adopt closed screening, squeezing washing to carry out the adverse current pulp washing with the vacuum displacement washing mode of combining.
(12) bleaching: oxygen takes off (O) section condition and is: with alkali 2.5%, oxygen is pressed 0.5MPa, 100 ℃ of temperature, 60 minutes time.D0 section condition is: ClO
2Consumption 1%, pH value 2.5, temperature 60 C, 120 minutes time.E
PThe section condition is: with alkali 1.5%, hydrogen peroxide 1%, and chelating agent: 0.05%, 75 ℃ of temperature, 120 minutes time.D1 section condition is: ClO
2Consumption 0.3%, chelating agent: 0.05%, pH value 3, temperature 60 C, 150 minutes time.
(13) acid treatment: chelating agent 0.1%, pH value 2 was processed 40 minutes at 38 ℃.
Slurry after the acid treatment send the oven dry of manufacturing paper with pulp of pulpboard workshop after washing, cut at last metering and pack.By present embodiment gained bamboo pulp for cellulose viscose, content of alphacellulose 95.5%, whiteness 87%, iron part 18ppm, ash content 0.08%, 2.6 seconds/11ml of reactivity worth.
Embodiment 3
(1) get the raw materials ready: bamboo wood is cut into the rectangle bamboo chip of long 20-50mm, wide 10-20 mm, for subsequent use.
(2) wash material: the bamboo chip that cuts is washed first, removed the impurity on surface after the washing, for subsequent use.
(3) steam dress pot: when entering digester, bamboo chip in pot, passes into low-pressure steam in described (2), limit dress pot limit preheating, and further improve dress pot amount.
(4) steam prehydrolysis: bamboo chip carries out first steaming step before carrying out sulphate cook after the washing; Described decatize is carried out in digester, and steam circulates and the adding of digester lower cone bottom under the bottom of a pan, and steam prehydrolysis temperature is 170 ℃, temperature retention time 60 minutes.
(5) acid discharge: prehydrolysis is drained the acid solution that condensation in the pot produces latter stage.
(6) neutralization: after decatize meets the requirements of the P factor, in digester, inject 75 ℃ white liquid, make in the whole pot to transfer rapidly strong basicity to, stop the prehydrolysis reaction.
(7) pre-boiling: injecting neutralization hot black liquor and Re Bai liquid that and then to inject 155 ℃ of residual alkali after with white liquid be 25g/l, will neutralize white liquid layer from the bottom of a pan be pushed into the pot mouth until pot in be full of this hot black liquor.Then play circulation 30 minutes.
(8) soda boiling: after finishing pre-boiling, continue in steamer, to inject simultaneously the hot black liquor of the white liquid of heat and step (9), with Na
2The O meter, white liquid quality is 16% to over dry tablet quality, sulphidity 20% was protected 60 minutes at 170 ℃.
(9) reclaim: soda boiling reaches after the H factor of regulation beginning and injects washing in the pot and float the rare black liquor of low temperature, and the displacement interior hot black liquor that takes the dish out of the pot is stored for subsequent use to hot black liquor groove and warm black liquor slot heat recovery in the pot.
(10) put pot: treat that kettle temperature drops to 98 ℃, begin to take out slurry and put pot.
(11) pulp washing: adopt closed screening, squeezing washing to carry out the adverse current pulp washing with the vacuum displacement washing mode of combining.
(12) bleaching: oxygen takes off (O) section condition and is: with alkali 3%, oxygen is pressed 0.5MPa, 105 ℃ of temperature, 60 minutes time.D0 section condition is: ClO
2Consumption 1%, pH value 3, temperature 60 C, 120 minutes time.E
PThe section condition is: with alkali 2%, hydrogen peroxide 1.5%, and chelating agent: 0.1%, 80 ℃ of temperature, 120 minutes time.D1 section condition is: ClO
2Consumption 0.3%, chelating agent: 0.1%, pH value 3, temperature 60 C, 240 minutes time.
(13), acid treatment: chelating agent 0.2%, pH value 2.5 was processed 60 minutes at 42 ℃.
Slurry after the acid treatment send the oven dry of manufacturing paper with pulp of pulpboard workshop after washing, cut at last metering and pack.By present embodiment gained bamboo pulp for cellulose viscose, content of alphacellulose 96%, whiteness 88%, iron part 19ppm, ash content 0.05%, 0.4 second/11ml of reactivity worth.