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CN102493257B - Masson pine dissolving pulp and production method thereof - Google Patents

Masson pine dissolving pulp and production method thereof Download PDF

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Publication number
CN102493257B
CN102493257B CN 201110403237 CN201110403237A CN102493257B CN 102493257 B CN102493257 B CN 102493257B CN 201110403237 CN201110403237 CN 201110403237 CN 201110403237 A CN201110403237 A CN 201110403237A CN 102493257 B CN102493257 B CN 102493257B
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pulp
cooking
black liquor
bleaching
temperature
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CN102493257A (en
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马乐凡
周鲲鹏
徐远梅
万政
黄百文
徐应盛
屈琴琴
周万勇
汪芳
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Hunan Jun Thai New Materials Technology Co Ltd
Changsha University of Science and Technology
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Hu'nan Juntai Pulp Paper Co Ltd
Changsha University of Science and Technology
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Abstract

一种马尾松溶解浆及其生产方法,该马尾松溶解浆由马尾松木片经蒸汽预水解、硫酸盐法蒸煮、二段氧脱木素、D0EoPD1D2漂白而制得,白度不低于89%、甲种纤维素不低于91%、多戊糖不高于3%、动力粘度值为9~25mPa.s、灰分不高于0.1%、铁含量不高于15mg·kg-1。所述马尾松溶解浆的生产方法包括以下步骤:马尾松木片经过蒸汽预水解,蒸汽预水解P-因子为300~800;蒸汽预水解后进行硫酸盐法蒸煮制浆;浆料经二段氧脱木素后,进行D0EoPD1D2漂白;漂白后浆料进行洗涤干燥处理成马尾松溶解浆。A dissolving pulp of masson pine and a production method thereof, the dissolving pulp of masson pine is prepared by steam prehydrolysis of masson pine wood chips, kraft cooking, two-stage oxygen delignification, and D 0 Eo P D 1 D 2 bleaching, The whiteness is not lower than 89%, the cellulose A is not lower than 91%, the pentose is not higher than 3%, the dynamic viscosity is 9-25mPa.s, the ash content is not higher than 0.1%, and the iron content is not higher than 15mg • kg −1 . The production method of the masson pine dissolving pulp comprises the following steps: the masson pine wood chips undergo steam pre-hydrolysis, and the P-factor of the steam pre-hydrolysis is 300-800; after the steam pre-hydrolysis, kraft cooking and pulping are carried out; After delignification, D 0 Eo P D 1 D 2 bleaching is carried out; after bleaching, the pulp is washed and dried to become masson pine dissolving pulp.

Description

A kind of Chinese red pine dissolving pulp and production method thereof
Technical field
The present invention relates to a kind of cellulose pulp, especially relate to a kind of Chinese red pine dissolving pulp, the invention still further relates to a kind of production method of cellulose pulp, especially relate to a kind of production method of Chinese red pine dissolving pulp.
Background technology
Common chemical pulping is the lignin of removing in pulping process in plant fiber material, keeps as much as possible cellulose and hemicellulose; Dissolving pulp requires to remove lignin and hemicellulose in pulping process, only keep cellulose, and therefore, early stage dissolving pulp is to adopt the high cotton linter production of content of cellulose.Due to socioeconomic fast development, living standards of the people improve constantly, and the consumption of resource is rapid growth also, particularly also rapid growth of the raw materials consumption of textile industry viscose glue, cellulose mystery and nitrated production field.At present the quantity of the prepared dissolving pulp of cotton linter far can not satisfy the demand in weaving dissolving pulp, nitrated dissolving pulp, acetate dissolution slurry, cellulose ether field.Along with the growth of dissolving pulp demand, at present raw materials for production are take timber as main, and domestic also have the enterprise that produces cellulose viscose pulp take bamboo as raw material.
Patent CN101158121A discloses the technique of making dissolving pulp with ethanol, sulfate, acetic acid, and technique sequentially comprises blank, screening ash disposal, washes material, ethanol extracting, sulphate cook, slurries separation, washing, purifying, chlorination processing, alkali treatment, acetic acid bleaching+H 2O 2The organic bleaching of oxidation, sour complexing are processed, are manufactured paper with pulp.Though production procedure can be effectively shortened in this invention, improve utilize production such as bamboo wood, timber, masson pine, ramulus mori, Chinese alpine rush for the dissolving pulp of weaving, nitrated dissolving pulp, acetate dissolution starch, cellulose ether dissolving pulp field the production efficiency of dissolving pulp, improve simultaneously the yield rate that bamboo wood, timber, masson pine, ramulus mori, Chinese alpine rush etc. are produced dissolving pulp.
Patent CN1013682951A discloses a kind of preparation method of Chinese red pine dissolving pulp, comprises the following steps: 1) get the raw materials ready, choose the masson pine raw material; 2) steam prehydrolysis, technical conditions are: 165~180 ℃ of temperature, pressure 6.5~8.0kg/cm 2, time 50~120min; 3) soda boiling, technical conditions are: total alkali content is with respect to oven dry stock amount 18~25%, total time: the 150~240min that heats up, little steam bleeding number of times: 〉=1 time, be divided into and be three phases: the phase I, be increased to 130~140 ℃ by initial temperature, heating-up time 70~90min; Second stage rises to 165~180 ℃ by 130~140 ℃, heating-up time 70~90min, and 5~10min wherein exits one time; Phase III, 165~180 ℃, insulation 50~70min; Batch turning after boiling, wash material, slightly starched; 4) the pressurized screen screening is adopted in washing, screening, desanding; 5) bleaching, technical conditions are: bleaching liquor effective chlorine density 20~30g/L, bleaching liquor base excess concentration 1~6g/L, bleaching time: 270~310min; 6) acid treatment, technical conditions are: with the relative oven dry stock amount 2.0~5.0% of acid amount, time: 40~60min, temperature: normal temperature; 7) the pressurized screen screening is adopted in bleaching screening; 8) papermaking.
Above invention is adopted and is contained the elemental chlorine bleaching process, and waste water is difficult to process, and big for environment pollution, the whiteness of gained paper pulp is lower, and metal ion content is also higher.
Summary of the invention
In order to overcome the defective of prior art, technical problem to be solved by this invention is that the better Chinese red pine dissolving pulps of performance such as a kind of whiteness, viscosity, purity are provided; For this reason, the present invention also will provide a kind of method of making this Chinese red pine dissolving pulp.
For solving the problems of the technologies described above, dissolving pulp of the present invention by the masson pine wood chip through steam prehydrolysis, kraft cooking, two sections oxygen delignifications, D 0Eo PD 1D 2Bleaching forms, whiteness is not less than 89%, alpha cellulose is not less than 91%, pentosan not higher than 3%, the dynamic viscosity value be 9~25mPa.s, ash content not higher than 0.1%, iron content is higher than 15mgkg -1
In order to obtain above-mentioned Chinese red pine dissolving pulp, manufacture method of the present invention comprises following several step:
(1) in the pinus massoniana sheet was packed digester into, wood chip was through steam prehydrolysis, and the steam prehydrolysis P-factor is 300~800;
(2) through the post-job wood chip of step (1) in digester, be filled with the cooking liquor of 135~145 ℃, in and the acidic materials that produce of prehydrolysis and wood chip is carried out elementary boiling, the cooking liquor sulphidity that this step is used is 15%~30%, with the effective alkali consumption of sodium oxide molybdena calculating as 7%~10% of over dry wood chip weight;
(3) utilize the cooking liquor that the cooking liquor of 145~170 ℃ adds step (2) to replace at least one black liquor slot, the effective alkali consumption that the cooking liquor sulphidity that this step is used is 15%~30%, calculate with sodium oxide molybdena is as 9%~12% of over dry wood chip weight;
(4) step (3) is added cooking liquor heat temperature raising in digester, after reaching 160~172 ℃ of temperature, stopping heating up enters holding stage, reaches at 900~1400 o'clock until the H factor, completes this step;
(5) with step (4) gained slurry, filter black liquor with pulp washing and add the cooking liquor in digester to replace at least one black liquor slot step (3), make the interior slurry temperature of digester lower than 100 ℃;
(6) with step (5) gained slurry, send in spraying pot, through black liquid extraction, obtain masson pine prehydrolysis natural color pulp by screening;
(7) step (6) gained masson pine prehydrolysis natural color pulp after two sections oxygen delignifications, carries out D 0Eo PD 1D 2Bleaching;
(8) the bleaching disposed slurry washs drying and is processed into Chinese red pine dissolving pulp.
Preferably, the process conditions of the described steam prehydrolysis of step (1) are: be warming up to 160~175 ℃ with steam at 25~40 min after the masson pine chip filling, be incubated to the P-factor at 160~175 ℃ and reach 300~800.
Preferably, the described cooking liquor of step (3) is replaced at least one black liquor slot and is: enter the first black liquor slot lower than the cooking liquors of 100 ℃, the cooking liquor that is not less than 100 ℃ enters the second black liquor slot.
Preferably, the described cooking liquor of step (5) is replaced at least one black liquor slot and is: be not less than 160 ℃ enter the 3rd black liquor slot, 140~160 ℃ enter the 4th black liquor slot, lower than 140 ℃ enter the 5th black liquor slot or described the second black liquor slot.
Preferably, the cooking liquor that step (2) is described 135~145 ℃ is the interior black liquor of the second black liquor slot and/or the 5th black liquor slot and the mixed liquor of alkali lye, and described alkali lye is the causticization alkali that obtains in commercially available alkali or alkali recovery process.
Preferably, the cooking liquor that step (3) is described 145~170 ℃ is the interior black liquor of the 3rd black liquor slot and/or the 4th black liquor slot and the mixed liquor of alkali lye, and described alkali lye is the causticization alkali that obtains in commercially available alkali or alkali recovery process.
Preferably, the described two sections oxygen delignifications of step (7), first paragraph Oxygen Delignification of Fast-Growing condition is: NaOH consumption 2%~3%, oxygen pressure 1.0 ~ 1.5 MPa, MgSO 4Consumption 0.2%~0.4%, oxygen delignification slurry concentration 8%~12%, 85~95 ℃ of temperature, times 30~60 min; Slurry after one section oxygen delignification does not wash, and then carries out the second segment oxygen delignification, and second segment oxygen delignification condition is: oxygen pressure 1.0 ~ 1.5 MPa, 95~100 ℃ of oxygen delignification temperature, times 40~60 min.
Preferably, the described D of step (7) 0Eo PD 1D 2Bleaching, D 0The process conditions of section are: ClO 2Consumption 1%~2%, bleached pulp concentration 8%~12%, time 40~60min, 60~75 ℃ of temperature are regulated with sulfuric acid and are made bleaching endpoint pH≤2.6; E OPThe process conditions of section are: NaOH consumption 1%~2%, H 2O 2Consumption 0.5%~1%, O 2Pressure 1.0 ~ 1.5MPa, bleached pulp concentration 8%~12%, time 60~90min, 75~95 ℃ of temperature, bleaching endpoint pH 11~12; D 1The process conditions of section are: ClO 2Consumption 0.4%~0.8%, bleached pulp concentration 8%~12%, time 120~150min, 60~75 ℃ of temperature, making the bleaching endpoint pH with the sulfuric acid adjusting is 4~5; D 2The process conditions of section are: ClO 2Consumption 0.2%~0.5%, bleached pulp concentration 8%~12%, time 60~100min, 60~75 ℃ of temperature, making the bleaching endpoint pH with sulfuric acid or NaOH adjusting is 4~5.
Above preferred version can be implemented separately, also can two and two above scheme combination enforcements.
The invention has the beneficial effects as follows: because adopting steam prehydrolysis, oxygen delignification, element chlorine free bleaching, the generation of waste water and waste gas is few, and pollutional load is low, is easy to process, little to ambient influnence, the products obtained therefrom quality is easy to control, can satisfy well QUALITY STANDARD and customer requirements; Can reclaim the energy in digestion process, energy consumption is lower.Because adopting ClO 2 bleaching, effectively reduce in slurry the heavy metal ion contents such as gray iron, improve the reactivity worth of slurry.
The specific embodiment
Embodiment 1:
The pinus massoniana sheet is packed into after digester, is warming up to 160 ℃ with steam at 25min, carries out steam prehydrolysis, is incubated to the prehydrolysis P-factor to reach 400 under maximum temperature.Through the post-job wood chip of prehydrolysis in digester, be filled with the cooking liquor of 135~145 ℃, in and the acidic materials that produce of prehydrolysis and wood chip is carried out elementary boiling, this step cooking liquor used is the black liquor and the mixed liquor of commercially available alkali and akali sulphide in aftermentioned the 5th black liquor slot, and sulphidity is 15%, take the effective alkali consumption of sodium oxide molybdena calculating as 7% of over dry wood chip weight.Cooking liquor in wood chip after utilizing the cooking liquor of 145~170 ℃ with elementary cooking operation cements out, enter the first black liquor slot lower than the cooking liquors of 100 ℃, the cooking liquor that is not less than 100 ℃ enters the second black liquor slot, the cooking liquor that this step is used is the mixed liquor of the black liquor of aftermentioned the 3rd black liquor slot and commercially available alkali, akali sulphide, and the effective alkali consumption that sulphidity is 30%, calculate take sodium oxide molybdena is as 12% of over dry wood chip weight.To the cooking liquor heat temperature raising in digester, after reaching 172 ℃ of temperature, stop heating up and enter holding stage, reach at 1300 o'clock until the H factor, filtering black liquor with pulp washing will add the cooking liquor in digester to cement out, make slurry temperature in digester lower than 100 ℃, be not less than 160 ℃ enter the 3rd black liquor slot, 140 ℃~160 ℃ enter the 4th black liquor slot and lower than 140 ℃ enter the 5th black liquor slot or the second black liquor slot.After completing, boiling with the gained slurry, sends in spraying pot, through black liquid extraction, obtain masson pine prehydrolysis natural color pulp by screening.Gained masson pine prehydrolysis natural color pulp is through two sections oxygen delignification, and first paragraph Oxygen Delignification of Fast-Growing condition is: the NaOH consumption be absolute dried paper pulp weight 3%, oxygen pressure 1.5 MPa, oxygen delignification slurry concentration 8%, 95 ℃ of temperature, MgSO 4Consumption be absolute dried paper pulp weight 0.4%, oxygen delignification times 30 min; Slurry after one section oxygen delignification does not wash, and then carries out the second segment oxygen delignification, and second segment oxygen delignification condition is: oxygen pressure 1.0 MPa, 95 ℃ of oxygen delignification temperature, oxygen delignification times 60 min.The oxygen delignification disposed slurry is through D 0Eo PD 1D 2Bleaching, wherein D 0The process conditions of section are: ClO 2Consumption is 1% of absolute dried paper pulp weight, bleached pulp concentration 12%, and time 40min, 75 ℃ of bleaching temperatures, making the bleaching endpoint pH with the sulfuric acid adjusting is 2.3; E OPThe process conditions of section are: the NaOH consumption is 2% of absolute dried paper pulp weight, H 2O 2Consumption is 1% of absolute dried paper pulp weight, O 2Pressure 1.5MPa, bleached pulp concentration 8%, time 90min, 75 ℃ of bleaching temperatures, bleaching endpoint pH 11; D 1The process conditions of section are: ClO 2Consumption is 0.8% of absolute dried paper pulp weight, bleached pulp concentration 8%, and time 120min, 75 ℃ of bleaching temperatures, making the bleaching endpoint pH with the sulfuric acid adjusting is 4; D 2The process conditions of section are: ClO 2Consumption is 0.2% of absolute dried paper pulp weight, bleached pulp concentration 8%, and time 60min, 60 ℃ of bleaching temperatures, making the bleaching endpoint pH with sulfuric acid or NaOH adjusting is 5.
Embodiment 2:
The pinus massoniana sheet is packed into after digester, is warming up to 175 ℃ with steam at 40min, carries out steam prehydrolysis, is incubated to the prehydrolysis P-factor to reach 650 under maximum temperature.Through the post-job wood chip of prehydrolysis in digester, be filled with the cooking liquor of 135~145 ℃, in and the acidic materials that produce of prehydrolysis and wood chip is carried out elementary boiling, this step cooking liquor used is the mixed liquor of the causticization alkali that obtains in black liquor and alkali recovery process in aftermentioned the 5th black liquor slot, and sulphidity is 30%, take the effective alkali consumption of sodium oxide molybdena calculating as 10% of over dry wood chip weight.Cooking liquor in wood chip after utilizing the cooking liquor of 145~160 ℃ with elementary cooking operation cements out, enter the first black liquor slot lower than the cooking liquors of 100 ℃, the cooking liquor that is not less than 100 ℃ enters the second black liquor slot, the cooking liquor that this step is used is the mixed liquor of the black liquor of aftermentioned the 3rd black liquor slot and commercially available alkali, akali sulphide, and the effective alkali consumption that sulphidity is 15%, calculate take sodium oxide molybdena is as 9% of over dry wood chip weight.To the cooking liquor heat temperature raising in digester, after reaching 160 ℃ of temperature, stop heating up and enter holding stage, reach at 1400 o'clock until the H factor, filtering black liquor with pulp washing will add the cooking liquor in digester to cement out, make slurry temperature in digester lower than 100 ℃, be not less than 160 ℃ enter the 3rd black liquor slot, 140 ℃~160 ℃ enter the 4th black liquor slot and lower than 140 ℃ enter the 5th black liquor slot or the second black liquor slot.After completing, boiling with the gained slurry, sends in spraying pot, through black liquid extraction, obtain masson pine prehydrolysis natural color pulp by screening.Gained masson pine prehydrolysis natural color pulp is through two sections oxygen delignification, and first paragraph Oxygen Delignification of Fast-Growing condition is: the NaOH consumption be absolute dried paper pulp weight 2%, oxygen pressure 1.0MPa, MgSO 4Consumption be absolute dried paper pulp weight 0.2%, oxygen delignification slurry concentration 12%, 85 ℃ of temperature, times 60 min; Slurry after one section oxygen delignification does not wash, and then carries out the second segment oxygen delignification, and second segment oxygen delignification condition is: oxygen pressure 1.5MPa, 100 ℃ of oxygen delignification temperature, times 40 min.The oxygen delignification disposed slurry is through D 0Eo PD 1D 2Bleaching, wherein D 0The process conditions of section are: ClO 2Consumption is 2% of absolute dried paper pulp weight, bleached pulp concentration 8%, and time 40min, temperature 60 C, making the bleaching endpoint pH with the sulfuric acid adjusting is 2.4; E OPThe process conditions of section are: the NaOH consumption is 1% of absolute dried paper pulp weight, H 2O 2Consumption is 0.5% of absolute dried paper pulp weight, O 2Pressure 1.0MPa, bleached pulp concentration 12%, time 60min, 95 ℃ of temperature, bleaching endpoint pH 12; D 1The process conditions of section are: ClO 2Consumption is 0.4% of absolute dried paper pulp weight, bleached pulp concentration 12%, and time 150min, temperature 60 C, making the bleaching endpoint pH with the sulfuric acid adjusting is 5; D 2The process conditions of section are: ClO 2Consumption is 0.5% of absolute dried paper pulp weight, bleached pulp concentration 12%, and time 100min, 75 ℃ of temperature, making the bleaching endpoint pH with sulfuric acid or NaOH adjusting is 4.
Embodiment 3:
The pinus massoniana sheet is packed into after digester, is warming up to 170 ℃ with steam at 35min, carries out steam prehydrolysis, is incubated to the prehydrolysis P-factor to reach 500 under maximum temperature.Through the post-job wood chip of prehydrolysis in digester, be filled with the cooking liquor of 135~145 ℃, in and the acidic materials that produce of prehydrolysis and wood chip is carried out elementary boiling, this step cooking liquor used is the mixed liquor of the causticization alkali that obtains in black liquor and alkali recovery process in aftermentioned the second black liquor slot, and sulphidity is 22%, take the effective alkali consumption of sodium oxide molybdena calculating as 8% of over dry wood chip weight.Cooking liquor in wood chip after utilizing the cooking liquor of 145~168 ℃ with elementary cooking operation cements out, enter the first black liquor slot lower than the cooking liquors of 100 ℃, the cooking liquor that is not less than 100 ℃ enters the second black liquor slot, the cooking liquor that this step is used is the mixed liquor of the causticization alkali that obtains in the black liquor of aftermentioned the 4th black liquor slot and alkali recovery process, and the effective alkali consumption that sulphidity is 23%, calculate take sodium oxide molybdena is as 11% of over dry wood chip weight.To the cooking liquor heat temperature raising in digester, after reaching 168 ℃ of temperature, stop heating up and enter holding stage, reach at 1350 o'clock until the H factor, filtering black liquor with pulp washing will add the cooking liquor in digester to cement out, make slurry temperature in digester lower than 100 ℃, be not less than 160 ℃ enter the 3rd black liquor slot, 140 ℃~160 ℃ enter the 4th black liquor slot and lower than 140 ℃ enter the 5th black liquor slot or the second black liquor slot.After completing, boiling with the gained slurry, sends in spraying pot, through black liquid extraction, obtain masson pine prehydrolysis natural color pulp by screening.Gained masson pine prehydrolysis natural color pulp is through two sections oxygen delignification, and the process conditions of first paragraph oxygen delignification are: the NaOH consumption be absolute dried paper pulp weight 2.5%, oxygen pressure 1.3 MPa, MgSO 4Consumption be absolute dried paper pulp weight 0.3%, oxygen delignification slurry concentration 10%, 90 ℃ of temperature, time 45min; Slurry after one section oxygen delignification then carries out the second segment oxygen delignification without washing, and second segment oxygen delignification condition is: oxygen pressure 1.1MPa, 97 ℃ of oxygen delignification temperature, times 50 min.The oxygen delignification disposed slurry is through D 0Eo PD 1D 2Bleaching, D 0The process conditions of section are: ClO 2Consumption is 1.5% of absolute dried paper pulp weight, bleached pulp concentration 10%, and time 50min, temperature 70 C, making the bleaching endpoint pH with the sulfuric acid adjusting is 2.5; E OPThe process conditions of section are: the NaOH consumption is 1.5% of absolute dried paper pulp weight, H 2O 2Consumption is 0.7% of absolute dried paper pulp weight, O 2Pressure 1.0MPa, bleached pulp concentration 10%, time 75min, 85 ℃ of temperature, bleaching endpoint pH 11.5; D 1The process conditions of section are: ClO 2Consumption is 0.6% of absolute dried paper pulp weight, bleached pulp concentration 10%, and time 135min, 68 ℃ of temperature, making the bleaching endpoint pH with the sulfuric acid adjusting is 4.5; D 2The process conditions of section are: ClO 2Consumption is 0.35% of absolute dried paper pulp weight, bleached pulp concentration 10%, and time 80min, temperature 70 C, making the bleaching endpoint pH with sulfuric acid or NaOH adjusting is 4.5.
Embodiment 4:
The pinus massoniana sheet is packed into after digester, is warming up to 168 ℃ with steam at 30min, carries out steam prehydrolysis, is incubated to the prehydrolysis P-factor to reach 300 under maximum temperature.Through the post-job wood chip of prehydrolysis in digester, be filled with the cooking liquor of 135~145 ℃, in and the acidic materials that produce of prehydrolysis and wood chip is carried out elementary boiling, this step cooking liquor used is the mixed liquor of the causticization alkali that obtains in black liquor and alkali recovery process in aftermentioned the second black liquor slot and the 5th black liquor slot, and sulphidity is 25%, take the effective alkali consumption of sodium oxide molybdena calculating as 8% of over dry wood chip weight.Cooking liquor in wood chip after utilizing the cooking liquor of 145~170 ℃ with elementary cooking operation cements out, enter the first black liquor slot lower than the cooking liquors of 100 ℃, the cooking liquor that is not less than 100 ℃ enters the second black liquor slot, the cooking liquor that this step is used is the mixed liquor of the causticization alkali that obtains in the black liquor of aftermentioned the 3rd black liquor slot and the 4th black liquor slot and alkali recovery process, and the effective alkali consumption that sulphidity is 24%, calculate take sodium oxide molybdena is as 11% of over dry wood chip weight.To the cooking liquor heat temperature raising in digester, after reaching 167 ℃ of temperature, stop heating up and enter holding stage, reach at 900 o'clock until the H factor, filtering black liquor with pulp washing will add the cooking liquor in digester to cement out, make slurry temperature in digester lower than 100 ℃, be not less than 160 ℃ enter the 3rd black liquor slot, 140 ℃~160 ℃ enter the 4th black liquor slot and lower than 140 ℃ enter the 5th black liquor slot or the second black liquor slot.After completing, boiling with the gained slurry, sends in spraying pot, through black liquid extraction, obtain masson pine prehydrolysis natural color pulp by screening.Gained masson pine prehydrolysis natural color pulp is through two sections oxygen delignification, and the process conditions of first paragraph oxygen delignification are: the NaOH consumption be absolute dried paper pulp weight 2.7%, oxygen pressure 1.5 MPa, 95 ℃ of temperature, MgSO 4Consumption be absolute dried paper pulp weight 0.4%, oxygen delignification slurry concentration 11%, times 40 min; Slurry after one section oxygen delignification does not wash, and then carries out the second segment oxygen delignification, and the process conditions of second segment oxygen delignification are: oxygen pressure 1.2 MPa, 98 ℃ of temperature, times 58 min.The oxygen delignification disposed slurry is through D 0Eo PD 1D 2Bleaching, D 0The process conditions of section are: ClO 2Consumption is 1.8% of absolute dried paper pulp weight, bleached pulp concentration 11.5%, and time 55min, temperature 70 C, making the bleaching endpoint pH with the sulfuric acid adjusting is 2.6; E OPThe process conditions of section are: the NaOH consumption is 1.4% of absolute dried paper pulp weight, H 2O 2Consumption is 0.7% of absolute dried paper pulp weight, O 2Pressure 1.1MPa, bleached pulp concentration 10.3%, time 80min, 85 ℃ of temperature, bleaching endpoint pH 11.6; D 1The process conditions of section are: ClO 2Consumption is 0.6% of absolute dried paper pulp weight, bleached pulp concentration 11.7%, and time 140min, 72 ℃ of temperature, making the bleaching endpoint pH with the sulfuric acid adjusting is 4.5; D 2The process conditions of section are: ClO 2Consumption is 0.29% of absolute dried paper pulp weight, bleached pulp concentration 10.5%, and time 85min, 72 ℃ of temperature, making the bleaching endpoint pH with sulfuric acid or NaOH adjusting is 4.7.
Embodiment 5:
The pinus massoniana sheet is packed into after digester, is warming up to 173 ℃ with steam at 35min, carries out steam prehydrolysis, is incubated to the prehydrolysis P-factor to reach 800 under maximum temperature.Through the post-job wood chip of prehydrolysis in digester, be filled with 135~145 cooking liquor, in and the acidic materials that produce of prehydrolysis and wood chip is carried out elementary boiling, this step cooking liquor used is the mixed liquor of the causticization alkali that obtains in black liquor and alkali recovery process in aftermentioned the second black liquor slot and the 5th black liquor slot, and sulphidity is 27%, take the effective alkali consumption of sodium oxide molybdena calculating as 8.5% of over dry wood chip weight.Cooking liquor in wood chip after utilizing the cooking liquor of 145~165 ℃ with elementary cooking operation cements out, enter the first black liquor slot lower than the cooking liquors of 100 ℃, the cooking liquor that is not less than 100 ℃ enters the second black liquor slot, the cooking liquor that this step is used is the mixed liquor of the causticization alkali that obtains in the black liquor of aftermentioned the 3rd black liquor slot and the 4th black liquor slot and alkali recovery process, and the effective alkali consumption that sulphidity is 22%, calculate take sodium oxide molybdena is as 10% of over dry wood chip weight.To the cooking liquor heat temperature raising in digester, after reaching 168 ℃ of temperature, stop heating up and enter holding stage, reach at 1400 o'clock until the H factor, filtering black liquor with pulp washing will add the cooking liquor in digester to cement out, make slurry temperature in digester lower than 100 ℃, be not less than 160 ℃ enter the 3rd black liquor slot, 140 ℃~160 ℃ enter the 4th black liquor slot and lower than 140 ℃ enter the 5th black liquor slot or the second black liquor slot.After completing, boiling with the gained slurry, sends in spraying pot, through black liquid extraction, obtain masson pine prehydrolysis natural color pulp by screening.Gained masson pine prehydrolysis natural color pulp is through two sections oxygen delignification, and the process conditions of first paragraph oxygen delignification are: the NaOH consumption be absolute dried paper pulp weight 2.7%, oxygen pressure 1.4 MPa, MgSO 4Consumption be absolute dried paper pulp weight 0.3%, oxygen delignification slurry concentration 11%, 90 ℃ of temperature, times 35 min; Slurry after one section oxygen delignification does not wash, and then carries out the second segment oxygen delignification, and the process conditions of second segment oxygen delignification are: oxygen pressure 1.1 MPa, 97 ℃ of oxygen delignification temperature, times 52 min.The oxygen delignification disposed slurry is through D 0Eo PD 1D 2Bleaching, D 0The process conditions of section are: ClO 2Consumption is 1.5% of absolute dried paper pulp weight, bleached pulp concentration 10.7%, and time 55min, temperature 70 C, making the bleaching endpoint pH with the sulfuric acid adjusting is 2.5; E OPThe process conditions of section are: the NaOH consumption is 1.2% of absolute dried paper pulp weight, H 2O 2Consumption is 0.6% of absolute dried paper pulp weight, O 2Pressure 1.02MPa, bleached pulp concentration 11.7%, time 70min, 85 ℃ of temperature, bleaching endpoint pH 11.7; D 1The process conditions of section are: ClO 2Consumption is 0.5% of absolute dried paper pulp weight, bleached pulp concentration 11%, and time 130min, 69 ℃ of temperature, making the bleaching endpoint pH with the sulfuric acid adjusting is 4.6; D 2The process conditions of section are: ClO 2Consumption is 0.26% of absolute dried paper pulp weight, bleached pulp concentration 11.8, and time 92min, 67 ℃ of temperature, making the bleaching endpoint pH with sulfuric acid or NaOH adjusting is 4.5.
The part process of above-described embodiment and test data is as follows as a result:
Test event Embodiment 1 Embodiment 2 Embodiment 3 Embodiment 4 Embodiment 5
The prehydrolysis P factor 400 650 500 300 800
The boiling H-factor 1300 1400 1350 900 1400
Screened yield after boiling (%) 35.70 34.43 35.42 36.26 33.97
Brown stock viscosity (mLg -1 766 714 727 655 623
Whiteness (ISO%) 90.23 90.52 89.73 89.21 91.03
Alpha cellulose (%) 91.64 92.65 92.06 91.02 92.1
Pentosan (%) 2.93 2.82 2.90 3.62 2.57
Dynamic viscosity (mPa.s) 25 22 23 19 9
Ash content (%) 0.06 0.06 0.05 0.06 0.05
Iron content (mgkg -1 12 14 13 15 15
In the present invention, the analysis of liquid used and product quality is all undertaken by national standard method, and definite method of the P factor please refer to " pulping chemistry " that Chen Jiaxiang writes, and light industry in June nineteen ninety publishing house publishes, and the content that the 232-236 page discloses is determined.
Obviously, the invention is not restricted to above preferred embodiment, also can change other process conditions in spirit of the present invention, have same effect, therefore do not repeat.Those of ordinary skill in the art can from content disclosed by the invention directly or all methods of associating, also belong to content of the present invention.

Claims (7)

1. 一种马尾松溶解浆,白度不低于89%、甲种纤维素不低于91%、多戊糖不高于3%、动力粘度值为9~25mPa.s、灰分不高于0.1%、铁含量不高于15mg·kg-1,其特征在于,由马尾松木片经蒸汽预水解、硫酸盐法蒸煮、二段氧脱木素、D0EoPD1D2漂白而制得,制取过程包括以下步骤: 1. A masson pine dissolving pulp, with a whiteness of not less than 89%, a cellulose of not less than 91%, a polysaccharide not higher than 3%, a dynamic viscosity of 9-25mPa.s, and an ash content not higher than 0.1%, iron content not higher than 15mg·kg -1 , characterized in that it is made of masson pine wood chips through steam prehydrolysis, kraft cooking, two-stage oxygen delignification, and D 0 Eo P D 1 D 2 bleaching The preparation process includes the following steps: (1) 马尾松木片装入蒸煮锅内,木片经过蒸汽预水解,蒸汽预水解P-因子为300~800; (1) Masson pine wood chips are put into the cooking pot, and the wood chips are pre-hydrolyzed by steam, and the P-factor of steam pre-hydrolysis is 300-800; (2) 经步骤(1)作业后的木片在蒸煮锅中,充入135~145℃的蒸煮液,中和预水解产生的酸性物质并对木片进行初级蒸煮,本步骤使用的蒸煮液硫化度为15%~30%、以氧化钠计算的有效碱用量为绝干木片重量的7%~10%; (2) The wood chips after step (1) are filled in the cooking pot with cooking liquid at 135-145°C to neutralize the acidic substances produced by pre-hydrolysis and perform primary cooking on the wood chips. The degree of sulfidity of the cooking liquid used in this step is 15% to 30%, and the effective alkali dosage calculated by sodium oxide is 7% to 10% of the weight of dry wood chips; (3) 利用145~170℃的蒸煮液将步骤(2)加入的蒸煮液置换入至少一个黑液槽中,本步骤使用的蒸煮液硫化度为15%~30%、以氧化钠计算的有效碱用量为绝干木片重量的9%~12%; (3) Use the cooking liquid at 145-170°C to replace the cooking liquid added in step (2) into at least one black liquor tank. The cooking liquid used in this step has a sulfide degree of 15%-30%, and the effective The amount of alkali is 9% to 12% of the weight of dry wood chips; (4) 将步骤(3)加入蒸煮锅中的蒸煮液加热升温,达到160~172℃温度后,停止升温进入保温阶段,待H因子达到900~1400时,完成本步骤; (4) Add step (3) to the cooking liquid in the cooking pot and heat it up. After the temperature reaches 160-172°C, stop the heating and enter the heat preservation stage. When the H factor reaches 900-1400, complete this step; (5) 将步骤(4)所得浆料,用洗浆过滤黑液将步骤(3)加入蒸煮锅内的蒸煮液置换入至少一个黑液槽中,使蒸煮锅内的浆料温度低于100℃; (5) With the slurry obtained in step (4), filter the black liquor with pulp washing and replace the cooking solution added in the cooking pot in step (3) into at least one black liquor tank, so that the temperature of the slurry in the cooking pot is lower than 100 ℃; (6) 将步骤(5)所得浆料,送入喷放锅内,经黑液提取、筛选制得马尾松预水解本色浆; (6) Put the slurry obtained in step (5) into the spray pot, extract and screen the black liquor to obtain the pre-hydrolyzed natural color slurry of Pinus massoniana; (7) 步骤(6) 所得马尾松预水解本色浆经二段氧脱木素后,进行D0EoPD1D2漂白;所述二段氧脱木素,第一段氧脱木素工艺条件为:NaOH用量为绝干纸浆重量的2%~3%、氧气压力1.0~1.5 MPa、MgSO4用量为绝干纸浆重量的0.2%~0.4%、氧脱木素浆料浓度8wt%~12wt%、温度85~95℃、时间30~60 min;一段氧脱木素后的浆料不洗涤,接着进行第二段氧脱木素,第二段氧脱木素条件为:氧气压力1.0~1.5MPa、氧脱木素温度95~100℃、时间40~60 min;所述D0EoPD1D2漂白,D0段的工艺条件为:ClO2用量为绝干纸浆重量的1%~2%,漂白纸浆浓度8wt%~12wt%,时间40~60min,温度60~75℃,用硫酸调节使漂白终点pH值≤2.6;EOP段的工艺条件为:NaOH用量为绝干纸浆重量的1%~2%,H2O2用量为绝干纸浆重量的0.5%~1%,O2压力1.0~1.5MPa,漂白纸浆浓度8wt%~12wt%,时间60~90min,温度75~95℃,漂白终点pH值11~12;D1段的工艺条件为:ClO2用量为绝干纸浆重量的0.4%~0.8%,漂白纸浆浓度8wt%~12wt%,时间120~150min,温度60~75℃,用硫酸调节使漂白终点pH值为4~5;D2段的工艺条件为:ClO2用量为绝干纸浆重量的0.2%~0.5%,漂白纸浆浓度8wt%~12wt%,时间60~100min,温度60~75℃,用硫酸或NaOH调节使漂白终点pH值为4~5; (7) After the masson pine pre-hydrolyzed natural color pulp obtained in step (6) undergoes the second-stage oxygen delignification, D 0 Eo P D 1 D 2 bleaching is carried out; the second-stage oxygen delignification, the first-stage oxygen delignification The process conditions are: the amount of NaOH is 2% to 3% of the dry pulp weight, the oxygen pressure is 1.0 to 1.5 MPa, the amount of MgSO4 is 0.2% to 0.4% of the dry pulp weight, and the oxygen delignification pulp concentration is 8wt% to 12wt%, temperature 85-95°C, time 30-60 min; the pulp after the first stage of oxygen delignification is not washed, and then the second stage of oxygen delignification is carried out. The condition of the second stage of oxygen delignification is: oxygen pressure 1.0 ~1.5MPa, oxygen delignification temperature 95~100℃, time 40~60 min; the process conditions of the D 0 Eo P D 1 D 2 bleaching, D 0 stage are: the amount of ClO 2 is 1% of the dry pulp weight %~2%, bleached pulp concentration 8wt%~12wt%, time 40~60min, temperature 60~75°C, adjust with sulfuric acid to make the pH value of the bleaching end point ≤2.6; the process conditions of the E OP section are: the amount of NaOH is the absolute dry pulp 1% to 2% of the weight, the amount of H 2 O 2 is 0.5% to 1% of the dry pulp weight, the O 2 pressure is 1.0~1.5MPa, the bleached pulp concentration is 8wt%~12wt%, the time is 60~90min, the temperature is 75~ 95°C, the pH value of the bleaching end point is 11-12; the process conditions of the D 1 stage are: the amount of ClO2 is 0.4%-0.8% of the weight of the dry pulp, the concentration of the bleached pulp is 8wt%-12wt%, the time is 120-150min, and the temperature is 60 ~75°C, adjust with sulfuric acid to make the pH value of the end point of bleaching 4~5; the process conditions of D 2 stage are: the amount of ClO2 is 0.2%~0.5% of the absolute dry pulp weight, the concentration of bleached pulp is 8wt%~12wt%, and the time 60-100min, temperature 60-75°C, adjust with sulfuric acid or NaOH to make the pH value of the bleaching end point 4-5;  (8) 漂白后浆料进行洗涤干燥处理成马尾松溶解浆。 (8) After bleaching, the pulp is washed and dried into dissolving pulp of masson pine. 2.一种权利要求1所述马尾松溶解浆的生产方法,其特征在于,包括以下步骤: 2. a production method of masson pine dissolving pulp described in claim 1, is characterized in that, comprises the following steps: (1) 马尾松木片装入蒸煮锅内,木片经过蒸汽预水解,蒸汽预水解P-因子为300~800; (1) Masson pine wood chips are put into the cooking pot, and the wood chips are pre-hydrolyzed by steam, and the P-factor of steam pre-hydrolysis is 300-800; (2) 经步骤(1)作业后的木片在蒸煮锅中,充入135~145℃的蒸煮液,中和预水解产生的酸性物质并对木片进行初级蒸煮,本步骤使用的蒸煮液硫化度为15%~30%、以氧化钠计算的有效碱用量为绝干木片重量的7%~10%; (2) The wood chips after step (1) are filled in the cooking pot with cooking liquid at 135-145°C to neutralize the acidic substances produced by pre-hydrolysis and perform primary cooking on the wood chips. The degree of sulfidity of the cooking liquid used in this step is 15% to 30%, and the effective alkali dosage calculated by sodium oxide is 7% to 10% of the weight of dry wood chips; (3) 利用145~170℃的蒸煮液将步骤(2)加入的蒸煮液置换入至少一个黑液槽中,本步骤使用的蒸煮液硫化度为15%~30%、以氧化钠计算的有效碱用量为绝干木片重量的9%~12%; (3) Use the cooking liquid at 145-170°C to replace the cooking liquid added in step (2) into at least one black liquor tank. The cooking liquid used in this step has a sulfide degree of 15%-30%, and the effective The amount of alkali is 9% to 12% of the weight of dry wood chips; (4) 将步骤(3)加入蒸煮锅中的蒸煮液加热升温,达到160~172℃温度后,停止升温进入保温阶段,待H因子达到900~1400时,完成本步骤; (4) Add step (3) to the cooking liquid in the cooking pot and heat it up. After the temperature reaches 160-172°C, stop the heating and enter the heat preservation stage. When the H factor reaches 900-1400, complete this step; (5) 将步骤(4)所得浆料,用洗浆过滤黑液将步骤(3)加入蒸煮锅内的蒸煮液置换入至少一个黑液槽中,使蒸煮锅内的浆料温度低于100℃; (5) With the slurry obtained in step (4), filter the black liquor with pulp washing and replace the cooking solution added in the cooking pot in step (3) into at least one black liquor tank, so that the temperature of the slurry in the cooking pot is lower than 100 ℃; (6) 将步骤(5)所得浆料,送入喷放锅内,经黑液提取、筛选制得马尾松预水解本色浆; (6) Put the slurry obtained in step (5) into the spray pot, extract and screen the black liquor to obtain the pre-hydrolyzed natural color slurry of Pinus massoniana; (7) 步骤(6) 所得马尾松预水解本色浆经二段氧脱木素后,进行D0EoPD1D2漂白;所述二段氧脱木素,第一段氧脱木素工艺条件为:NaOH用量为绝干纸浆重量的2%~3%、氧气压力1.0~1.5 MPa、MgSO4用量为绝干纸浆重量的0.2%~0.4%、氧脱木素浆料浓度8wt%~12wt%、温度85~95℃、时间30~60 min;一段氧脱木素后的浆料不洗涤,接着进行第二段氧脱木素,第二段氧脱木素条件为:氧气压力1.0~1.5MPa、氧脱木素温度95~100℃、时间40~60 min;所述D0EoPD1D2漂白,D0段的工艺条件为:ClO2用量为绝干纸浆重量的1%~2%,漂白纸浆浓度8wt%~12wt%,时间40~60min,温度60~75℃,用硫酸调节使漂白终点pH值≤2.6;EOP段的工艺条件为:NaOH用量为绝干纸浆重量的1%~2%,H2O2用量为绝干纸浆重量的0.5%~1%,O2压力1.0~1.5MPa,漂白纸浆浓度8wt%~12wt%,时间60~90min,温度75~95℃,漂白终点pH值11~12;D1段的工艺条件为:ClO2用量为绝干纸浆重量的0.4%~0.8%,漂白纸浆浓度8wt%~12wt%,时间120~150min,温度60~75℃,用硫酸调节使漂白终点pH值为4~5;D2段的工艺条件为:ClO2用量为绝干纸浆重量的0.2%~0.5%,漂白纸浆浓度8wt%~12wt%,时间60~100min,温度60~75℃,用硫酸或NaOH调节使漂白终点pH值为4~5; (7) After the masson pine pre-hydrolyzed natural color pulp obtained in step (6) undergoes the second-stage oxygen delignification, D 0 Eo P D 1 D 2 bleaching is carried out; the second-stage oxygen delignification, the first-stage oxygen delignification The process conditions are: the amount of NaOH is 2% to 3% of the dry pulp weight, the oxygen pressure is 1.0 to 1.5 MPa, the amount of MgSO4 is 0.2% to 0.4% of the dry pulp weight, and the oxygen delignification pulp concentration is 8wt% to 12wt%, temperature 85-95°C, time 30-60 min; the pulp after the first stage of oxygen delignification is not washed, and then the second stage of oxygen delignification is carried out. The condition of the second stage of oxygen delignification is: oxygen pressure 1.0 ~1.5MPa, oxygen delignification temperature 95~100℃, time 40~60 min; the process conditions of the D 0 Eo P D 1 D 2 bleaching, D 0 stage are: the amount of ClO 2 is 1% of the dry pulp weight %~2%, bleached pulp concentration 8wt%~12wt%, time 40~60min, temperature 60~75°C, adjust with sulfuric acid to make the pH value of the bleaching end point ≤2.6; the process conditions of the E OP section are: the amount of NaOH is the absolute dry pulp 1% to 2% of the weight, the amount of H 2 O 2 is 0.5% to 1% of the dry pulp weight, the O 2 pressure is 1.0~1.5MPa, the bleached pulp concentration is 8wt%~12wt%, the time is 60~90min, the temperature is 75~ 95°C, the pH value of the bleaching end point is 11-12; the process conditions of the D 1 stage are: the amount of ClO2 is 0.4%-0.8% of the weight of the dry pulp, the concentration of the bleached pulp is 8wt%-12wt%, the time is 120-150min, and the temperature is 60 ~75°C, adjust with sulfuric acid to make the pH value of the end point of bleaching 4~5; the process conditions of D 2 stage are: the amount of ClO2 is 0.2%~0.5% of the absolute dry pulp weight, the concentration of bleached pulp is 8wt%~12wt%, and the time 60-100min, temperature 60-75°C, adjust with sulfuric acid or NaOH to make the pH value of the bleaching end point 4-5;  (8) 漂白后浆料进行洗涤干燥处理成马尾松溶解浆。 (8) After bleaching, the pulp is washed and dried into dissolving pulp of masson pine. 3.根据权利要求2所述马尾松溶解浆的生产方法,其特征在于:步骤(1)所述蒸汽预水解的工艺条件为:马尾松木片装锅后用蒸汽在25~40min升温至160~175℃,在160~175℃保温至P-因子达到300~800。 3. according to the production method of the described masson pine dissolving pulp of claim 2, it is characterized in that: the processing condition of the steam prehydrolysis described in step (1) is: after the masson pine wood chips are packed in a pot, the temperature is raised to 160~160~160℃ in 25~40min with steam. 175°C, keep warm at 160-175°C until the P-factor reaches 300-800. 4.根据权利要求2所述马尾松溶解浆的生产方法,其特征在于:步骤(3)所述蒸煮液置换入至少一个黑液槽中为:低于100℃的蒸煮液进入第一黑液槽,不低于100℃的蒸煮液进入第二黑液槽。 4. according to the production method of the described masson pine dissolving pulp of claim 2, it is characterized in that: step (3) described cooking liquor is replaced in at least one black liquor tank: the cooking liquor below 100 ℃ enters the first black liquor Tank, the cooking liquid not lower than 100°C enters the second black liquor tank. 5.根据权利要求2所述马尾松溶解浆的生产方法,其特征在于:步骤(5)所述蒸煮液置换入至少一个黑液槽中为:不低于160℃的进入第三黑液槽、140~160℃的进入第四黑液槽、低于140℃的进入第五黑液槽或所述第二黑液槽。 5. The production method of masson pine dissolving pulp according to claim 2, characterized in that: the cooking liquid in step (5) is replaced in at least one black liquor tank as: entering the third black liquor tank at a temperature not lower than 160°C , 140-160 ° C into the fourth black liquor tank, lower than 140 ° C into the fifth black liquor tank or the second black liquor tank. 6.根据权利要求2所述马尾松溶解浆的生产方法,其特征在于:步骤(2)所述135~145℃的蒸煮液为第二黑液槽和/或第五黑液槽内的黑液与碱液的混合液,所述碱液为商品碱或碱回收过程中得到的苛化碱。 6. The production method of masson pine dissolving pulp according to claim 2, characterized in that: the cooking liquor at 135-145°C in step (2) is the black liquor in the second black liquor tank and/or the fifth black liquor tank. The mixed solution of lye and lye, the lye is the caustic soda obtained in the process of commercial alkali or alkali recovery. 7.根据权利要求2所述马尾松溶解浆的生产方法,其特征在于:步骤(3)所述145~170℃的蒸煮液为第三黑液槽和/或第四黑液槽内的黑液与碱液的混合液,所述碱液为商品碱或碱回收过程中得到的苛化碱。 7. The production method of masson pine dissolving pulp according to claim 2, characterized in that: the cooking liquor at 145-170°C in step (3) is the black liquor in the third black liquor tank and/or the fourth black liquor tank. The mixed solution of lye and lye, the lye is the caustic soda obtained in the process of commercial alkali or alkali recovery.
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