CN102493257B - Masson pine dissolving pulp and production method thereof - Google Patents
Masson pine dissolving pulp and production method thereof Download PDFInfo
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Abstract
The invention discloses a masson pine dissolving pulp and a production method thereof, wherein the masson pine dissolving pulp is prepared after the steam prehydrolysis, sulfate cooking, two stages of oxygen delignification and D0EoPD1 bleaching of masson pine pieces, the whiteness is not less than 89%, the alpha cellulose is not less than 91%, the pentosan 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 that: the masson pine pieces undergo the steam prehydrolysis, and the P- factor of the steam prehydrolysis is 300-800; the sulfate cooking is carried out after the steam prehydrolysis to obtain the pulp; the pulp undergoes the D0EoPD1 bleaching after two stages of oxygen delignification; and after the bleaching, the pulp is washed, dried and processed into the masson pine dissolving pulp.
Description
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. Chinese red pine dissolving pulp, whiteness are 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, it is characterized in that, by the masson pine wood chip through steam prehydrolysis, kraft cooking, two sections oxygen delignifications, D
0Eo
PD
1D
2Bleach and make, the process of producing comprises the following steps:
(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; Described two sections oxygen delignifications, first paragraph Oxygen Delignification of Fast-Growing condition is: the NaOH consumption be absolute dried paper pulp weight 2%～3%, oxygen pressure 1.0～1.5 MPa, MgSO
4Consumption be absolute dried paper pulp weight 0.2%～0.4%, oxygen delignification slurry concentration 8wt%～12wt%, 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 1.0～1.5MPa, 95～100 ℃ of oxygen delignification temperature, times 40～60 min; Described D
0Eo
PD
1D
2Bleaching, D
0The process conditions of section are: ClO
2Consumption is 1%～2% of absolute dried paper pulp weight, bleached pulp concentration 8wt%～12wt%, and 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: the NaOH consumption is 1%～2% of absolute dried paper pulp weight, H
2O
2Consumption is 0.5%～1% of absolute dried paper pulp weight, O
2Pressure 1.0 ~ 1.5MPa, bleached pulp concentration 8wt%～12wt%, time 60～90min, 75～95 ℃ of temperature, bleaching endpoint pH 11～12; D
1The process conditions of section are: ClO
2Consumption is 0.4%～0.8% of absolute dried paper pulp weight, bleached pulp concentration 8wt%～12wt%, and 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 is 0.2%～0.5% of absolute dried paper pulp weight, bleached pulp concentration 8wt%～12wt%, and time 60～100min, 60～75 ℃ of temperature, making the bleaching endpoint pH with sulfuric acid or NaOH adjusting is 4～5;
(8) the bleaching disposed slurry washs drying and is processed into Chinese red pine dissolving pulp.
2. the production method of the described Chinese red pine dissolving pulp of claim 1, is characterized in that, comprises the following steps:
(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; Described two sections oxygen delignifications, first paragraph Oxygen Delignification of Fast-Growing condition is: the NaOH consumption be absolute dried paper pulp weight 2%～3%, oxygen pressure 1.0～1.5 MPa, MgSO
4Consumption be absolute dried paper pulp weight 0.2%～0.4%, oxygen delignification slurry concentration 8wt%～12wt%, 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 1.0～1.5MPa, 95～100 ℃ of oxygen delignification temperature, times 40～60 min; Described D
0Eo
PD
1D
2Bleaching, D
0The process conditions of section are: ClO
2Consumption is 1%～2% of absolute dried paper pulp weight, bleached pulp concentration 8wt%～12wt%, and 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: the NaOH consumption is 1%～2% of absolute dried paper pulp weight, H
2O
2Consumption is 0.5%～1% of absolute dried paper pulp weight, O
2Pressure 1.0 ~ 1.5MPa, bleached pulp concentration 8wt%～12wt%, time 60～90min, 75～95 ℃ of temperature, bleaching endpoint pH 11～12; D
1The process conditions of section are: ClO
2Consumption is 0.4%～0.8% of absolute dried paper pulp weight, bleached pulp concentration 8wt%～12wt%, and 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 is 0.2%～0.5% of absolute dried paper pulp weight, bleached pulp concentration 8wt%～12wt%, and time 60～100min, 60～75 ℃ of temperature, making the bleaching endpoint pH with sulfuric acid or NaOH adjusting is 4～5;
(8) the bleaching disposed slurry washs drying and is processed into Chinese red pine dissolving pulp.
3. the production method of Chinese red pine dissolving pulp according to claim 2, it is characterized in that: the process conditions of the described steam prehydrolysis of step (1) are: be warming up to 160～175 ℃ with steam at 25～40min after the masson pine chip filling, be incubated to the P-factor at 160～175 ℃ and reach 300～800.
4. the production method of Chinese red pine dissolving pulp according to claim 2, it is characterized in that: 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.
5. the production method of Chinese red pine dissolving pulp according to claim 2, it is characterized in that: 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.
6. the production method of Chinese red pine dissolving pulp according to claim 2, it is characterized in that: 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.
7. the production method of Chinese red pine dissolving pulp according to claim 2, it is characterized in that: 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.
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| JP6075976B2 (en) * | 2012-06-15 | 2017-02-08 | 日本製紙株式会社 | Method for producing dissolved kraft pulp |
| CN102888772B (en) * | 2012-10-17 | 2015-01-28 | 四川永丰纸业股份有限公司 | Method for preparing bamboo pulp by replacing cooking sulfate with steaming sulfate |
| US10947669B2 (en) * | 2016-02-16 | 2021-03-16 | Valmet Ab | Method for recovering concentrated hydrolysate after hydrolysis of cellulose material |
| JP6423838B2 (en) * | 2016-09-23 | 2018-11-14 | 日本製紙株式会社 | Method for producing dissolved kraft pulp |
| CN109505178B (en) * | 2018-11-21 | 2021-08-17 | 湖南骏泰新材料科技有限责任公司 | Cooking method for preparing cellulose from agricultural and forestry residues |
| CN110983848A (en) * | 2019-11-06 | 2020-04-10 | 福建省青山纸业股份有限公司 | Preparation process of bamboo unbleached pulp |
| CN110904710A (en) * | 2019-11-06 | 2020-03-24 | 福建省青山纸业股份有限公司 | Bamboo pulp preparation process |
| CN114277598A (en) * | 2021-03-30 | 2022-04-05 | 赣南师范大学 | Preparation method of hollow and porous hybrid cells and bamboo dissolving pulp |
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| CN101368295A (en) * | 2008-09-19 | 2009-02-18 | 福建省南纸股份有限公司 | Preparation method for Chinese red pine dissolving pulp |
| CN101748630A (en) * | 2009-12-14 | 2010-06-23 | 昆明理工大学 | Acid-free pre-hydrolysis enzymolysis-free method for preparing bamboo pulp of Dendrocalamus giganteus Munro series |
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| CN101368295A (en) * | 2008-09-19 | 2009-02-18 | 福建省南纸股份有限公司 | Preparation method for Chinese red pine dissolving pulp |
| CN101748630A (en) * | 2009-12-14 | 2010-06-23 | 昆明理工大学 | Acid-free pre-hydrolysis enzymolysis-free method for preparing bamboo pulp of Dendrocalamus giganteus Munro series |
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