CN102493257A - Masson pine dissolving pulp and production method thereof - Google Patents
Masson pine dissolving pulp and production method thereof Download PDFInfo
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- CN102493257A CN102493257A CN2011104032370A CN201110403237A CN102493257A CN 102493257 A CN102493257 A CN 102493257A CN 2011104032370 A CN2011104032370 A CN 2011104032370A CN 201110403237 A CN201110403237 A CN 201110403237A CN 102493257 A CN102493257 A CN 102493257A
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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 masson 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 masson pine dissolving pulp.
Background technology
Common chemical pulping is the lignin of in pulping process, removing in the plant fiber material, keeps cellulose and hemicellulose as much as possible; Dissolving pulp then requires in pulping process, to remove lignin and hemicellulose, only keeps cellulose, and therefore, early stage dissolving pulp is to adopt the high cotton linter production of content of cellulose.Because socioeconomic fast development, living standards of the people improve constantly, and the consumption of resource also increases fast, and particularly the raw materials consumption of textile industry viscose glue, cellulose mystery and nitrated production field also increases fast.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 at present.Along with the growth of dissolving pulp demand, raw materials for production are main with timber at present, and domestic is the enterprise of raw material production cellulose viscose pulp with the bamboo in addition.
Patent CN101158121A discloses the technology of making dissolving pulp with ethanol, sulfate, acetate, and technology comprises blank, screening ash disposal in regular turn, washes material, ethanol extracting, sulphate cook, slurries separation, washing, purifying, chloridized, alkali treatment, acetate bleaching+H
2O
2The organic bleaching of oxidation, sour complexing are handled, are manufactured paper with pulp.Though production procedure can be effectively shortened in this invention; Improve the production efficiency of utilizing bamboo wood, timber, masson pine, ramulus mori, Chinese alpine rush etc. to produce confession weaving dissolving pulp, nitrated dissolving pulp, acetate dissolution slurry, the employed dissolving pulp in cellulose ether dissolving pulp field, improve the yield rate that bamboo wood, timber, masson pine, ramulus mori, Chinese alpine rush etc. are produced dissolving pulp simultaneously.
Patent CN1013682951A discloses a kind of preparation method of masson pine dissolving pulp, may further comprise the 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 the 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) copy slurry.
More than invention is adopted and is contained the elemental chlorine bleaching process, and waste water is difficult to handle, 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 masson 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 masson 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, and whiteness is not less than 89%, alpha cellulose is not less than 91%, pentosan is not higher than 3%, the dynamic viscosity value is that 9～25mPa.s, ash content are not higher than 0.1%, iron content is not higher than 15mgkg
-1
In order to obtain above-mentioned masson pine dissolving pulp, manufacturing approach of the present invention comprises following several 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; Charge into 135～145 ℃ cooking liquor; In the acidic materials that produce with prehydrolysis and wood chip carried out elementary boiling, the cooking liquor sulphidity that this step is used is 15%～30%, be 7%～10% of over dry wood chip weight with the effective alkali consumption of sodium oxide molybdena calculating;
(3) utilize 145～170 ℃ cooking liquor that the cooking liquor that step (2) adds is replaced at least one black liquor groove, the cooking liquor sulphidity that this step is used is 15%～30%, be 9%～12% of over dry wood chip weight with the effective alkali consumption of sodium oxide molybdena calculating;
(4) step (3) is added the cooking liquor heat temperature raising in the digester, reach 160～172 ℃ of temperature after, stopping to heat up gets into holding stage, treats that the H factor reaches at 900～1400 o'clock, accomplishes this step;
(5) with step (4) gained slurry, filter black liquor with pulp washing the cooking liquor that step (3) adds in the digester is replaced at least one black liquor groove, make the slurry temperature in the digester be lower than 100 ℃;
(6) with step (5) gained slurry, send in the 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 carries out D behind two sections oxygen delignifications
0Eo
PD
1D
2Bleaching;
(8) the bleaching disposed slurry washs dried and becomes the masson pine dissolving pulp.
Preferably, the process conditions of the said steam prehydrolysis of step (1) are: be warming up to 160～175 ℃ with steam at 25～40 min behind the masson pine chip filling, be incubated to the P-factor at 160～175 ℃ and reach 300～800.
Preferably, the said cooking liquor of step (3) is replaced at least one black liquor groove and is: the cooking liquor that is lower than 100 ℃ gets into the first black liquor groove, and the cooking liquor that is not less than 100 ℃ gets into the second black liquor groove.
Preferably, the said cooking liquor of step (5) is replaced at least one black liquor groove and is: be not less than 160 ℃ entering the 3rd black liquor groove, 140～160 ℃ entering the 4th black liquor groove, be lower than 140 ℃ entering the 5th black liquor groove or the said second black liquor groove.
Preferably, said 135～145 ℃ cooking liquor of step (2) is the interior black liquor of the second black liquor groove and/or the 5th black liquor groove and the mixed liquor of alkali lye, and said alkali lye is the causticization alkali that obtains in commercially available alkali or the alkali recovery process.
Preferably, said 145～170 ℃ cooking liquor of step (3) is the interior black liquor of the 3rd black liquor groove and/or the 4th black liquor groove and the mixed liquor of alkali lye, and said alkali lye is the causticization alkali that obtains in commercially available alkali or the alkali recovery process.
Preferably, the said two sections oxygen delignifications of step (7), first section oxygen delignification process conditions 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 behind one section oxygen delignification does not wash, and then carries out second section oxygen delignification, and second section oxygen delignification condition is: oxygen pressure 1.0 ~ 1.5 MPa, 95～100 ℃ of oxygen delignification temperature, times 40～60 min.
Preferably, the said 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 make bleaching endpoint pH≤2.6 with the sulfuric acid adjusting; 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, use sulfuric acid to regulate making the bleaching endpoint pH 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, use sulfuric acid or NaOH to regulate making the bleaching endpoint pH 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 of 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 handle; Little to ambient influnence, the products obtained therefrom quality is easy to control, can satisfies QUALITY STANDARD and customer requirements well; Can reclaim the energy in the digestion process, energy consumption is lower.Because of adopting ClO 2 bleaching, effectively reduce in the slurry 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 behind the digester, is warming up to 160 ℃ with steam at 25min, carries out steam prehydrolysis, under maximum temperature, is incubated to the prehydrolysis P-factor to reach 400.Through the post-job wood chip of prehydrolysis in digester; Charge into 135～145 ℃ cooking liquor; In the acidic materials that produce with prehydrolysis and wood chip carried out elementary boiling; The used cooking liquor of this step is stated the black liquor and the mixed liquor of commercially available alkali and akali sulphide in the 5th black liquor groove after being, sulphidity is 15%, be 7% of over dry wood chip weight with the effective alkali consumption of sodium oxide molybdena calculating.Cooking liquor in the wood chip after utilizing 145～170 ℃ cooking liquor with elementary cooking operation cements out; The cooking liquor that is lower than 100 ℃ gets into the first black liquor groove; The cooking liquor that is not less than 100 ℃ gets into the second black liquor groove; The cooking liquor that this step is used for after state the black liquor of the 3rd black liquor groove and the mixed liquor of commercially available alkali, akali sulphide, sulphidity is 30%, be 12% of over dry wood chip weight with the effective alkali consumption of sodium oxide molybdena calculating.To the cooking liquor heat temperature raising in the digester; After reaching 172 ℃ of temperature; Stopping to heat up gets into holding stage, treats that the H factor reaches at 1300 o'clock, and the cooking liquor that will add in the digester with pulp washing filtration black liquor cements out; Make the slurry temperature in the digester be lower than 100 ℃, be not less than 160 ℃ entering the 3rd black liquor groove, 140 ℃～160 ℃ entering the 4th black liquor groove and be lower than 140 ℃ entering the 5th black liquor groove or the second black liquor groove.After accomplishing, boiling, sends in the spraying pot, through black liquid extraction, obtain masson pine prehydrolysis natural color pulp by screening the gained slurry.Gained masson pine prehydrolysis natural color pulp is through two sections oxygen delignification, and first section oxygen delignification process conditions 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 behind one section oxygen delignification does not wash, and then carries out second section oxygen delignification, and second section 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 an absolute dried paper pulp weight, bleached pulp concentration 12%, and time 40min, 75 ℃ of bleaching temperatures, use sulfuric acid to regulate making the bleaching endpoint pH is 2.3; E
OPThe process conditions of section are: the NaOH consumption is 2% of an absolute dried paper pulp weight, H
2O
2Consumption is 1% of an 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 an absolute dried paper pulp weight, bleached pulp concentration 8%, and time 120min, 75 ℃ of bleaching temperatures, use sulfuric acid to regulate making the bleaching endpoint pH is 4; D
2The process conditions of section are: ClO
2Consumption is 0.2% of an absolute dried paper pulp weight, bleached pulp concentration 8%, and time 60min, 60 ℃ of bleaching temperatures, use sulfuric acid or NaOH to regulate making the bleaching endpoint pH is 5.
Embodiment 2:
The pinus massoniana sheet is packed into behind the digester, is warming up to 175 ℃ with steam at 40min, carries out steam prehydrolysis, under maximum temperature, is incubated to the prehydrolysis P-factor to reach 650.Through the post-job wood chip of prehydrolysis in digester; Charge into 135～145 ℃ cooking liquor; In the acidic materials that produce with prehydrolysis and wood chip carried out elementary boiling; The used cooking liquor of this step is stated the mixed liquor of the causticization alkali that obtains in black liquor and the alkali recovery process in the 5th black liquor groove after being, sulphidity is 30%, be 10% of over dry wood chip weight with the effective alkali consumption of sodium oxide molybdena calculating.Cooking liquor in the wood chip after utilizing 145～160 ℃ cooking liquor with elementary cooking operation cements out; The cooking liquor that is lower than 100 ℃ gets into the first black liquor groove; The cooking liquor that is not less than 100 ℃ gets into the second black liquor groove; The cooking liquor that this step is used for after state the black liquor of the 3rd black liquor groove and the mixed liquor of commercially available alkali, akali sulphide, sulphidity is 15%, be 9% of over dry wood chip weight with the effective alkali consumption of sodium oxide molybdena calculating.To the cooking liquor heat temperature raising in the digester; After reaching 160 ℃ of temperature; Stopping to heat up gets into holding stage, treats that the H factor reaches at 1400 o'clock, and the cooking liquor that will add in the digester with pulp washing filtration black liquor cements out; Make the slurry temperature in the digester be lower than 100 ℃, be not less than 160 ℃ entering the 3rd black liquor groove, 140 ℃～160 ℃ entering the 4th black liquor groove and be lower than 140 ℃ entering the 5th black liquor groove or the second black liquor groove.After accomplishing, boiling, sends in the spraying pot, through black liquid extraction, obtain masson pine prehydrolysis natural color pulp by screening the gained slurry.Gained masson pine prehydrolysis natural color pulp is through two sections oxygen delignification, and first section oxygen delignification process conditions 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 behind one section oxygen delignification does not wash, and then carries out second section oxygen delignification, and second section 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 an absolute dried paper pulp weight, bleached pulp concentration 8%, and time 40min, 60 ℃ of temperature, use sulfuric acid to regulate making the bleaching endpoint pH is 2.4; E
OPThe process conditions of section are: the NaOH consumption is 1% of an absolute dried paper pulp weight, H
2O
2Consumption is 0.5% of an 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 an absolute dried paper pulp weight, bleached pulp concentration 12%, and time 150min, 60 ℃ of temperature, use sulfuric acid to regulate making the bleaching endpoint pH is 5; D
2The process conditions of section are: ClO
2Consumption is 0.5% of an absolute dried paper pulp weight, bleached pulp concentration 12%, and time 100min, 75 ℃ of temperature, use sulfuric acid or NaOH to regulate making the bleaching endpoint pH is 4.
Embodiment 3:
The pinus massoniana sheet is packed into behind the digester, is warming up to 170 ℃ with steam at 35min, carries out steam prehydrolysis, under maximum temperature, is incubated to the prehydrolysis P-factor to reach 500.Through the post-job wood chip of prehydrolysis in digester; Charge into 135～145 ℃ cooking liquor; In the acidic materials that produce with prehydrolysis and wood chip carried out elementary boiling; The used cooking liquor of this step is stated the mixed liquor of the causticization alkali that obtains in black liquor and the alkali recovery process in the second black liquor groove after being, sulphidity is 22%, be 8% of over dry wood chip weight with the effective alkali consumption of sodium oxide molybdena calculating.Cooking liquor in the wood chip after utilizing 145～168 ℃ cooking liquor with elementary cooking operation cements out; The cooking liquor that is lower than 100 ℃ gets into the first black liquor groove; The cooking liquor that is not less than 100 ℃ gets into the second black liquor groove; The cooking liquor that this step is used for after state the 4th black liquor groove black liquor and alkali recovery process in the mixed liquor of the causticization alkali that obtains, sulphidity is 23%, be 11% of over dry wood chip weight with the effective alkali consumption of sodium oxide molybdena calculating.To the cooking liquor heat temperature raising in the digester; After reaching 168 ℃ of temperature; Stopping to heat up gets into holding stage, treats that the H factor reaches at 1350 o'clock, and the cooking liquor that will add in the digester with pulp washing filtration black liquor cements out; Make the slurry temperature in the digester be lower than 100 ℃, be not less than 160 ℃ entering the 3rd black liquor groove, 140 ℃～160 ℃ entering the 4th black liquor groove and be lower than 140 ℃ entering the 5th black liquor groove or the second black liquor groove.After accomplishing, boiling, sends in the spraying pot, through black liquid extraction, obtain masson pine prehydrolysis natural color pulp by screening the gained slurry.Gained masson pine prehydrolysis natural color pulp is through two sections oxygen delignification, and the process conditions of first section 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 behind one section oxygen delignification then carries out second section oxygen delignification without washing, and second section 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 an absolute dried paper pulp weight, bleached pulp concentration 10%, and time 50min, 70 ℃ of temperature, use sulfuric acid to regulate making the bleaching endpoint pH is 2.5; E
OPThe process conditions of section are: the NaOH consumption is 1.5% of an absolute dried paper pulp weight, H
2O
2Consumption is 0.7% of an 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 an absolute dried paper pulp weight, bleached pulp concentration 10%, and time 135min, 68 ℃ of temperature, use sulfuric acid to regulate making the bleaching endpoint pH is 4.5; D
2The process conditions of section are: ClO
2Consumption is 0.35% of an absolute dried paper pulp weight, bleached pulp concentration 10%, and time 80min, 70 ℃ of temperature, use sulfuric acid or NaOH to regulate making the bleaching endpoint pH is 4.5.
Embodiment 4:
The pinus massoniana sheet is packed into behind the digester, is warming up to 168 ℃ with steam at 30min, carries out steam prehydrolysis, under maximum temperature, is incubated to the prehydrolysis P-factor to reach 300.Through the post-job wood chip of prehydrolysis in digester; Charge into 135～145 ℃ cooking liquor; In the acidic materials that produce with prehydrolysis and wood chip carried out elementary boiling; The used cooking liquor of this step is stated the mixed liquor of the causticization alkali that obtains in black liquor and the alkali recovery process in the second black liquor groove and the 5th black liquor groove after being, sulphidity is 25%, be 8% of over dry wood chip weight with the effective alkali consumption of sodium oxide molybdena calculating.Cooking liquor in the wood chip after utilizing 145～170 ℃ cooking liquor with elementary cooking operation cements out; The cooking liquor that is lower than 100 ℃ gets into the first black liquor groove; The cooking liquor that is not less than 100 ℃ gets into the second black liquor groove; The cooking liquor that this step is used for after state the 3rd black liquor groove and the 4th black liquor groove black liquor and alkali recovery process in the mixed liquor of the causticization alkali that obtains, sulphidity is 24%, be 11% of over dry wood chip weight with the effective alkali consumption of sodium oxide molybdena calculating.To the cooking liquor heat temperature raising in the digester; After reaching 167 ℃ of temperature; Stopping to heat up gets into holding stage, treats that the H factor reaches at 900 o'clock, and the cooking liquor that will add in the digester with pulp washing filtration black liquor cements out; Make the slurry temperature in the digester be lower than 100 ℃, be not less than 160 ℃ entering the 3rd black liquor groove, 140 ℃～160 ℃ entering the 4th black liquor groove and be lower than 140 ℃ entering the 5th black liquor groove or the second black liquor groove.After accomplishing, boiling, sends in the spraying pot, through black liquid extraction, obtain masson pine prehydrolysis natural color pulp by screening the gained slurry.Gained masson pine prehydrolysis natural color pulp is through two sections oxygen delignification, and the process conditions of first section 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 behind one section oxygen delignification does not wash, and then carries out second section oxygen delignification, and the process conditions of second section 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 an absolute dried paper pulp weight, bleached pulp concentration 11.5%, and time 55min, 70 ℃ of temperature, use sulfuric acid to regulate making the bleaching endpoint pH is 2.6; E
OPThe process conditions of section are: the NaOH consumption is 1.4% of an absolute dried paper pulp weight, H
2O
2Consumption is 0.7% of an 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 an absolute dried paper pulp weight, bleached pulp concentration 11.7%, and time 140min, 72 ℃ of temperature, use sulfuric acid to regulate making the bleaching endpoint pH is 4.5; D
2The process conditions of section are: ClO
2Consumption is 0.29% of an absolute dried paper pulp weight, bleached pulp concentration 10.5%, and time 85min, 72 ℃ of temperature, use sulfuric acid or NaOH to regulate making the bleaching endpoint pH is 4.7.
Embodiment 5:
The pinus massoniana sheet is packed into behind the digester, is warming up to 173 ℃ with steam at 35min, carries out steam prehydrolysis, under maximum temperature, is incubated to the prehydrolysis P-factor to reach 800.Through the post-job wood chip of prehydrolysis in digester; Charge into 135～145 cooking liquor; In the acidic materials that produce with prehydrolysis and wood chip carried out elementary boiling; The used cooking liquor of this step is stated the mixed liquor of the causticization alkali that obtains in black liquor and the alkali recovery process in the second black liquor groove and the 5th black liquor groove after being, sulphidity is 27%, be 8.5% of over dry wood chip weight with the effective alkali consumption of sodium oxide molybdena calculating.Cooking liquor in the wood chip after utilizing 145～165 ℃ cooking liquor with elementary cooking operation cements out; The cooking liquor that is lower than 100 ℃ gets into the first black liquor groove; The cooking liquor that is not less than 100 ℃ gets into the second black liquor groove; The cooking liquor that this step is used for after state the 3rd black liquor groove and the 4th black liquor groove black liquor and alkali recovery process in the mixed liquor of the causticization alkali that obtains, sulphidity is 22%, be 10% of over dry wood chip weight with the effective alkali consumption of sodium oxide molybdena calculating.To the cooking liquor heat temperature raising in the digester; After reaching 168 ℃ of temperature; Stopping to heat up gets into holding stage, treats that the H factor reaches at 1400 o'clock, and the cooking liquor that will add in the digester with pulp washing filtration black liquor cements out; Make the slurry temperature in the digester be lower than 100 ℃, be not less than 160 ℃ entering the 3rd black liquor groove, 140 ℃～160 ℃ entering the 4th black liquor groove and be lower than 140 ℃ entering the 5th black liquor groove or the second black liquor groove.After accomplishing, boiling, sends in the spraying pot, through black liquid extraction, obtain masson pine prehydrolysis natural color pulp by screening the gained slurry.Gained masson pine prehydrolysis natural color pulp is through two sections oxygen delignification, and the process conditions of first section 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 behind one section oxygen delignification does not wash, and then carries out second section oxygen delignification, and the process conditions of second section 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 an absolute dried paper pulp weight, bleached pulp concentration 10.7%, and time 55min, 70 ℃ of temperature, use sulfuric acid to regulate making the bleaching endpoint pH is 2.5; E
OPThe process conditions of section are: the NaOH consumption is 1.2% of an absolute dried paper pulp weight, H
2O
2Consumption is 0.6% of an 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 an absolute dried paper pulp weight, bleached pulp concentration 11%, and time 130min, 69 ℃ of temperature, use sulfuric acid to regulate making the bleaching endpoint pH is 4.6; D
2The process conditions of section are: ClO
2Consumption is 0.26% of an absolute dried paper pulp weight, bleached pulp concentration 11.8, and time 92min, 67 ℃ of temperature, use sulfuric acid or NaOH to regulate making the bleaching endpoint pH is 4.5.
The part process of the foregoing description and test data is following 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 the 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 |
Among the present invention, the analysis of used soup and product quality is all undertaken by national standard method, " pulping chemistry " that definite method of the P factor is please write with reference to Chen Jiaxiang, and light industry in June nineteen ninety publishing house publishes, and the content that the 232-236 page or leaf is disclosed is confirmed.
Obviously, the invention is not restricted to above preferred implementation, also can in spirit of the present invention, change other process conditions, have same effect, so 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 (9)
1. masson pine dissolving pulp is characterized in that: by the masson pine wood chip through steam prehydrolysis, kraft cooking, two sections oxygen delignifications, D
0Eo
PD
1D
2Bleaching and making, whiteness is not less than 89%, alpha cellulose is not less than 91%, pentosan is not higher than 3%, the dynamic viscosity value is that 9～25mPa.s, ash content are not higher than 0.1%, iron content is not higher than 15mgkg
-1
2. the production method of the said masson pine dissolving pulp of claim 1 is characterized in that, may further comprise the 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; Charge into 135～145 ℃ cooking liquor; In the acidic materials that produce with prehydrolysis and wood chip carried out elementary boiling, the cooking liquor sulphidity that this step is used is 15%～30%, be 7%～10% of over dry wood chip weight with the effective alkali consumption of sodium oxide molybdena calculating;
(3) utilize 145～170 ℃ cooking liquor that the cooking liquor that step (2) adds is replaced at least one black liquor groove, the cooking liquor sulphidity that this step is used is 15%～30%, be 9%～12% of over dry wood chip weight with the effective alkali consumption of sodium oxide molybdena calculating;
(4) step (3) is added the cooking liquor heat temperature raising in the digester, reach 160～172 ℃ of temperature after, stopping to heat up gets into holding stage, treats that the H factor reaches at 900～1400 o'clock, accomplishes this step;
(5) with step (4) gained slurry, filter black liquor with pulp washing the cooking liquor that step (3) adds in the digester is replaced at least one black liquor groove, make the slurry temperature in the digester be lower than 100 ℃;
(6) with step (5) gained slurry, send in the 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 carries out D behind two sections oxygen delignifications
0Eo
PD
1D
2Bleaching;
(8) the bleaching disposed slurry washs dried and becomes the masson pine dissolving pulp.
3. according to the production method of the said masson pine dissolving pulp of claim 2; It is characterized in that: the process conditions of the said steam prehydrolysis of step (1) are: be warming up to 160～175 ℃ with steam at 25～40min behind the masson pine chip filling, be incubated to the P-factor at 160～175 ℃ and reach 300～800.
4. according to the production method of the said masson pine dissolving pulp of claim 2; It is characterized in that: the said cooking liquor of step (3) is replaced at least one black liquor groove and is: the cooking liquor that is lower than 100 ℃ gets into the first black liquor groove, and the cooking liquor that is not less than 100 ℃ gets into the second black liquor groove.
5. according to the production method of the said masson pine dissolving pulp of claim 2, it is characterized in that: the said cooking liquor of step (5) is replaced at least one black liquor groove and is: be not less than 160 ℃ entering the 3rd black liquor groove, 140～160 ℃ entering the 4th black liquor groove, be lower than 140 ℃ entering the 5th black liquor groove or the said second black liquor groove.
6. according to the production method of the said masson pine dissolving pulp of claim 2; It is characterized in that: said 135～145 ℃ cooking liquor of step (2) is the interior black liquor of the second black liquor groove and/or the 5th black liquor groove and the mixed liquor of alkali lye, and said alkali lye is the causticization alkali that obtains in commercially available alkali or the alkali recovery process.
7. according to the production method of the said masson pine dissolving pulp of claim 2; It is characterized in that: said 145～170 ℃ cooking liquor of step (3) is the interior black liquor of the 3rd black liquor groove and/or the 4th black liquor groove and the mixed liquor of alkali lye, and said alkali lye is the causticization alkali that obtains in commercially available alkali or the alkali recovery process.
8. according to the production method of the said masson pine dissolving pulp of claim 2, it is characterized in that: the said two sections oxygen delignifications of step (7), first section oxygen delignification process conditions 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 behind one section oxygen delignification does not wash, and then carries out second section oxygen delignification, and second section oxygen delignification condition is: oxygen pressure 1.0～1.5MPa, 95～100 ℃ of oxygen delignification temperature, times 40～60 min.
9. according to the production method of the said masson pine dissolving pulp of claim 2, it is characterized in that: the said 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 make bleaching endpoint pH≤2.6 with the sulfuric acid adjusting; 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, use sulfuric acid to regulate making the bleaching endpoint pH 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, use sulfuric acid or NaOH to regulate making the bleaching endpoint pH is 4～5.
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| CN102888772A (en) * | 2012-10-17 | 2013-01-23 | 四川永丰纸业股份有限公司 | Method for preparing bamboo pulp by replacing cooking sulfate with steaming sulfate |
| JP2014001470A (en) * | 2012-06-15 | 2014-01-09 | Nippon Paper Industries Co Ltd | Manufacturing method for dissolving kraft pulp |
| JP2016211142A (en) * | 2016-09-23 | 2016-12-15 | 日本製紙株式会社 | Manufacturing method of dissolved kraft pulp |
| CN109505178A (en) * | 2018-11-21 | 2019-03-22 | 湖南骏泰新材料科技有限责任公司 | A kind of agricultural three remain the boiling method that object prepares cellulose |
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| 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 |
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| EP3673110A4 (en) * | 2017-08-25 | 2021-05-12 | Valmet AB | Improved compact process for producing prehydrolyzed pulp |
| CN109505178A (en) * | 2018-11-21 | 2019-03-22 | 湖南骏泰新材料科技有限责任公司 | A kind of agricultural three remain the boiling method that object prepares cellulose |
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| 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 |
| 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 |
| 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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Address after: 418005 Huaihua Industrial Park, Hunan, Huaihua Patentee after: Hunan Jun Thai New Materials Technology Co. Ltd. Patentee after: Changsha University of Sciences and Technology Address before: 418005 Huaihua Industrial Park, Hunan, Huaihua Patentee before: Hu'nan Juntai Pulp Paper Co., Ltd. Patentee before: Changsha University of Sciences and Technology |