CN103266517B - Technology for pulping broussonetia papyrifera white barks by using phosphoric acid pretreatment and magnesiumsulfite process - Google Patents

Technology for pulping broussonetia papyrifera white barks by using phosphoric acid pretreatment and magnesiumsulfite process Download PDF

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CN103266517B
CN103266517B CN201310186697.1A CN201310186697A CN103266517B CN 103266517 B CN103266517 B CN 103266517B CN 201310186697 A CN201310186697 A CN 201310186697A CN 103266517 B CN103266517 B CN 103266517B
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raw material
distilled water
phosphoric acid
pulping
white
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CN103266517A (en
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何洁
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Kunming University of Science and Technology
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Abstract

The invention discloses a technology for pulping broussonetia papyrifera white barks by using phosphoric acid pretreatment and a magnesiumsulfite process. According to the technology, with broussonetia papyrifera white bark bast fiber as a raw material, the raw material is pretreated with (NaPO3)6 and phosphoric acid and then is processed through the magnesiumsulfite process. The broussonetia papyrifera white bark long fibered pulp prepared by using the technology has the characteristics of high whiteness and good strength, the pulping technology is mild in condition and the temperature of the overall process is lower than 100 DEG C.

Description

The phosphoric acid preliminary treatment magnesium sulfite process pulping technique of broussonetia white bast
Technical field
The invention belongs to the chemical pulping technical field of bast class raw material, particularly after the preliminary treatment of a kind of broussonetia white bast phosphoric acid, magnesium sulfite process pulping technique in a mild condition.
Background technology
Light leaf paper mulberry be Japan in recent years from wild paper mulberry a mutation of seed selection belong to Moraceae paper mulberry belong to, a kind of papermaking new raw material of seed selection in recent years, it is fast growing hard wood kind, easy to raise grows, a peeling to be cut every year and could promote that it constantly grows, its skin belongs to renewable resource, can cut down once every 2-3 annual ring, can utilize land resource preferably and can not destroy ecological environment.The full skin of light leaf paper mulberry accounts for 12% of full bar, and white skin accounts for 72% of full skin.White skin content of lignin is low, and fiber is elongated, pure white, can obtain the high-quality chemical pulp that quality is good, economic worth is high, is the raw material of papermaking fiber of high-quality.
If use existing the most frequently used pulping process, i.e. common soda pulping process and sulfite pulping, mostly carry out under high temperature (>=150 DEG C) high pressure, need specific high temperature resistant pressure vessel, pulping process cannot be carried out at ambient pressure.Although broussonetia white bast lignin content is very low, the content of its pectin is very high, reaches nearly 9%, therefore removes the process of pectin, namely a part for pulping process, thus the pulping process condition more relaxed can be used to reach the object of pulping.
Summary of the invention
The object of the invention is the phosphoric acid preliminary treatment magnesium sulfite process pulping technique providing a kind of broussonetia white bast, it is gentleer that the method has overall pulping process condition, slurrying maximum temperature not higher than 100 DEG C, and obtained bast fiber slurry to have magma whiteness higher, the good feature of intensity.
In pulping process of the present invention, be bast fiber raw material broussonetia white bast be raw material, adopt (NaPO 3) 6, H 3pO 4, (ortho acid, main component is Mg (HSO to the magnesium bisulfite cooking liquor that provides of MgO medicament and slurrying factory 3) 2, MgSO 3and a certain amount of MgO), carry out slurrying.
The phosphoric acid preliminary treatment magnesium sulfite process pulping technique of broussonetia white bast of the present invention, carries out according to following concrete steps, and wherein solid-liquid ratio is solid over dry material quality to the ratio of total liquor capacity:
(1) broussonetia white bast is cut into 3cm-5cm, the skin section of width 15mm-25mm, as chemical pulping raw material;
(2) step (1) raw materials treated is carried out rinsing and is boiled: add distilled water in the feed and make solid-liquid ratio (solid over dry material quality is to the ratio of total liquor capacity) be 1:6-1:10, boils 6min-10min and go out enzyme after at room temperature soaking 60min;
(3) the raw material distilled water after step (2) process washs 6 times, drains;
(4) raw material after step (3) washing is carried out phosphoric acid preliminary treatment: (the NaPO adding raw material absolute dry mass 0.4%-0.6% 3) 6and add distilled water and make solid-liquid ratio (solid over dry material quality is to the ratio of total liquor capacity) be 1:10-1:20, at room temperature soak 30min, then use phosphoric acid adjust ph to 1.5-2.0, at 85 DEG C-95 DEG C, 90min-120mim is incubated after stirring, make pectin in broussonetia white bast in diluted acid, change into water soluble pectin to be dissolved out, follow-up pectin extraction can be done and use;
(5) raw material that step (4) processed is washed with distilled water to pH=6.5-7.5;
(6) step (5) is washed the magnesium sulfite process process that rear raw material carries out temperate condition;
(7) slurry of the gained after step (6) process is washed with distilled water to pH=6.5-7.5;
(8) step (7) is washed disposed slurry and be placed in pulp screen, use sieve seam to be that the sieve plate of 0.40mm adds clear water and screens, be separated screening reject, namely obtain clean paper pulp.
According to the low permanganate number of final paper pulp and high viscosity requirement, the magnesium sulfite process treatment conditions of step (6) can regulate, above-mentioned steps (6) place according to solid-liquid ratio (ratio of solid over dry material quality and total liquor capacity) for 1:4-1:6 calculates required cooked solution volume, cooked solution total acid T.A. is the quality-percentage by volume of 1.0%-1.2%(relative to total liquor capacity as requested) calculate that required slurrying factory provides newly join magnesium bisulfite cooking liquor (i.e. ortho acid, slurrying factory provides, general total acid T.A. is higher, acid is less than or equal to 1 than F.A., T.A. and C.A. of ortho acid is by total SO 2, free SO 2measure and calculation), cooked solution combined acid C.A. is the quality-percentage by volume of 0.7%-0.9%(relative to total liquor capacity as requested again) calculate and determine MgO addition, finally add after distilled water mixes and add pretreated raw material, after feed liquid uniform stirring, at 85 DEG C-95 DEG C, be incubated 90min-120min.
Magnesium bisulfite raw aqueous acid required processing stage of sulfite hydrogen magnesium of the present invention is newly joined by slurrying factory to be provided, different slurrying factory provide all can, main adopt it to provide the self-produced SO of MgO absorbing emulsions for oneself 2obtain, its main component is all Mg (HSO 3) 2, MgSO 3and a certain amount of MgO, general total acid T.A. is higher, and acid is less than or equal to 1 than F.A.; T.A. and C.A. of ortho acid is by total SO 2, free SO 2measure and calculation; Other reagent, without specified otherwise, are commercially available conventional reagent, and the reagent such as calgon, phosphoric acid, magnesia of use is AR.
The present invention is relative to the advantage of prior art:
(1) the light leaf paper mulberry used is a kind of papermaking new raw material of seed selection in recent years, easily plants, and growth is fast, and will cut a peeling every year and could promote that it constantly grows, its skin belongs to renewable resource, can utilize land resource preferably and can not destroy ecological environment;
(2) broussonetia white bast content of lignin low (< 9%), fiber is pure white, and fibre length long (about average length 6.7mm), length-width ratio large (about 332) is the raw material of papermaking fiber of high-quality;
(3) rinsing and phosphoric acid preliminary treatment, first to make in broussonetia white bast pectolysis out, water-insoluble pectin in plant cell can be changed into water soluble pectin and be dissolved out by acid treatment in diluted acid, and the pectin solution be dissolved out can be expected to carry out pectin extraction further.Although the incomplete pulping of raw material after acid treatment, only rely on the subsequent treatment of condition milder, namely the magnesium sulfite process process of temperate condition, can obtain satisfactory paper pulp.And the composition of magnesium sulfite process pulping and digesting liquid mainly Mg (HSO 3) 2, MgSO 3.The pH value of cooking liquor is generally 3-6, and the effect adding MgO is used to regulate combined acid.Conventional magnesium sulfite process obtains magma, and just to have whiteness higher, the good feature of bleachability.In sulphite, the use of magnesium base makes it have the cheap of calcium salt base equally, and improves the problem that sodium base cooking waste liquor reclaims difficulty.And the magnesium sulfite process process re-used after the preliminary treatment of broussonetia white bast phosphoric acid, can use the process conditions more relaxed, reduce drug dosage, maximum temperature is reduced to less than 100 DEG C, and slurrying whole process can be carried out at ambient pressure.
In a word, novel material broussonetia white bast fiber quality is good, content of lignin is low, coordinate suitable phosphoric acid preliminary treatment magnesium sulfite process slurrying again, there are the potentiality preparing high-quality bast long fiber slurry, adopt the inventive method to make broussonetia white bast slurrying temperature not higher than 100 DEG C, and obtained magma whiteness is higher, intensity is better, and magma whiteness can reach 50%ISO-60%ISO, and viscosity can reach 1300-1400mL/g.
Detailed description of the invention
Below by embodiment the invention will be further described explanation, but scope is not limited to described content, in the present embodiment, method is conventional method if no special instructions, uses the reagent that reagent is conventional commercial reagent if no special instructions or prepares according to a conventional method; In embodiment, solid-liquid ratio is solid over dry material quality to the ratio of total liquor capacity, and total acid T.A. and combined acid C.A. is the quality-percentage by volume relative to total liquor capacity, T.A. and C.A. of ortho acid is by total SO 2, free SO 2measure and calculation.
Embodiment 1: the phosphoric acid preliminary treatment magnesium sulfite process pulping technique of this broussonetia white bast, particular content is as follows:
(1) be raw material with broussonetia white bast, be cut into length 3cm-5cm with chopper, the skin section of width 15mm-25mm;
(2) skin section is positioned in distilled water, makes solid-liquid ratio be 1:6, after at room temperature soaking 60min, boil 6min;
(3) with the raw material that distilled water washing step (2) processed, wash 6 times, drain;
(4) raw material after step (3) washing is carried out phosphoric acid preliminary treatment, in the raw material after draining, add (the NaPO of raw material absolute dry mass 0.4% 3) 6, and add distilled water and make solid-liquid ratio be 1:10, at room temperature first soak 30min after stirring, and then use phosphoric acid adjust ph to 1.5, after stirring, at 85 DEG C, be incubated 100mim;
(5) with the raw material that distilled water washing step (4) processed, wash to pH=6.5;
(6) step (5) is washed rear raw material and carry out magnesium sulfite process process, the ratio being 1:4 according to solid-liquid ratio calculates required liquor capacity, consumption (the i.e. ortho acid of cooked solution total acid T.A. magnesium bisulfite cooking liquor needed for 1.2% calculating as requested, slurrying factory provides, newly join, general total acid T.A. is higher, acid is less than or equal to 1 than F.A.), be 0.7% determine MgO addition by calculating according to combined acid C.A. again, finally add after distilled water mixes and add pretreated raw material, after feed liquid stirs, at 95 DEG C, be incubated 90min;
(7) with the slurry of the gained after distilled water washing step (6) process, wash to pH=7.5;
(8) step (7) is washed disposed slurry and be placed in pulp screen, use sieve seam to be that the sieve plate of 0.40mm adds clear water and screens, be separated screening reject, namely obtain clean paper pulp.
Result: paper pulp screened yield 54.2%, permanganate number 8.60, viscosity 1350mL/g, whiteness 54.3%ISO.
Embodiment 2: the magnesium sulfite process pulping technique of temperate condition after the phosphoric acid preliminary treatment of this broussonetia white bast, particular content is as follows:
(1) be raw material with broussonetia white bast, be cut into length 3cm-5cm with chopper, the skin section of width 15mm-25mm;
(2) skin section is positioned in distilled water, makes solid-liquid ratio be 1:8, after at room temperature soaking 60min, boil 8min;
(3) with the raw material that distilled water washing step (2) processed, wash 6 times, drain;
(4) raw material after step (3) washing is carried out phosphoric acid preliminary treatment, in the raw material after draining, add (the NaPO of raw material absolute dry mass 0.5% 3) 6, and add distilled water and make solid-liquid ratio 1:15, at room temperature first soak 30min after stirring, and then use phosphoric acid adjust ph to 2.0, after stirring, at 90 DEG C, be incubated 100mim;
(5) with the raw material that distilled water washing step (4) processed, wash to pH=7.0;
(6) step (5) is washed rear raw material and carry out magnesium sulfite process process, the ratio being 1:5 according to solid-liquid ratio calculates required liquor capacity, cooked solution total acid T.A. magnesium bisulfite cooking liquor (i.e. ortho acid needed for 1.2% calculating as requested, slurrying factory provides, newly join, general total acid T.A. is higher, acid is less than or equal to 1 than F.A.), be 0.8% determine MgO addition by calculating according to combined acid C.A. again, finally add after distilled water mixes and add pretreated raw material, after feed liquid stirs, at 85 DEG C, be incubated 120min;
(7) with the slurry of the gained after distilled water washing step (6) process, wash to pH=7.0;
(8) step (7) is washed disposed slurry and be placed in pulp screen, use sieve seam to be that the sieve plate of 0.40mm adds clear water and screens, be separated screening reject, namely obtain clean paper pulp.
Result: paper pulp screened yield 52.0%, permanganate number 7.65, viscosity 1320mL/g, whiteness 54.0%ISO.
Embodiment 3: the magnesium sulfite process pulping technique of temperate condition after the phosphoric acid preliminary treatment of this broussonetia white bast, particular content is as follows:
(1) be raw material with broussonetia white bast, be cut into length 3cm-5cm with chopper, the skin section of width 15mm-25mm;
(2) skin section is positioned in distilled water, makes solid-liquid ratio be 1:10, after at room temperature soaking 60min, boil 10min;
(3) with the raw material that distilled water washing step (2) processed, wash 6 times, drain;
(4) raw material after step (3) washing is carried out phosphoric acid preliminary treatment, in the raw material after draining, add (the NaPO of raw material absolute dry mass 0.6% 3) 6, and add distilled water and make solid-liquid ratio 1:20, at room temperature first soak 30min after stirring, and then use phosphoric acid adjust ph to 2.0, after stirring, at 95 DEG C, be incubated 90mim;
(5) with the raw material that distilled water washing step (4) processed, wash to pH=7.5;
(6) step (5) is washed rear raw material and carry out magnesium sulfite process process, the ratio being 1:6 according to solid-liquid ratio calculates required liquor capacity, cooked solution total acid T.A. magnesium bisulfite cooking liquor (i.e. ortho acid needed for 1.0% calculating as requested, slurrying factory provides, newly join, general total acid T.A. is higher, acid is less than or equal to 1 than F.A.), be 0.7% determine MgO addition by calculating according to combined acid C.A. again, finally add after distilled water mixes and add pretreated raw material, after feed liquid stirs, at 90 DEG C, be incubated 100min;
(7) with the slurry of the gained after distilled water washing step (6) process, wash to pH=7;
(8) step (7) is washed disposed slurry and be placed in pulp screen, use sieve seam to be that the sieve plate of 0.40mm adds clear water and screens, be separated screening reject, namely obtain clean paper pulp.
Result: paper pulp screened yield 52.3%, permanganate number 7.84, viscosity 1390mL/g, whiteness 58.2%ISO.
Embodiment 4: the magnesium sulfite process pulping technique of temperate condition after the phosphoric acid preliminary treatment of this broussonetia white bast, particular content is as follows:
(1) be raw material with broussonetia white bast, be cut into length 3cm-5cm with chopper, the skin section of width 15mm-25mm;
(2) skin section is positioned in distilled water, makes solid-liquid ratio 1:8, after at room temperature soaking 60min, boil 9min;
(3) with the raw material that distilled water washing step (2) processed, wash 6 times, drain;
(4) raw material after step (3) washing is carried out phosphoric acid preliminary treatment, in the raw material after draining, add (the NaPO of raw material absolute dry mass 0.5% 3) 6, and add distilled water and make solid-liquid ratio 1:12, at room temperature first soak 30min after stirring, and then use phosphoric acid adjust ph to 1.8, after stirring, at 85 DEG C, be incubated 120mim;
(5) with the raw material that distilled water washing step (4) processed, wash to pH=7.5;
(6) step (5) is washed rear raw material and carry out magnesium sulfite process process, the ratio being 1:5 according to solid-liquid ratio calculates required liquor capacity, cooked solution total acid T.A. magnesium bisulfite cooking liquor (i.e. ortho acid needed for 1.1% calculating as requested, slurrying factory provides, newly join, general total acid T.A. is higher, acid is less than or equal to 1 than F.A.), be 0.9% determine MgO addition by calculating according to combined acid C.A. again, finally add after distilled water mixes and add pretreated raw material, after feed liquid stirs, at 90 DEG C, be incubated 110min;
(7) with the slurry of the gained after distilled water washing step (6) process, wash to pH=6.5;
(8) step (7) is washed disposed slurry and be placed in pulp screen, use sieve seam to be that the sieve plate of 0.40mm adds clear water and screens, be separated screening reject, namely obtain clean paper pulp.
Result: paper pulp screened yield 52.6%, permanganate number 7.30, viscosity 1370mL/g, whiteness 53.8%ISO.

Claims (1)

1. a broussonetia white bast phosphoric acid preliminary treatment magnesium sulfite process pulping process, slurrying is carried out with broussonetia white bast raw material, it is characterized in that: first raw material carries out rinsing and boil, then phosphoric acid preliminary treatment is carried out to it, finally adopt the magnesium sulfite process of temperate condition to process obtained paper pulp to it;
The concrete pulping process step of said method is as follows:
(1) broussonetia white bast is cut into long 3cm-5cm, the skin section of width 15mm-25mm, as chemical pulping raw material;
(2) rinsing is boiled: be positioned over by raw material in distilled water, makes solid-liquid ratio be 1:6-1:10, boils 6min-10min after at room temperature soaking 60min;
(3) raw materials treated filtration washing, washs 6 times with distilled water, drains;
(4) phosphoric acid the preliminary treatment: (NaPO adding raw material absolute dry mass 0.4%-0.6% in the raw material after draining 3) 6, and add distilled water and make solid-liquid ratio be 1:10-1:20, use phosphoric acid adjust ph to 1.5-2.0 after at room temperature soaking 30min, after stirring, at 85 DEG C-95 DEG C, be incubated 90min-120mim;
(5) pretreated raw material is washed with distilled water to pH is 6.5-7.5;
(6) raw material after washing carries out the magnesium sulfite process process of temperate condition, and having processed rear paper pulp, to be washed with distilled water to pH be 6.5-7.5;
(7) after washing, gained slurry is placed in pulp screen, uses sieve seam to be that the sieve plate of 0.40mm adds clear water and screens, is separated screening reject, namely obtains clean paper pulp;
Wherein the process conditions of the magnesium sulfite process process of step (6) temperate condition are: be that 1:4-1:6 calculates required cooked solution volume according to solid-liquid ratio, the cooked solution total acid T.A. consumption of newly joining magnesium bisulfite cooking liquor that required slurrying factory provides for 1.0%-1.2% calculates as requested, cooked solution combined acid C.A. is that MgO addition is determined in 0.7%-0.9% calculating as requested again, finally add the raw material after adding washing after distilled water mixes, after feed liquid uniform stirring, at 85 DEG C-95 DEG C, be incubated 90min-120min.
CN201310186697.1A 2013-05-20 2013-05-20 Technology for pulping broussonetia papyrifera white barks by using phosphoric acid pretreatment and magnesiumsulfite process Expired - Fee Related CN103266517B (en)

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CN1124791A (en) * 1994-04-14 1996-06-19 武汉大学 Fast degumming aid for ramie and Broussonetia papyrifera bark and technique
CN101158127A (en) * 2007-11-01 2008-04-09 大连工业大学 Broussonetia white bast biological pulping method
KR101526267B1 (en) * 2008-11-28 2015-06-11 (주)아모레퍼시픽 Mask pack composed of the cosmetic cotton-like material produced from a paper mulberry

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