CN103266517A - 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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CN103266517A
CN103266517A CN2013101866971A CN201310186697A CN103266517A CN 103266517 A CN103266517 A CN 103266517A CN 2013101866971 A CN2013101866971 A CN 2013101866971A CN 201310186697 A CN201310186697 A CN 201310186697A CN 103266517 A CN103266517 A CN 103266517A
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raw material
distilled water
phosphoric acid
broussonetia
acid
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CN103266517B (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, the magnesium sulfite process pulping technique under temperate condition.
Background technology
Light leaf paper mulberry be Japan in recent years from wild paper mulberry seed selection mutation belong to the Moraceae paper mulberry and belong to, a kind of papermaking new raw material of seed selection in recent years, system's speed is given birth to the broad-leaved assortment, the easy to raise growth, a peeling to be cut every year and its continuous growth could be promoted, its skin belongs to renewable resource, can cut down once every the 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 make 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, namely common soda pulping process and sulfite pulping mostly carry out under high temperature (〉=150 ℃) high pressure, need specific high temperature resistant pressure vessel, can't carry out pulping process under normal pressure.Though the broussonetia white bast lignin content is very low, the content of its pectin is very high, has reached nearly 9%, therefore removes the process of pectin, the part of pulping process just, thus can use the pulping process condition that more relaxes to reach the purpose of pulping.
Summary of the invention
The object of the invention is to provide a kind of phosphoric acid preliminary treatment magnesium sulfite process pulping technique of broussonetia white bast, it is gentle that this method has overall pulping process condition, the slurrying maximum temperature is not higher than 100 ℃, and the bast fiber that makes slurry to have a former pulp brightness higher, intensity is characteristics preferably.
In the pulping process of the present invention, be that bast fiber raw material broussonetia white bast is raw material, adopt (NaPO 3) 6, H 3PO 4, (ortho acid, main component are 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 raw 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 is as the chemical pulping raw material;
(2) step (1) raw materials treated is carried out rinsing and boiled: adding distilled water in raw material, to make solid-liquid ratio (solid over dry raw material quality is to the ratio of total liquor capacity) be 1:6-1:10, at room temperature soaks and boil the 6min-10min enzyme that goes out behind the 60min;
(3) raw material after step (2) is handled drains with distilled water washing 6 times;
(4) step (3) washing back raw material is carried out the phosphoric acid preliminary treatment: (the NaPO that adds raw material over dry quality 0.4%-0.6% 3) 6And adding distilled water, to make solid-liquid ratio (solid over dry raw material quality is to the ratio of total liquor capacity) be 1:10-1:20, at room temperature soak 30min, use the phosphorus acid for adjusting pH value to 1.5-2.0 then, back insulation 90min-120mim under 85 ℃-95 ℃ stirs, make in the broussonetia white bast pectin in diluted acid, change into water soluble pectin and be dissolved out, can make follow-up pectin and extract and use;
(5) raw material handled of step (4) is washed with distilled water to pH=6.5-7.5;
(6) step (5) is washed the magnesium sulfite process processing that the back raw material carries out temperate condition;
The slurry of the gained after (7) step (6) is handled is washed with distilled water to pH=6.5-7.5;
(8) step (7) is washed disposed slurry and place pulp screen, use sieve seam to add clear water as the sieve plate of 0.40mm and screen, separate 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 be regulated, above-mentioned steps (6) is located to calculate required cooked solution volume according to solid-liquid ratio (ratio of solid over dry raw material quality and total liquor capacity) for 1:4-1:6, cooked solution total acid T.A. is that 1.0%-1.2%(is with respect to the quality-percentage by volume of total liquor capacity as requested) the magnesium bisulfite cooking liquor of newly joining that calculates required slurrying factory and provide (is ortho acid, slurrying factory provides, general total acid T.A. is higher, and acid is less than or equal to 1 than F.A.; The T.A. of ortho acid and C.A. can pass through total SO 2, free SO 2Mensuration calculate), cooked solution combined acid C.A. is that 0.7%-0.9%(is with respect to the quality-percentage by volume of total liquor capacity as requested again) calculate and determine the MgO addition, add distilled water at last and mix the pretreated raw material of back adding, feed liquid evenly stirs the back and is incubated 90min-120min down at 85 ℃-95 ℃.
Among the present invention magnesium bisulfite the processing stage the required former acid solution of magnesium bisulfite newly joined by slurrying factory and provide, different slurrying factory provide all can, mainly adopt it to provide the MgO emulsion for oneself and absorb self-produced SO 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.; The T.A. of ortho acid and C.A. can pass through total SO 2, free SO 2Mensuration calculate; Other reagent do not have specified otherwise, are commercially available conventional reagent, and reagent such as the calgon that uses, phosphoric acid, magnesia are AR.
The present invention is with respect to the advantage of prior art:
(1) the light leaf paper mulberry of Shi Yonging is a kind of papermaking new raw material of seed selection in recent years, easily plantation, and growth is fast, will cut a peeling every year and could promote its continuous growth, and 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), and length-width ratio big (about 332) is the raw material of papermaking fiber of high-quality;
(3) rinsing and phosphoric acid preliminary treatment, make at first that pectolysis comes out in the broussonetia white bast, acid treatment can change into the water-insoluble pectin in the plant cell water soluble pectin and be dissolved out in diluted acid, the pectin solution that is dissolved out can be expected further to carry out pectin and be extracted.Though raw material complete pulping after the acid treatment only relies on the subsequent treatment of condition milder, namely the magnesium sulfite process of temperate condition is handled, and can obtain satisfactory paper pulp.And the composition of magnesium sulfite process pulping and digesting soup mainly is Mg (HSO 3) 2, MgSO 3The pH value of cooking liquor is generally 3-6, and the effect that adds MgO is to regulate combined acid.Conventional magnesium sulfite process makes magma, and just to have whiteness higher, and bleachability is characteristics preferably.The use of magnesium base makes it have the cheap of calcium salt base equally in the sulphite, and has improved the sodium base cooking waste liquor and reclaimed difficult problem.And the magnesium sulfite process that re-uses after the preliminary treatment of broussonetia white bast phosphoric acid is handled, and can use the process conditions that more relax, and reduces drug dosage, and maximum temperature is reduced to below 100 ℃, and slurrying whole process can be carried out under normal pressure.
In a word, novel material broussonetia white bast fiber quality is good, content of lignin is low, cooperate suitable phosphoric acid preliminary treatment magnesium sulfite process slurrying again, have the potentiality of preparation high-quality bast long fiber slurry, adopt the inventive method to make broussonetia white bast slurrying temperature not be higher than 100 ℃, and the former pulp brightness that makes is higher, intensity is better, and former pulp brightness can reach 50%ISO-60%ISO, and viscosity can reach 1300-1400mL/g.
The specific embodiment
Be further described explanation below by the present invention of embodiment, but protection domain of the present invention is not limited to described content, method is conventional method if no special instructions in the present embodiment, the reagent that uses reagent to be conventional commercial reagent if no special instructions or to prepare according to a conventional method; Solid-liquid ratio is solid over dry raw material quality to the ratio of total liquor capacity among the embodiment, and total acid T.A. and combined acid C.A. are the quality-percentage by volume with respect to total liquor capacity, and the T.A. of ortho acid and C.A. can pass through total SO 2, free SO 2Mensuration calculate.
Embodiment 1: the phosphoric acid preliminary treatment magnesium sulfite process pulping technique of this broussonetia white bast, and particular content is as follows:
(1) is raw material with the broussonetia white bast, is cut into length 3cm-5cm with chopper, the skin section of width 15mm-25mm;
(2) the skin section is positioned in the distilled water, making solid-liquid ratio is 1:6, boils 6min after at room temperature soaking 60min;
(3) raw material of handling with distilled water washing step (2) washs 6 times, drains;
(4) step (3) washing back raw material is carried out the phosphoric acid preliminary treatment, add (the NaPO of raw material over dry quality 0.4% in the raw material after draining 3) 6, and adding distilled water, to make solid-liquid ratio be 1:10, at room temperature soaks 30min after stirring earlier, and then use phosphorus acid for adjusting pH value to 1.5, the back that stirs is at 85 ℃ of insulation 100mim down;
(5) raw material of handling with distilled water washing step (4) washs to pH=6.5;
(6) step (5) is washed the back raw material and carry out the magnesium sulfite process processing, be that the proportional meter of 1:4 is calculated required liquor capacity according to solid-liquid ratio, cooked solution total acid T.A. is that 1.2% consumption that calculates required magnesium bisulfite cooking liquor (is ortho acid 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% by calculate determining the MgO addition according to combined acid C.A. again, add distilled water at last and mix the pretreated raw material of back adding, be incubated 90min down at 95 ℃ after feed liquid stirs;
(7) with the slurry of the gained after distilled water washing step (6) processing, wash to pH=7.5;
(8) step (7) is washed disposed slurry and place pulp screen, use sieve seam to add clear water as the sieve plate of 0.40mm and screen, separate 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, and particular content is as follows:
(1) is raw material with the broussonetia white bast, is cut into length 3cm-5cm with chopper, the skin section of width 15mm-25mm;
(2) the skin section is positioned in the distilled water, making solid-liquid ratio is 1:8, boils 8min after at room temperature soaking 60min;
(3) raw material of handling with distilled water washing step (2) washs 6 times, drains;
(4) step (3) washing back raw material is carried out the phosphoric acid preliminary treatment, add (the NaPO of raw material over dry quality 0.5% in the raw material after draining 3) 6, and add distilled water and make solid-liquid ratio 1:15, at room temperature to soak 30min after stirring earlier, and then use phosphorus acid for adjusting pH value to 2.0, the back that stirs is at 90 ℃ of insulation 100mim down;
(5) raw material of handling with distilled water washing step (4) washs to pH=7.0;
(6) step (5) is washed the back raw material and carry out the magnesium sulfite process processing, be that the proportional meter of 1:5 is calculated required liquor capacity according to solid-liquid ratio, cooked solution total acid T.A. is that the required magnesium bisulfite cooking liquor of 1.2% calculating (is ortho acid 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% by calculate determining the MgO addition according to combined acid C.A. again, add distilled water at last and mix the pretreated raw material of back adding, be incubated 120min down at 85 ℃ after feed liquid stirs;
(7) with the slurry of the gained after distilled water washing step (6) processing, wash to pH=7.0;
(8) step (7) is washed disposed slurry and place pulp screen, use sieve seam to add clear water as the sieve plate of 0.40mm and screen, separate 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, and particular content is as follows:
(1) is raw material with the broussonetia white bast, is cut into length 3cm-5cm with chopper, the skin section of width 15mm-25mm;
(2) the skin section is positioned in the distilled water, making solid-liquid ratio is 1:10, boils 10min after at room temperature soaking 60min;
(3) raw material of handling with distilled water washing step (2) washs 6 times, drains;
(4) step (3) washing back raw material is carried out the phosphoric acid preliminary treatment, add (the NaPO of raw material over dry quality 0.6% in the raw material after draining 3) 6, and add distilled water and make solid-liquid ratio 1:20, at room temperature to soak 30min after stirring earlier, and then use phosphorus acid for adjusting pH value to 2.0, the back that stirs is at 95 ℃ of insulation 90mim down;
(5) raw material of handling with distilled water washing step (4) washs to pH=7.5;
(6) step (5) is washed the back raw material and carry out the magnesium sulfite process processing, be that the proportional meter of 1:6 is calculated required liquor capacity according to solid-liquid ratio, cooked solution total acid T.A. is that the required magnesium bisulfite cooking liquor of 1.0% calculating (is ortho acid 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% by calculate determining the MgO addition according to combined acid C.A. again, add distilled water at last and mix the pretreated raw material of back adding, be incubated 100min down at 90 ℃ after feed liquid stirs;
(7) with the slurry of the gained after distilled water washing step (6) processing, wash to pH=7;
(8) step (7) is washed disposed slurry and place pulp screen, use sieve seam to add clear water as the sieve plate of 0.40mm and screen, separate 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, and particular content is as follows:
(1) is raw material with the broussonetia white bast, is cut into length 3cm-5cm with chopper, the skin section of width 15mm-25mm;
(2) the skin section is positioned in the distilled water, makes solid-liquid ratio 1:8, boil 9min after at room temperature soaking 60min;
(3) raw material of handling with distilled water washing step (2) washs 6 times, drains;
(4) step (3) washing back raw material is carried out the phosphoric acid preliminary treatment, add (the NaPO of raw material over dry quality 0.5% in the raw material after draining 3) 6, and add distilled water and make solid-liquid ratio 1:12, at room temperature to soak 30min after stirring earlier, and then use phosphorus acid for adjusting pH value to 1.8, the back that stirs is at 85 ℃ of insulation 120mim down;
(5) raw material of handling with distilled water washing step (4) washs to pH=7.5;
(6) step (5) is washed the back raw material and carry out the magnesium sulfite process processing, be that the proportional meter of 1:5 is calculated required liquor capacity according to solid-liquid ratio, cooked solution total acid T.A. is that the required magnesium bisulfite cooking liquor of 1.1% calculating (is ortho acid 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% by calculate determining the MgO addition according to combined acid C.A. again, add distilled water at last and mix the pretreated raw material of back adding, be incubated 110min down at 90 ℃ after feed liquid stirs;
(7) with the slurry of the gained after distilled water washing step (6) processing, wash to pH=6.5;
(8) step (7) is washed disposed slurry and place pulp screen, use sieve seam to add clear water as the sieve plate of 0.40mm and screen, separate 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 (3)

1. broussonetia white bast phosphoric acid preliminary treatment magnesium sulfite process pulping process, carry out slurrying with the broussonetia white bast raw material, it is characterized in that: raw material at first carries out rinsing and boils, then it is carried out the phosphoric acid preliminary treatment, adopt the magnesium sulfite process of temperate condition that it is handled at last and make paper pulp.
2. according to the described broussonetia white bast phosphoric acid of claim 1 preliminary treatment magnesium sulfite process pulping process, it is characterized in that concrete pulping process step is as follows:
(1) broussonetia white bast is cut into long 3cm-5cm, the skin section of width 15mm-25mm is as the chemical pulping raw material;
(2) rinsing is boiled: raw material is positioned in the distilled water, and making solid-liquid ratio is 1:6-1:10, boils 6min-10min after at room temperature soaking 60min;
(3) raw materials treated filtration washing with distilled water washing 6 times, drains;
(4) phosphoric acid the preliminary treatment: (NaPO that adds raw material over dry quality 0.4%-0.6% in the raw material after draining 3) 6, and adding distilled water, to make solid-liquid ratio be 1:10-1:20, uses the phosphorus acid for adjusting pH value to 1.5-2.0 after at room temperature soaking 30min, the back that stirs is at 85 ℃-95 ℃ insulation 90min-120mim down;
(4) to be washed with distilled water to pH be 6.5-7.5 to pretreated raw material;
(5) pretreated raw material carries out the magnesium sulfite process processing of temperate condition, and it is 6.5-7.5 that the back paper pulp of finishing dealing with is washed with distilled water to pH;
(6) gained slurry in washing back places pulp screen, uses the sieve seam to add clear water as the sieve plate of 0.40mm and screens, and the separation screening reject namely obtains clean paper pulp.
3. according to the technology of the described broussonetia white bast phosphoric acid of claim 2 preliminary treatment magnesium sulfite process slurrying, it is characterized in that: the process conditions that the magnesium sulfite process of step (5) temperate condition is handled 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 the 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 0.7%-0.9% calculates definite MgO addition as requested again, add distilled water at last and mix the pretreated raw material of back adding, feed liquid evenly stirs the back and is incubated 90min-120min down at 85 ℃-95 ℃.
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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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
JP2012512138A (en) * 2008-11-28 2012-05-31 株式會社アモーレパシフィック Facial pack manufactured using Korean paper cotton for makeup

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
JP2012512138A (en) * 2008-11-28 2012-05-31 株式會社アモーレパシフィック Facial pack manufactured using Korean paper cotton for makeup

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
何洁: "光叶楮白皮制浆方法的比较及亚铵制浆工艺的优化", 《中国造纸》 *
何洁: "光叶楮白皮化学制浆的研究及其生物制浆的初探", 《中国学位论文全文数据库》 *
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