CN102517968B - Method for preparing dissolving pulp for viscose fibers by using mulberry twig stem cores - Google Patents

Method for preparing dissolving pulp for viscose fibers by using mulberry twig stem cores Download PDF

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CN102517968B
CN102517968B CN201110429153.4A CN201110429153A CN102517968B CN 102517968 B CN102517968 B CN 102517968B CN 201110429153 A CN201110429153 A CN 201110429153A CN 102517968 B CN102517968 B CN 102517968B
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pressure
pulp
dissolving pulp
bar core
concentration
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CN102517968A (en
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王乐军
马君志
秦翠梅
姜明亮
王东
吴亚红
李昌垒
郝连庆
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Weifang Xinlong Biomaterials Co Ltd
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CHTC Helon Co Ltd
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Abstract

The invention discloses a method for preparing dissolving pulp for viscose fiber by adopting mulberry branch stem core, which comprises the steps of raw material preparation, steaming, material washing, concentration, stewing, pulp extrusion, screening, alkali refining, bleaching, acid treatment, water washing, after-selection and pulp making to obtain finished pulp; the invention has the advantages that: the invention provides a method for preparing dissolving pulp by using mulberry twig stem cores independently, which avoids the problems that the product quality and yield are influenced by over-severe or insufficient cooking conditions caused by different structures of the mulberry twigs and the mulberry twig stem cores during full-stem pulping.

Description

A kind of method that adopts ramulus mori bar core Making viscose fiber to use dissolving pulp
Technical field
The present invention relates to a kind of preparation method of dissolving pulp, specifically a kind of method that adopts ramulus mori bar core Making viscose fiber to use dissolving pulp, belongs to dissolving pulp manufacturing technology field.
Background technology
The consumption proportion of textile fabric, over nearly 200 years, has particularly had huge development over nearly 30 years.But the growth of textile fiber material, is faced with many difficulties.At present cellulose viscose is that people apply a kind of fiber very widely, and is used for the raw material of production of cellulose viscose, mainly with needlebush, leaf wood or velveteen, is main raw material.Due to the pressure of population in the world to grain demand, cotton field sown area can not increase from now on again, and the growth space of yield per unit area is little.Required wood pulp, the cotton linter dissolving pulp of regenerated celulose fibre reaches capacity, and domestic viscose manufacturer constantly expanded production in recent years, when production capacity improves, technical merit also makes great progress, cause viscose constantly to increase by raw materials requirement, therefore, open up the guarantee that new raw material sources become viscose industry energy steady development.
Mulberry tree is a kind of main industrial crops in current people's agricultural production, and the output of the byproduct ramulus mori bar of planting as mulberry tree is very considerable, and the average fiber length of ramulus mori is 1.94mm, average diameter 11.1 μ m; Mu is planted mulberry tree 5000~5500 strains, and just energy per mu yield ramulus mori is more than two tons, so the output of ramulus mori is very large.And current people gather in later ramulus mori to mulberry tree and only have sub-fraction to be used as feed, fertilizer, all the other multiplex works combustion bavins or set fire and have mercy on have caused great waste in contaminated environment.
If using the exploitation of ramulus mori bar as the pulping raw material of producing viscose, not only can greatly alleviate the nervous problem of current viscose raw materials for production, also can greatly improve value and the economic worth of ramulus mori bar.Yet ramulus mori bast and bar core morphosis differ larger.Phloem fiber cellulose content is high, and filament length is longer, is good pulping raw material, by the existing a large amount of research of bast slurrying and ripe technique; Bar core part fiber is shorter, and content of cellulose is low, and slurrying difficulty is larger.At present ramulus mori is used in and in slurrying, is total-bar slurry making, yet thisly with same technique, bast and bar core is processed, and can cause and react inhomogeneous, affects quality and yield, and cost significantly rises.
Summary of the invention
In order to address the above problem, the present invention has designed a kind of method of dissolving pulp for ramulus mori bar core Making viscose fiber that adopts, the method is by carrying out decatize and reduce hemicellulose level removing ramulus mori bar core after bast fiber, reduce boiling intensity, improve reactivity worth, by alkali refining, improve the fine content of first, technique is simple, easy to operate, and greatly reduce the pollution to environment of the pulping waste liquor that produces after slurrying.
Technical scheme of the present invention is:
A kind of method that adopts ramulus mori bar core Making viscose fiber to use dissolving pulp, comprise material preparation, decatize, wash material, make finished pulp after concentrated, boiling, shove, screening, alkali refining, bleaching, acid treatment, washing, rear selected, papermaking, concrete operations are as follows:
(1) get the raw materials ready: mulberry bar core is cut to after the section shape of long 3-7cm, carries out conquassation processing, collapse pressure 0.30~0.60MPa, to improve the penetrating power of decatize and alkali lye, makes boiling more even, increases the contact area of fiber and steam and cooking liquor;
(2) decatize: the bar core that above-mentioned steps (1) is got the raw materials ready after processing, 30 ± 5min is warming up to 110~130 ℃, and under 0.20~0.35MPa, decatize is processed 40~60min, poly-pentose content 2~5% after decatize;
(3) wash material: 50~60 ℃ of temperature of washing water, wash 2~3 times;
(4) concentrated: to send the slurry after washing to row squeezing concentrated, squeeze pressure 0.15~0.25MPa; By waste water and washes sewer treatment plant after membrane filtration after squeezing;
(5) boiling: cooking liquor, than 1:2.5~3.5, is joined alkali and be take NaOH concentration as 30~50g/L, and alkali charge is counted 8~12% of over dry quality of material with NaOH; Adopt secondary temperature elevation method, the 30 ± 5min that once heats up, the pressure in digesting apparatus reaches 0.25 ± 0.05MPa, and little steam bleeding to the pressure in digesting apparatus is 0MPa; Secondary temperature elevation 40 ± 5min, the pressure in digesting apparatus reaches 0.5 ± 0.05MPa, is incubated large steam bleeding after 100~150min; Black liquor CODcr 9000~12000 mg/L after boiling, 2000~3000 times of colourities, half stuff ash 0.80~1.5 %, iron part 80~120mg/kg, viscosity 12.0~14.0mpa.s, lignin content 0.15~0.25%;
(6) shove: enter to starch concentration 2~5%, pulp concentration 15~25%, shove pressure 0.10~0.25 MPa;
(7) screening: the frame plansifter that shakes enters to starch concentration 1~1.5%, pulp concentration 0.6~0.8%; Pressurized screen enters to starch concentration 1.0~2.5%, enters to starch pressure 0.1~0.25 MPa;
(8) alkali refining: starch dense 6~10%, 80 ℃~100 ℃ of alkali refining temperature, addition amount of sodium hydroxide is 7~10% of over dry stock quality, time 40~60min;
(9) bleaching: floating front slurry dense is 4.5~8.0%, regulates pH value between 8~11, and bleaching liquor addition is 0.5~4% of over dry stock quality, bleaching time 40~90min, ten minutes residual chlorine 0.20~0.70g/L;
(10) post processing: by the slurry after bleaching through peracid treatment, washing, after selected, papermaking and dry after obtain described dissolving pulp finished product.
Certainly can the situation according to the needs of producing and in producing carry out suitable adjustment, this is known general knowledge concerning those skilled in that art.
The invention has the advantages that:
(1) provide a kind of independent method of preparing dissolving pulp with ramulus mori bar core, while having avoided total-bar slurry making, because ramulus mori is different with ramulus mori bar cored structure, caused conditions of cooking to cross violent or not enough, affected product quality and yield;
(2) the direct boiling of bar core meeting causes the consumption of chemical industry material large, pollutes and weighs, and by decatize, makes ramulus mori bar core become soft, has reduced space, has increased the charge amount of digesting apparatus; Decatize has reduced the content of poly-pentose and lignin in raw material, reduced follow-up boiling intensity, and the waste liquid after decatize can be used for extracting lignin and sugar;
(3) boiling intensity is low, and traditional chemical pulp alkali charge is in 20% left and right, and alkali charge of the present invention, 8~12%, reduces chemicals usage, and cooking waste liquor CODcr content is reduced, and reduces cost of sewage disposal;
(4) provide a kind of quality raw materials of Making viscose fiber, effectively alleviated the nervous problem of raw materials for production of current viscose, and for ramulus mori exploitation provides a kind of approach that utilizes of high added value, turned waste into wealth.
The specific embodiment
Below the preferred embodiments of the present invention are described, should be appreciated that preferred embodiment described herein, only for description and interpretation the present invention, is not intended to limit the present invention.
Except as otherwise noted, the percentage adopting in the present invention is percetage by weight.
Embodiment 1
Adopt a method for dissolving pulp for ramulus mori bar core Making viscose fiber, concrete operations are as follows:
(1) get the raw materials ready: bar core is cut to after the section shape of long 5cm, carries out conquassation, collapse pressure 0.30MPa;
(2) decatize: storehouse is steamed in the bar core admission after above-mentioned steps (1) is got the raw materials ready and processed, heating-up time 25min, at 0.20MPa, processes 60min, poly-pentose content 4.85% after decatize, lignin content 5.84% at 115 ℃;
(3) wash material: 50 ℃ of temperature of washing water, wash 3 times;
(4) concentrated: the slurry after washing is delivered to squeezer concentrated, squeeze pressure 0.15MPa, by waste water and washes sewer treatment plant after membrane filtration after squeezing;
(5) boiling: cooking liquor, than 1:2.5, is joined alkali and be take NaOH concentration as 30g/L, and alkali charge is counted 8% of over dry quality of material with NaOH; Adopt secondary temperature elevation method, the 25min that once heats up, the force value of digesting apparatus reaches 0.20MPa, and little steam bleeding to the force value in vertical pot is 0MPa; Secondary temperature elevation 35min, the force value in vertical pot reaches 0.45MPa, large steam bleeding after insulation 150min; Black liquor CODcr 11320 mg/L, 2216 times of colourities, half stuff ash 0.90%, iron part 89mg/kg, viscosity 13.8mpa.s, lignin content 0.24% after boiling;
(6) shove: enter to starch concentration 2%, pulp concentration 15%, shove pressure 0.10 MPa;
(7) screening: the frame plansifter that shakes enters to starch concentration 1%, pulp concentration 0.6%; Pressurized screen enters to starch concentration 1.0%, enters to starch pressure 0.1 MPa;
(8) alkali refining: starch dense 6%, 80 ℃ of alkali refining temperature, addition amount of sodium hydroxide is 7% of over dry stock quality, time 60min;
(9) bleaching: floating front slurry dense is 4.5%, and floating front tune PH is 8, and bleaching liquor addition is 4% of over dry stock quality, bleaching time 40min, ten minutes residual chlorine 0.69g/L;
(10) post processing: by the slurry after bleaching through peracid treatment, washing, after selected, papermaking and dry after obtain described dissolving pulp finished product.
Finished product index: first fibre 93.2%, ash 0.10%, iron part 18 mg/kg, viscosity 10.2 mpa.s, reactivity worth 182s, little dust 162mg/kg, whiteness 80%.
Embodiment 2
Adopt a method for dissolving pulp for ramulus mori bar core Making viscose fiber, concrete operations are as follows:
(1) get the raw materials ready: bar core is cut to after the section shape of long 5cm left and right, carries out conquassation, collapse pressure 0.40MPa;
(2) decatize: storehouse is steamed in the bar core admission after above-mentioned steps (1) is got the raw materials ready and processed, heating-up time 30min, at 0.30MPa, processes 50min at 128 ℃.Poly-pentose content 3.52% after decatize, lignin content 4.95%;
(3) wash material: 50 ℃ of temperature of washing water, wash 3 times;
(4) concentrated: the slurry after washing to be delivered to squeezer concentrated, squeeze pressure 0.20MPa; By waste water and washes sewer treatment plant after membrane filtration after squeezing;
(5) boiling: cooking liquor, than 1:3.0, is joined alkali and be take NaOH concentration as 40g/L, and alkali charge is counted 10% of over dry quality of material with NaOH; Adopt secondary temperature elevation method, the 30min that once heats up, the pressure in digesting apparatus rotary spherical digester reaches 0.20MPa, and little steam bleeding to the pressure in rotary spherical digester is 0MPa; Secondary temperature elevation 40min, the pressure in rotary spherical digester reaches 0.50MPa, large steam bleeding after insulation 120min; Black liquor CODcr 9264 mg/L, 2066 times of colourities, half stuff ash 1.14 %, iron part 99mg/kg, viscosity 12.6mpa.s, lignin content 0.20% after boiling;
(6) shove: enter to starch concentration 4%, pulp concentration 20%, shove pressure 0.15MPa;
(7) screening: the frame plansifter that shakes enters to starch concentration 1%, pulp concentration 0.7%; Pressurized screen enters to starch concentration 2.0%, enters to starch pressure 0.20 MPa;
(8) alkali refining: starch dense 8%, 90 ℃ of alkali refining temperature, addition amount of sodium hydroxide is 8% of over dry stock quality, time 50min;
(9) bleaching: floating front slurry dense is 5%, and floating front tune PH is 10, and bleaching liquor addition is 2% of over dry stock quality, bleaching time 50min, ten minutes residual chlorine 0.36g/L;
(10) post processing: by the slurry after bleaching through peracid treatment, washing, after selected, papermaking and dry after obtain described dissolving pulp finished product.
Finished product index: first fibre 93.7%, ash 0.08%, iron part 15 mg/kg, viscosity 10.7 mpa.s, reactivity worth 206s, little dust 182mg/kg, whiteness 81%.
Embodiment 3
(1) get the raw materials ready: bar core is cut to after the section shape of long 5cm left and right, carries out conquassation, collapse pressure 0.60MPa;
(2) decatize: storehouse is steamed in the bar core admission after above-mentioned steps (1) is got the raw materials ready and processed, heating-up time 35min, at 0.35MPa, processes 40min, poly-pentose content 2.08% after decatize, lignin content 5.01% at 130 ℃;
(3) wash material: 60 ℃ of temperature of washing water, wash 2 times;
(4) concentrated: the slurry after washing to be delivered to squeezer concentrated, squeeze pressure 0.25MPa; By waste water and washes sewer treatment plant after membrane filtration after squeezing;
(5) boiling: cooking liquor, than 1:3.5, is joined alkali and be take NaOH concentration as 50g/L, and alkali charge is counted 12% of over dry quality of material with NaOH; Adopt secondary temperature elevation method, the 35min that once heats up, the pressure of digesting apparatus reaches 0.25MPa, and little steam bleeding to the pressure in vertical pot is 0MPa; Secondary temperature elevation 45min, the pressure in vertical pot reaches 0.55MPa, large steam bleeding after insulation 100min; Black liquor CODcr 11985 mg/L, 2933 times of colourities, half stuff ash 1.45 % after boiling, iron part 119mg/kg, viscosity 12.1mpa.s, lignin content 0.16%;
(6) shove: enter to starch concentration 5%, pulp concentration 25%, shove pressure 0.25 MPa;
(7) screening: the frame plansifter that shakes enters to starch concentration 1.5%, pulp concentration 0.8%; Pressurized screen enters to starch concentration 2.5%, enters to starch pressure 0.25 MPa;
(8) alkali refining: starch dense 10%, 100 ℃ of alkali refining temperature, addition amount of sodium hydroxide is 10% of over dry stock quality, time 40min;
(9) bleaching: floating front slurry dense is 8.0%, the material PH that sizes mixing before floating is 11, bleaching liquor addition is 0.5% of over dry stock quality, bleaching time 90min, ten minutes residual chlorine 0.20g/L;
(10) post processing: by the slurry after bleaching through peracid treatment, washing, after selected, papermaking and dry after obtain described dissolving pulp finished product.
Finished product index: first fibre 93.5%, ash 0.07%, iron part 12 mg/kg, viscosity 10.4 mpa.s, reactivity worth 185s, little dust 172mg/kg, whiteness 82%.
Except as otherwise noted, the percentage adopting in the present invention is mass percent.
In each embodiment of the present invention, chemical industry material used is in material ,Jun Kecong market used in the production of this area and obtains, and can not exert an influence for production result; The equipment of using in each operation, all adopts conventional equipment used in current production, there is no special feature.

Claims (10)

1. one kind adopts the method for dissolving pulp for ramulus mori bar core Making viscose fiber, it is characterized in that: comprise material preparation, decatize, wash material, make finished pulp after concentrated, boiling, shove, screening, alkali refining, bleaching, acid treatment, washing, rear selected, papermaking, concrete operations are as follows:
(1) get the raw materials ready: mulberry bar core is cut to after the section shape of long 3-7cm, carries out conquassation processing, collapse pressure 0.30~0.60MPa;
(2) decatize: the bar core that above-mentioned steps (1) is got the raw materials ready after processing, 30 ± 5min is warming up to 110~130 ℃, and under 0.20~0.35MPa, decatize is processed 40~60min, makes poly-pentose mass content 2~5%;
(3) wash material: 50~60 ℃ of temperature of washing water, wash 2~3 times;
(4) concentrated: the slurry after washing to be squeezed and concentrated, squeeze pressure 0.15~0.25MPa;
(5) boiling: cooking liquor, than 1:2.5~3.5, is joined alkali and be take NaOH concentration as 30~50g/L, and alkali charge is counted 8~12% of over dry quality of material with NaOH; Adopt secondary temperature elevation method, the 30 ± 5min that once heats up, the pressure in digesting apparatus reaches 0.25 ± 0.05MPa, and little steam bleeding to the pressure in digesting apparatus is 0MPa; Secondary temperature elevation 40 ± 5min, the pressure in digesting apparatus reaches 0.5 ± 0.05MPa, is incubated large steam bleeding after 100~150min; Black liquor CODcr 9000~12000 mg/L after boiling, 2000~3000 times of colourities, half stuff ash 0.80~1.5 %, iron part 80~120mg/kg, viscosity 12.0~14.0mPa.s, lignin content 0.15~0.25%;
(6) shove: enter to starch concentration 2~5%, pulp concentration 15~25%, shove pressure 0.10~0.25 MPa;
(7) screening: the frame plansifter that shakes enters to starch concentration 1~1.5%, pulp concentration 0.6~0.8%; Pressurized screen enters to starch concentration 1.0~2.5%, enters to starch pressure 0.1~0.25 MPa;
(8) alkali refining: starch dense 6~10%, 80 ℃~100 ℃ of alkali refining temperature, addition amount of sodium hydroxide is 7~10% of over dry stock quality, time 40~60min;
(9) bleaching: floating front slurry dense is 4.5~8.0%, regulates slurry pH value between 8~11, and bleaching liquor addition is 0.5~4% of over dry stock quality, bleaching time 40~90min, ten minutes residual chlorine 0.20~0.70g/L;
(10) post processing: by the slurry after bleaching through peracid treatment, washing, after selected, papermaking and dry after obtain described dissolving pulp finished product.
2. the method for dissolving pulp for employing ramulus mori bar core Making viscose fiber according to claim 1, is characterized in that:
The collapse pressure 0.40MPa of described step (1).
3. the method for dissolving pulp for employing ramulus mori bar core Making viscose fiber according to claim 1, is characterized in that:
Poly-pentose content 3.52% after described step (2) decatize, lignin content 4.95%.
4. the method for dissolving pulp for employing ramulus mori bar core Making viscose fiber according to claim 1, is characterized in that:
Described step (4) squeeze pressure is 0.20MPa.
5. the method for dissolving pulp for employing ramulus mori bar core Making viscose fiber according to claim 1, is characterized in that:
In described step (5) boiling, cooking liquor, than 1 ︰ 3.0, is joined alkali and be take NaOH concentration as 40g/L, and alkali charge is counted 10% of over dry quality of material with NaOH; Adopt secondary temperature elevation method, the 30min that once heats up, the pressure in digesting apparatus rotary spherical digester reaches 0.20MPa, and little steam bleeding to the pressure in rotary spherical digester is 0MPa; Secondary temperature elevation 40min, the pressure in rotary spherical digester reaches 0.50MPa, large steam bleeding after insulation 120min; Black liquor CODcr 9264 mg/L, 2066 times of colourities, half stuff ash 1.14 %, iron part 99mg/kg, viscosity 12.6mPa.s, lignin content 0.20% after boiling.
6. the method for dissolving pulp for employing ramulus mori bar core Making viscose fiber according to claim 1, is characterized in that:
Described step (6) shove enter to starch concentration 4%, pulp concentration 20%, shove pressure 0.15MPa.
7. the method for dissolving pulp for employing ramulus mori bar core Making viscose fiber according to claim 1, is characterized in that:
The frame plansifter that shakes of described step (7) screening enters to starch concentration 1%, pulp concentration 0.7%; Pressurized screen enters to starch concentration 2.0%, enters to starch pressure 0.20 MPa.
8. the method for dissolving pulp for employing ramulus mori bar core Making viscose fiber according to claim 1, is characterized in that:
Described step (8) alkali refining: starch dense 8%, 90 ℃ of alkali refining temperature, addition amount of sodium hydroxide is 8% of over dry stock quality, time 50min.
9. the method for dissolving pulp for employing ramulus mori bar core Making viscose fiber according to claim 1, is characterized in that:
Described step (9) bleaching: floating front slurry dense is 5%, and floating front tune pH is 10, and bleaching liquor addition is 2% of over dry stock quality, bleaching time 50min, ten minutes residual chlorine 0.36g/L.
10. the method for dissolving pulp for employing ramulus mori bar core Making viscose fiber according to claim 1, is characterized in that:
Prepare dissolving pulp product: first fibre 93.7%, ash 0.08%, iron part 15 mg/kg, viscosity 10.7 mPa.s, reactivity worth 206s, little dust 182mg/kg, whiteness 81%.
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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1657694A (en) * 2005-03-09 2005-08-24 中国制浆造纸研究院 Wood method for pulping using cotton stalk, bush or brush
CN101016653A (en) * 2006-08-02 2007-08-15 马立峰 Method of preparing rayon staple by benne stalk
CN101158121A (en) * 2007-11-15 2008-04-09 宜宾纸业股份有限公司 Process for manufacturing dissolved pulp by using ethanol, sulfate and acetic acid
US20080295982A1 (en) * 2005-04-27 2008-12-04 Kwon-Hyok Lee Process for Producing Fiber Pulp Utilizing Bamboo and Pulp Produced Using the Same
CN102127877A (en) * 2010-12-28 2011-07-20 宜宾竹海竹资源科技有限责任公司 Production process of bamboo-dissolving pulp

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1657694A (en) * 2005-03-09 2005-08-24 中国制浆造纸研究院 Wood method for pulping using cotton stalk, bush or brush
US20080295982A1 (en) * 2005-04-27 2008-12-04 Kwon-Hyok Lee Process for Producing Fiber Pulp Utilizing Bamboo and Pulp Produced Using the Same
CN101016653A (en) * 2006-08-02 2007-08-15 马立峰 Method of preparing rayon staple by benne stalk
CN101158121A (en) * 2007-11-15 2008-04-09 宜宾纸业股份有限公司 Process for manufacturing dissolved pulp by using ethanol, sulfate and acetic acid
CN102127877A (en) * 2010-12-28 2011-07-20 宜宾竹海竹资源科技有限责任公司 Production process of bamboo-dissolving pulp

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Patentee before: HENGTIAN HAILONG (WEIFANG) NEW MATERIALS CO.,LTD.

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