CN104153229A - Preparation method of bamboo dissolving pulp - Google Patents
Preparation method of bamboo dissolving pulp Download PDFInfo
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- CN104153229A CN104153229A CN201410339894.7A CN201410339894A CN104153229A CN 104153229 A CN104153229 A CN 104153229A CN 201410339894 A CN201410339894 A CN 201410339894A CN 104153229 A CN104153229 A CN 104153229A
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Abstract
The invention discloses a preparation method of bamboo dissolving pulp. The preparation method disclosed by the invention comprises bamboos as the raw material and comprises the following steps: pre-hydrolyzing bamboo chips through diluted acetic acid, stewing the pre-hydrolyzed raw material with sulphate, processing pulp through oxygen delignification, extracting the pulp with cold caustic, bleaching with D0-(EP)-D1, and thus obtaining the bamboo dissolving pulp. The prepared bamboo dissolving pulp is more than 90% of ISO (International Standardization Organization) in whiteness, more than 92% in content of alpha-cellulose, 959 ml/g in intrinsic viscosity, 3.23% in content of pentosan, 0.11% in content of ash, and 38% in yield; compared with the yield of 30-35% in the common process currently, the yield of the bamboo dissolving pulp disclosed by the invention is at least increased by 3-8%, and therefore, the preparation method of the bamboo dissolving pulp disclosed by the invention has great economic benefit.
Description
Technical field
The present invention relates to pulping process technical field, be specifically related to a kind of bamboo fibre dissolving pulp and production technology thereof.
Background technology
Dissolving pulp claims again spoelalty pulp, or refined stock, its main application is as the viscose of producing textile raw material, is also the raw material of the products such as glassine paper, pharmaceuticals industry sterilising filtration paper, acetate fiber (cigarette is crossed mouth rod raw material), nitrocellulose, carboxymethyl cellulose, microcrystalline cellulose, cellulose ether simultaneously.Dissolving pulp is the purer and uniform high-quality chemical pulp of one, and its alpha-cellulose content is 90%～98%.The traditional raw material of producing dissolving pulp is needlebush and cotton linter, but because domestic timber resources is under-supply, and cotton linter price is larger with market fluctuation, so for a long time, domestic dissolving pulp mainly depends on import.The consumption of dissolving pulp maximum is that Making viscose fiber is to produce artificial silk, as textile material.Along with the rapid growth of domestic market to viscose demand, the output of dissolving pulp also will keep the trend of a growth.
Although prepare the performance indications difference of desired dissolving pulp for different product, its basic demand is consistent, i.e. high the and degree of polymerization homogeneous of alpha-cellulose content, and poly-pentose and impurity content are low.Other raw material of research and utilization is produced dissolving pulp, not only can solve dissolving pulp and supply with nervous problem, also can reduce the felling to trees, protection of the environment.Bamboo is a kind of long fiber lignin raw material, because its chemical composition is close with needlebush, and has the feature that growth cycle is short, output is high, so be considered to a kind of raw material of production dissolving pulp of high-quality.In industrial production, although the production technology of dissolving pulp is very ripe, produces the product yield obtaining and be difficult to all the time exceed 30%-35%, this has limited the control of enterprise's production cost and the increase of profit greatly.So in keeping dissolving pulp product quality, the yield how research improves product is very significant.
Summary of the invention
The present invention has overcome the deficiencies in the prior art, provides that a kind of product yield is high, the preparation method of the measured bamboo dissolved pulp of matter.For solving the problems of the technologies described above, the invention provides following technical scheme.
A preparation method for bamboo dissolving pulp, comprises the steps:
(1) bamboo chip is adopted to diluted acid prehydrolysis, the condition of prehydrolysis is: diluted acid mass concentration 0.1%-10%, solid-to-liquid ratio 1:5-1:10, temperature 130-180 DEG C, heating-up time 60-150min, temperature retention time 15-120min;
(2) raw material after prehydrolysis is through washing, carry out sulphate cook, conditions of cooking is: solid-to-liquid ratio 1:5-1:10, boiling temperature 160-180 DEG C, heating-up time 60-90min, temperature retention time 30-120min, the mass ratio of NaOH and bamboo chip is 15%-20%, the mass ratio of vulcanized sodium and bamboo chip is 4%-8%; The described heating-up time refers to rise to the needed time of boiling temperature from 80 DEG C;
(3) slurry carries out oxygen delignification, and technique is as follows: slurry concentration is controlled to 8%-15%, and reaction temperature is 80-105 DEG C, reaction time is 50-90min, oxygen is pressed as 500-800KPa, and NaOH mass concentration is 1.5%-3%, magnesium sulfate mass concentration 0.15%-0.3%;
(4) slurry carries out cold alkali extracting processing, and technique is as follows: slurry concentration is controlled to 8%-15%, and reaction temperature is 25-50 DEG C, and the reaction time is 50-70min, and NaOH mass concentration is 3%-8%;
(5) slurry carries out D
0-(E
p)-D
1bleaching, technique is as follows: slurry concentration is controlled to 8%-15%, and reaction temperature is 60-80 DEG C, reaction time is 50-200min, the relative oven dry stock of Chlorine is 3%-6%, and hydrogen peroxide consumption is 0.2-0.4%, and sodium hydroxide concentration is 1.0-3.0%.
In step (1), diluted acid used is acetic acid.Preferably, the mass concentration of acetic acid is 0.1%-5%.
Described in step (1), temperature is 140-170 DEG C, and the heating-up time is 60-120min, and temperature retention time is 15-90min.
The boiling reagent that in step (2), sulfate process adopts is NaOH and vulcanized sodium, and wherein the mass ratio of NaOH and bamboo chip is 17%-20%, and the mass ratio of vulcanized sodium and bamboo chip is 5%-7%.
In step (2), boiling temperature is 160-170 DEG C, and the heating-up time is 70-90min, and temperature retention time is 30-90min.
In step (3), the added chemical reagent of oxygen delignification is oxygen, NaOH, magnesium sulfate, and oxygen is pressed as 600-700KPa, and NaOH mass concentration is 2%-3%, magnesium sulfate mass concentration 0.2%-0.3%; The slurry concentration of oxygen delignification is 10%-15%, and reaction temperature is 90-105 DEG C.
In step (4), the reaction paste concentration of cold alkali extracting processing is 10%-15%, and reaction temperature is 30-50 DEG C, and the reaction time is 50-70min, and NaOH mass concentration is 5%-8%.
That in step (5), bleaching adopts is D
0-(E
p)-D
1three sections are floated.D represents ClO 2 bleaching, (E
p) represent alkaline hydrogen peroxide bleaching.Described hydrogen peroxide consumption is 0.3%, sodium hydroxide concentration 1.5%.
Compared with existing dissolving pulp production technology, the invention has the advantages that:
(1) the dissolving pulp product yield obtaining is high, exceeds at least 3%-8% compared with other technique.
(2) bamboo chip adopts acetic acid,diluted to carry out prehydrolysis.Compare with traditional dilute sulfuric acid prehydrolysis, have following 2 benefits: 1, the acidity of acetic acid compared with sulfuric acid a little less than, reduced the corrosion to equipment; 2, prehydrolysis reaction causes removing of hemicellulose acetyl group, itself just can produce acetic acid, and the acid for catalysis that can extract to serve as prehydrolysis reaction to it, has realized the recycle of reagent.
(3) addition of acetic acid is reasonable.Certain mass strength acetic acid add catalysis hemicellulose remove reaction, reduced the needed temperature of reaction, shortened the reaction time, reduced the energy consumption of preprocessing process.
(4) technological parameter of prehydrolysis and follow-up sulphate cook process arranges rationally, has ensured the yield of product.The yield of dissolving pulp final products depends primarily on the reaction control of prehydrolysis and sulphate cook, and removing of half fiber and lignin need to reach corresponding balance in these two processes, could not only ensure cooking quality but also can make yield reach the highest.
(5) oxygen delignification, cold alkali extracting, D
0-(E
p)-D
1the technological parameter of operation arranges rationally, has ensured that the performance indications of product reach requirement.
Detailed description of the invention
Below in conjunction with embodiment, the invention will be further described, but the scope of protection of present invention is not limited to this.
Embodiment 1
A preparation method for bamboo dissolving pulp, improves implementation step as follows: bamboo chip is through acetic acid,diluted prehydrolysis, sulphate cook, oxygen delignification, cold alkali extracting, D
0-(E
p)-D
1bleaching obtains dissolving pulp product.Concrete technology is as shown in table 1.
The technological process of table 1. dissolving pulp
The whiteness of the dissolving pulp of gained is 92.24%ISO, and alpha-cellulose is 93.16%, and inherent viscosity is 959ml/g, and poly-pentose content is 5.23%, and content of ashes is 0.17%, and yield is 37.26%.
Embodiment 2
As described in Example 1, difference is that the temperature of prehydrolysis is 170 DEG C, and the temperature retention time of sulphate cook is 60min.The whiteness of the dissolving pulp of gained is 91.6%ISO, and alpha-cellulose is 95.74%, and inherent viscosity is 714ml/g, and poly-pentose content is 4.11%, and content of ashes is 0.11%, and yield is 31.12%.
Embodiment 3
As described in Example 1, difference is that the temperature of prehydrolysis is 150 DEG C, and the temperature retention time of sulphate cook is 60min.The whiteness of the dissolving pulp of gained is 89.84%ISO, and alpha-cellulose is 87.12%, and inherent viscosity is 951ml/g, and poly-pentose content is 10.01%, and content of ashes is 0.19%, and yield is 38.31%.
Embodiment 4
As described in Example 1, difference is that the temperature of prehydrolysis is 140 DEG C, and the temperature retention time of sulphate cook is 60min.The whiteness of the dissolving pulp of gained is 90.84%ISO, and alpha-cellulose is 83.12%, and inherent viscosity is 923ml/g, and poly-pentose content is 12.01%, and content of ashes is 0.21%, and yield is 40.31%.
Embodiment 5
As described in Example 1, difference is that the temperature retention time of sulphate cook is 60min.The whiteness of the dissolving pulp of gained is 90.84%ISO, and alpha-cellulose is 92.12%, and inherent viscosity is 906ml/g, and poly-pentose content is 5.12%, and content of ashes is 0.11%, and yield is 36.31%.
Embodiment 6
As described in Example 1, difference is that the temperature retention time of sulphate cook is 90min.The whiteness of the dissolving pulp of gained is 92.84%ISO, and alpha-cellulose is 92.12%, and inherent viscosity is 900ml/g, and poly-pentose content is 5.01%, and content of ashes is 0.11%, and yield is 36.31%.
Embodiment 7
As described in Example 1, difference is that the temperature retention time of sulphate cook is 120min.The whiteness of the dissolving pulp of gained is 91.84%ISO, and alpha-cellulose is 92.12%, and inherent viscosity is 951ml/g, and poly-pentose content is 4.01%, and content of ashes is 0.11%, and yield is 36.11%.
Embodiment 8
As described in Example 1, difference is that the consumption of acetic acid is 0.1%, and the temperature retention time of sulphate cook is 60min.The whiteness of the dissolving pulp of gained is 89.84%ISO, and alpha-cellulose is 90.12%, and inherent viscosity is 931ml/g, and poly-pentose content is 6.01%, and content of ashes is 0.15%, and yield is 37.31%.
Embodiment 9
As described in Example 1, difference is that in sulphate cook step, NaOH is 20% to the percentage of raw material, and vulcanized sodium is 8% to the percentage of raw material, and the temperature retention time of sulphate cook is 60min.The whiteness of the dissolving pulp of gained is 93.84%ISO, and alpha-cellulose is 96.12%, and inherent viscosity is 551ml/g, and poly-pentose content is 3.01%, and content of ashes is 0.09%, and yield is 30.31%.
Embodiment 10
As described in Example 1, difference is that in sulphate cook step, NaOH is 15% to the percentage of raw material, and vulcanized sodium is 4% to the percentage of raw material, and the temperature retention time of sulphate cook is 60min.The whiteness of the dissolving pulp of gained is 82.84%ISO, and alpha-cellulose is 81.12%, and inherent viscosity is 1001ml/g, and poly-pentose content is 15.01%, and content of ashes is 0.19%, and yield is 42.31%.
Embodiment 11
As described in Example 1, difference is that prehydrolysis temperature is 140 DEG C, and the heating-up time is 120min, and the temperature retention time of sulphate cook is 60min.The whiteness of the dissolving pulp of gained is 89.84%ISO, and alpha-cellulose is 91.12%, and inherent viscosity is 901ml/g, and poly-pentose content is 6.01%, and content of ashes is 0.15%, and yield is 37.31%.
Embodiment 12
As described in Example 1, difference is that prehydrolysis temperature is 140 DEG C, and temperature retention time is 120min, and the temperature retention time of sulphate cook is 60min.The whiteness of the dissolving pulp of gained is 92.84%ISO, and alpha-cellulose is 93.12%, and inherent viscosity is 851ml/g, and poly-pentose content is 6.11%, and content of ashes is 0.15%, and yield is 36.31%.
Embodiment 13
As described in Example 1, difference is that the boiling temperature of sulphate cook is 170 DEG C, and temperature retention time is 60min.The whiteness of the dissolving pulp of gained is 91.84%ISO, and alpha-cellulose is 94.12%, and inherent viscosity is 801ml/g, and poly-pentose content is 5.11%, and content of ashes is 0.12%, and yield is 35.32%.
Embodiment 14
As described in Example 1, difference is that the temperature retention time of sulphate cook is 60min, and the consumption of bleaching stage chlorine dioxide is 6%.The whiteness of the dissolving pulp of gained is 93.84%ISO, and alpha-cellulose is 95.12%, and inherent viscosity is 851ml/g, and poly-pentose content is 3.91%, and content of ashes is 0.11%, and yield is 35.82%.
Embodiment 15
As described in Example 1, difference is that the temperature retention time of sulphate cook is 60min, and the consumption of bleaching stage chlorine dioxide is 3%.The whiteness of the dissolving pulp of gained is 85.84%ISO, and alpha-cellulose is 88.12%, and inherent viscosity is 1051ml/g, and poly-pentose content is 9.91%, and content of ashes is 0.17%, and yield is 38.82%.
Claims (9)
1. a preparation method for bamboo dissolving pulp, is characterized in that, comprises the steps:
(1) bamboo chip is adopted to diluted acid prehydrolysis, the condition of prehydrolysis is: diluted acid mass concentration 0.1%-10%, solid-to-liquid ratio 1:5-1:10, temperature 130-180 DEG C, heating-up time 60-150min, temperature retention time 15-120min;
(2) raw material after prehydrolysis is through washing, carry out sulphate cook, conditions of cooking is: solid-to-liquid ratio 1:5-1:10, boiling temperature 160-180 DEG C, heating-up time 60-90min, temperature retention time 30-120min, the mass ratio of NaOH and bamboo chip is 15%-20%, the mass ratio of vulcanized sodium and bamboo chip is 4%-8%; The described heating-up time refers to rise to the needed time of boiling temperature from 80 DEG C;
(3) slurry carries out oxygen delignification, and technique is as follows: slurry concentration is controlled to 8%-15%, and reaction temperature is 80-105 DEG C, reaction time is 50-90min, oxygen is pressed as 500-800KPa, and NaOH mass concentration is 1.5%-3.0%, magnesium sulfate mass concentration 0.15%-0.3%;
(4) slurry carries out cold alkali extracting processing, and technique is as follows: slurry concentration is controlled to 8%-15%, and reaction temperature is 25-50 DEG C, and the reaction time is 50-70min, and NaOH mass concentration is 3%-8%;
(5) slurry carries out D
0-(E
p)-D
1bleaching, technique is as follows: slurry concentration is controlled to 8%-15%, and reaction temperature is 60-80 DEG C, reaction time is 50-200min, the relative oven dry stock of Chlorine is 3%-6%, and hydrogen peroxide consumption is 0.2-0.4%, and sodium hydroxide concentration is 1.0-3.0%.
2. method according to claim 1, is characterized in that, in step (1), diluted acid used is acetic acid.
3. method according to claim 2, is characterized in that, the mass concentration of acetic acid is 0.1%-5%.
4. according to the method described in claim 1 or 2 or 3, it is characterized in that, described in step (1), temperature is 140-170 DEG C, and the heating-up time is 60-120min, and temperature retention time is 15-90min.
5. according to the method described in claim 1 or 2 or 3, it is characterized in that, in step (2), the mass ratio of NaOH and bamboo chip is 17%-20%, and the mass ratio of vulcanized sodium and bamboo chip is 5%-7%.
6. according to the method described in claim 1 or 2 or 3, it is characterized in that, in step (2), boiling temperature is 160-170 DEG C, and the heating-up time is 70-90min, and temperature retention time is 30-90min.
7. according to the method described in claim 1 or 2 or 3, it is characterized in that, in step (3), the slurry concentration of oxygen delignification is 10%-15%, reaction temperature is 90-105 DEG C, oxygen is pressed as 600-700KPa, NaOH mass concentration is 2%-3%, magnesium sulfate mass concentration 0.2%-0.3%.
8. according to the method described in claim 1 or 2 or 3, it is characterized in that, in step (4), the reaction paste concentration of cold alkali extracting processing is 10%-15%, and reaction temperature is 30-50 DEG C, reaction time is 50-70min, and NaOH mass concentration is 5%-8%.
9. according to the method described in claim 1 or 2 or 3, it is characterized in that, described in step (5), hydrogen peroxide consumption is 0.3%, sodium hydroxide concentration 1.5%.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104863004A (en) * | 2015-04-23 | 2015-08-26 | 中国制浆造纸研究院 | Cotton brei pulp preparation and pollution treatment method |
| CN106436412A (en) * | 2015-08-08 | 2017-02-22 | 四川信联融创实业有限公司 | Preparation method of unbleached neosinocalamus affinis paper pulp |
| CN107696194A (en) * | 2017-11-24 | 2018-02-16 | 广西博白焕发工艺品有限公司 | It is a kind of to retain the blue or green bamboo cane processing method of the natural bamboo of bamboo |
| CN108867130A (en) * | 2018-04-26 | 2018-11-23 | 天津科技大学 | The pulping process of high yield pulp1 needlebush dissolving pulp and its dissolving pulp of preparation |
| CN108951254A (en) * | 2018-07-09 | 2018-12-07 | 广西大学 | A kind of method that bamboo hemicellulose efficiently separates |
| CN112431055A (en) * | 2020-11-16 | 2021-03-02 | 陕西科技大学 | Novel process for preparing dissolving pulp from chemical pulp for papermaking |
| CN112482069A (en) * | 2020-11-24 | 2021-03-12 | 中国林业科学研究院林产化学工业研究所 | Method for preparing high-yield dissolving pulp by using eutectic solvent |
| CN113319959A (en) * | 2021-05-27 | 2021-08-31 | 南京林业大学 | Preparation method of microfibrillated bamboo |
| CN114606788A (en) * | 2022-03-07 | 2022-06-10 | 华南理工大学 | Method for synchronously preparing dissolving pulp and furfural from wood fibers |
| CN114808512A (en) * | 2022-04-26 | 2022-07-29 | 赣南师范大学 | Bamboo dissolving pulp suitable for alkali urea system and preparation method thereof |
| CN116761914A (en) * | 2021-01-22 | 2023-09-15 | 东丽株式会社 | Wet nonwoven fabric sheet |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| RU2763878C1 (en) * | 2020-11-30 | 2022-01-11 | Акционерное общество "Научно-производственное объединение "БИОТЕХКОМПОЗИТ" | Method for obtaining cellulose for chemical processing from cellulose-containing raw materials |
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| CN1410627A (en) * | 2002-09-16 | 2003-04-16 | 成都春天绿竹资源开发有限责任公司 | Production technology of pure natural antibacterial bamboo paste |
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| CN1410627A (en) * | 2002-09-16 | 2003-04-16 | 成都春天绿竹资源开发有限责任公司 | Production technology of pure natural antibacterial bamboo paste |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104863004A (en) * | 2015-04-23 | 2015-08-26 | 中国制浆造纸研究院 | Cotton brei pulp preparation and pollution treatment method |
| CN106436412A (en) * | 2015-08-08 | 2017-02-22 | 四川信联融创实业有限公司 | Preparation method of unbleached neosinocalamus affinis paper pulp |
| CN107696194A (en) * | 2017-11-24 | 2018-02-16 | 广西博白焕发工艺品有限公司 | It is a kind of to retain the blue or green bamboo cane processing method of the natural bamboo of bamboo |
| CN108867130A (en) * | 2018-04-26 | 2018-11-23 | 天津科技大学 | The pulping process of high yield pulp1 needlebush dissolving pulp and its dissolving pulp of preparation |
| CN108951254A (en) * | 2018-07-09 | 2018-12-07 | 广西大学 | A kind of method that bamboo hemicellulose efficiently separates |
| CN112431055A (en) * | 2020-11-16 | 2021-03-02 | 陕西科技大学 | Novel process for preparing dissolving pulp from chemical pulp for papermaking |
| CN112482069A (en) * | 2020-11-24 | 2021-03-12 | 中国林业科学研究院林产化学工业研究所 | Method for preparing high-yield dissolving pulp by using eutectic solvent |
| CN116761914A (en) * | 2021-01-22 | 2023-09-15 | 东丽株式会社 | Wet nonwoven fabric sheet |
| CN113319959A (en) * | 2021-05-27 | 2021-08-31 | 南京林业大学 | Preparation method of microfibrillated bamboo |
| CN114606788A (en) * | 2022-03-07 | 2022-06-10 | 华南理工大学 | Method for synchronously preparing dissolving pulp and furfural from wood fibers |
| CN114808512A (en) * | 2022-04-26 | 2022-07-29 | 赣南师范大学 | Bamboo dissolving pulp suitable for alkali urea system and preparation method thereof |
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