• 专利附录
  • 专利说明
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    • 专利摘要:
    A preparation process of eucalyptus dissolving pulp comprises the following steps: a: performing pre-steaming; b: subjecting eucalyptus chips to prehydrolysis in an independent continuous hydrolysis tower; c: cooking the hydrolyzed eucalyptus chips by using a sulfate process. The beneficial effects thereof are: 1. by using the continuous prehydrolysis sulfate cooking process, the investment is small, the production efficiency is high, and the process is simple and is convenient to operate; 2. by adopting an acid-free hydrolysis process, degradation of cellulose and erosion of the device caused by a mineral acid are reduced; 3. the eucalyptus dissolving pulp has more stable quality and properties, the maximum content of α-cellulose reaches 96.2%, and the content of pentosan reaches 2.35%.
    公开号:AU2012375964A1
    申请号:U2012375964
    申请日:2012-12-28
    公开日:2014-09-25
    发明作者:Kefu Chen；Hongjin LINAG；Yanbo LIU；Zehua LIU；Qinghui Lu；Jun Qiao；Guangdong YING；Bingyan ZHAI；Wei Zhang；Hongxia Zhong
    申请人:SHANDONG TAIYANGZHIYE CO Ltd；
    IPC主号:D21C3-02
    专利说明:
    Method for Producing Dissolving Pulp from Eucalyptus TECHNICAL FIELD The invention relates to a production method about dissolving pulp. More specifically, it is a method for production of dissolving pulp from eucalyptus. BACKGROUND OF THE INVENTION Dissolving pulp is a cellulose derivative prepared with prehydrolysis kraft method or acid sulfite method, mainly used for the manufacture of viscose rayon, cellulose esters (cellulose acetate, cellulose propionate, cellulose butyrate, cellulose nitrate) and cellulose ether (carboxymethyl cellulose ethers, ethyl cellulose ethers, methyl cellulose ethers), the vast majority of which used for the textile industry. With the development of viscose fiber and cellulose derivatives industry, especially viscose staple fiber, the demand for dissolving pulp is being increased. The main raw materials of dissolving pulp are cotton linters, wood and bamboo. Planting areas of cotton has been declining and new seedless cultivation of cotton and labor costs have been increased, resulting in the yield of cotton linter declining year by year and price fluctuating wildly. The dissolving pulp used for viscose fibers requires high a-cellulose content, low pentosan content, scilicet the fiber is high purity, so hemicellulose especially xylan in the raw materials must be removed in the production of dissolving pulp, because of the interfere with the viscose production process with higher chemical consumption. In order to remove hemicellulose better and reduce the degradation of cellulose, there is one more hydrolysis process before the cooking in existing process, scilicet prehydrosis kraft method or sulfite multi-stage cooking. It mainly uses inorganic acid as a catalyst, intermittent cooking in multi-stage cooking process at home and abroad. Due to the application of inorganic acid, the degradation of cellulose is relatively stronger in the high temperature, the degree of polymerization will be impacted significantly. And the process of prehydrolysis has the higher requirement for the device corrosion resistance. The intermittent hydrolysis and cooking process includes:
    I
    filling, steam heating, the prehydrolysis reaction, cooking. And the intermittent production methods can not maintain continuous production, influencing the efficiency of production. SUMMARY OF THE INVENTION The present invention provides a production process of dissolving pulp from eucalyptus against the above shortcomings. The process uses eucalyptus as raw material to expand the sources of raw materials. And it uses acid-free continuous prehydrolysis and continuous cooking, improving the production efficiency. The present invention is achieved through the following technical solutions: A production process of dissolving pulp from eucalyptus includes the following steps: a: Select eucalyptus wood chips and pre-steaming; b: In accordance with the mass ratio of eucalyptus wood chips and water is 1:3 to 1:10, the aqueous solution of eucalyptus wood chips will be entered continuous hydrolysis tower from the top of the hydrolysis tower with a pump, with the time of hydrolysis reaction of 1-4h, the temperature of 120 C to 180'C, hydrolyzate is extracted from the bottom of the hydrolysis tower; c. The next step is kraft cooking process, with conditions as follows: Feeding the eucalyptus wood chips after hydrolysis with constant speed into the top of the digester; Effective alkali is 16-24% as NaOH basis and based on the oven dry weight of eucalyptus wood chips, the sulfidity is 20-40%; Cooking temperature of 140-170'C; Mass ratio of eucalyptus wood chips and water of 1:3 to 1:10; And cooking time of 1-4h. The requirements for eucalyptus wood chips are: length 25-40mm, width 20-30mm, and thickness 5 mm. A production process of dissolving pulp from eucalyptus above-mentioned includes the following steps: a: Select eucalyptus wood chips and pre-steaming; b: In accordance with the mass ratio of eucalyptus wood chips and water is 1:4 to 1:8, the aqueous solution of eucalyptus wood chips will be entered continuous 2 hydrolysis tower from the top of the hydrolysis tower with pumps, with the time of hydrolysis reaction of 2-3h, the temperature of 130'C to 170'C, hydrolyzate is extracted from the bottom of the hydrolysis tower; c: The next step is kraft cooking process, with conditions as follows: Feeding the eucalyptus wood chips after hydrolysis with constant speed into the top of the digester; Effective alkali is 18-22% as NaOH basis and based on the oven dry weight of eucalyptus wood chips, the sulfidity is 25-35%; Cooking temperature of 150-160'C; Mass ratio of eucalyptus wood chips and water of 1:3 to 1:5; And cooking time of 2-3h. A production process of dissolving pulp from eucalyptus above-mentioned includes the following steps: a: Select eucalyptus wood chips and pre-steaming; b: In accordance with the mass ratio of eucalyptus wood chips and water is 1:4, the aqueous solution of eucalyptus wood chips will be entered continuous hydrolysis tower from the top of the hydrolysis tower with pumps, with the time of hydrolysis reaction of 2.5h, the temperature of 170'C, hydrolyzate is extracted from the bottom of the hydrolysis tower; c: The next step is kraft cooking process,with conditions as follows: Feeding the eucalyptus wood chips after hydrolysis with constant speed into the top of the digester; Effective alkali is 20% as NaOH basis and based on the oven dry weight of eucalyptus wood chips, the sulfidity is 28%; Cooking temperature of 150'C; Mass ratio of eucalyptus wood chips and water of 1:3.5; And cooking time of 3h. The beneficial effects of the present invention are as follows: 1. The technology of continuous prehydrolysis kraft cooking with less investment, high production efficiency, and simply process, easily operation; 2. The hydrolysis process without acid reduces degradation of cellulose and corrosion of equipment from inorganic acid; 3. The quality and property of eucalyptus dissolving pulp are more stable, and the content of alpha-cellulose is up to 9 6
    .
    2 %, the content of pentosan is 2
    .
    3 5 %. DESCRIPTION OF THE PREFERRED EMBODIMENTS 3 The present invention will be described below in further detail with reference to the following examples, for better understanding by technical staff in this field, but not to be intended to limit the present invention. Example 1 A production process of dissolving pulp from eucalyptus includes the following steps: Eucalyptus wood chips with a length of 30mm, width of 20mm and thickness of 5mm, are fed with constant speed at the top of continuous hydrolysis tower after the pre-steaming. And steam is filled from the top of the hydrolysis tower to maintain the temperature to be 165'C. The ratio of water and eucalyptus wood chips is 5:1. And the reaction time is 2h. Then the hydrolyzate is extracted continuously from the bottom of the hydrolysis tower after pre-hydrolysis. The hydrolysis yield is determined by eucalyptus chips quality before and after hydrolysis Analysis: The yield of pulp is based on the average oven dry eucalyptus wood chips of 75%, so about 25% oven dry eucalyptus wood chips dissoluted in hydrolysis. The yield of pentosan in pre-hydrolyzate is based on oven dry eucalyptus wood chips of 16.2% , equivalently 71% of the pentosan contained in the original oven dry eucalyptus wood chips. Eucalyptus wood chips after hydrolysis will be put into continuous kraft cooking. The cooking conditions are as follows: Eucalyptus wood chips after hydrolysis are fed with constant speed at the top of digester; And steam is filled from the top of the digester to maintain the temperature to be 150'C; Cooking time is 2h; Alkali charging is 18% NaOH; Sulfidity is 28%. Then the pulp is cold blowing into the pulp tower, and the sample taken for analysis detection. Analysis: The total yield of pulp is based on 39% original eucalyptus wood chips, viscosity of 1010ml/g, pentosan content of 2.55%, a-cellulose content of 95.1%, and kappa value of 8.9. Example 2 Eucalyptus wood chips with a length of 30mm, width of 20mm and thickness of 5mm, are fed with constant speed at the top of continuous hydrolysis tower after the 4 pre-steaming. And steam is filled from the top of the hydrolysis tower to maintain the temperature to be 170'C. The ratio of water and eucalyptus wood chips is 4:1. And the reaction time is 2.5h. Then the hydrolyzate is extracted continuously from the bottom of the hydrolysis tower after pre-hydrolysis. The hydrolysis yield is determined by eucalyptus chips quality before and after hydrolysis. Analysis: The yield of pulp is based on the average oven dry eucalyptus wood chips of 73%, so about 27% oven dry eucalyptus wood chips dissoluted in hydrolysis. The yield of pentosan in pre-hydrolyzate is based on oven dry eucalyptus wood chips of 17.6% , equivalently 77.3% of the pentosan contained in the original oven dry eucalyptus wood chips. Eucalyptus wood chips after hydrolysis will be put into continuous kraft cooking. The cooking conditions are as follows: Eucalyptus wood chips after hydrolysis are fed with constant speed at the top of digester. And steam is filled from the top of the digester to maintain the temperature to be 148'C; Cooking time is 2.5h; Alkali charge is 18% NaOH; Sulfidity is 30%. Then the pulp is cold blowing into the pulp tower at the end of the cooking, and the sample taken for analysis detection. Analysis: The total yield of pulp is based on 39% original eucalyptus wood chips, viscosity of 980ml/g, pentosan content of 2
    .
    54 %, a-cellulose content of 9 5
    .
    4 %, and kappa value of 8.7. Example 3 Eucalyptus wood chips with a length of 30mm, width of 20mm and thickness of 5mm, are fed with constant speed at the top of continuous hydrolysis tower after the pre-steaming. And steam is filled from the top of the hydrolysis tower to maintain the temperature to be 120'C. The ratio of water and eucalyptus wood chips is 3:1. And the reaction time is lh.Then the hydrolyzate is extracted continuously from the bottom of the hydrolysis tower after pre-hydrolysis. The hydrolysis yield is determined by eucalyptus chips quality before and after hydrolysis. Analysis: The yield of pulp is based on an average of 84% of the oven dry eucalyptus wood chips, so about 16% oven dry eucalyptus wood chips dissoluted in hydrolysis. The yield of pentosan in pre-hydrolyzate is based on oven dry eucalyptus 5 wood chips of 10.4%, equivalently 45.8% of the pentosan contained in the original oven dry eucalyptus wood chips. Eucalyptus wood chips after hydrolysis will be put into continuous kraft cooking. The cooking conditions are as follows: Eucalyptus wood chips after hydrolysis are fed fed with constant speed at the top of digester. And steam is filled from the top of the digester to maintain the temperature to be 150'C; Cooking time is 3h; Alkali charge is 20% NaOH; Sulfidity is 28%; Then the pulp is cold blowing into the pulp tower at the end of the cooking, and the sample taken for analysis detection. Analysis: The total yield of pulp is based on 42% original eucalyptus wood chips, viscosity of 1100ml/g, pentosan content of 2.98%, a-cellulose content of 93.9%, and kappa value of 9.5. Example 4 Eucalyptus wood chips with a length of 30mm, width of 20mm and thickness of 5mm, are fed with constant speed at the top of continuous hydrolysis tower after the pre-steaming. And steam is filled from the top of the hydrolysis tower to maintain the temperature to be 150'C. The ratio of water and eucalyptus wood chips is 4:1. And the reaction time is 2h. Then the hydrolyzate is extracted continuously from the bottom of the hydrolysis tower after pre-hydrolysis. The hydrolysis yield is determined by eucalyptus chips quality before and after hydrolysis Analysis: The yield of pulp is based on the average oven dry eucalyptus wood chips of 78%, so about 22% oven dry eucalyptus wood chips dissoluted in hydrolysis. The yield of pentosan in pre-hydrolyzate is based on oven dry eucalyptus wood chips of 14
    .
    3 % , equivalently 63% of the pentosan contained in the original oven dry eucalyptus wood chips. Eucalyptus wood chips after hydrolysis will be put into continuous kraft cooking. The cooking conditions are as follows: Eucalyptus wood chips after hydrolysis are fed with constant speed at the top of digester. And steam is filled from the top of the digester to maintain the temperature to be 150'C; Cooking time is 3h; Alkali charge is 20% NaOH; Sulfidity is 28%. Then the pulp is cold blowing into the pulp tower at the end of the cooking, and the sample taken for analysis detection. 6 Analysis: The total yield of pulp is based on 40% original eucalyptus wood chips, viscosity of 1030ml/g, pentosan content of 2.68%, a-cellulose content of 94.9%, and kappa value of 9.0. Example 5 Eucalyptus wood chips with a length of 30mm, width of 20mm and thickness of 5mm, are fed with constant speed at the top of continuous hydrolysis tower after the pre-steaming. And steam is filled from the top of the hydrolysis tower to maintain the temperature to be 170'C. The ratio of water and eucalyptus wood chips is 4:1. And the reaction time is 2.5h. Then the hydrolyzate is extracted continuously from the bottom of the hydrolysis tower after pre-hydrolysis. The hydrolysis yield is determined by eucalyptus chips quality before and after hydrolysis Analysis: The yield of pulp is based on the average oven dry eucalyptus wood chips of 73%, so about 27% oven dry eucalyptus wood chips dissoluted in hydrolysis. The yield of pentosan in pre-hydrolyzate is based on oven dry eucalyptus wood chips of 17.6% , equivalently 7 7
    .
    3 % of the pentosan contained in the original oven dry eucalyptus wood chips. Eucalyptus wood chips after hydrolysis will be put into continuous kraft cooking. The cooking conditions are as follows: Eucalyptus wood chips after hydrolysis are fed with constant speed at the top of digester. And steam is filled from the top of the digester to maintain the temperature to be 150'C; Cooking time is 3h; Alkali charge is 20% NaOH; Sulfidity is 28%. Then the pulp is cold blowing into the pulp tower at the end of the cooking, and the sample taken for analysis detection. Analysis: The total yield of pulp is based on 38% original eucalyptus wood chips, viscosity of 870ml/g, pentosan content of 2
    .
    3 5 %, a-cellulose content of 9 6
    .
    2 %, and kappa value of 8.0. The quality indicators of eucalyptus dissolving pulp produced by the present invention are: a-cellulose: 8 8
    -
    9 6
    .
    2 %, pentosan content: < 3 .0%, the viscosity: 600-1200ml/g. .7
    权利要求:
    Claims (3)
    [1] 1. The method for producing dissolving pulp from eucalyptus, which includes following steps: a: Select eucalyptus wood chips and pre-steaming; b: In accordance with the mass ratio of eucalyptus wood chips and water is 1:3 to 1:10, the aqueous solution of eucalyptus wood chips will be entered continuous hydrolysis tower from the top of the hydrolysis tower with a pump, with the time for hydrolysis reaction of 1-4h, the temperature of 120'C to 180'C. Then the hydrolyzate is extracted from the bottom of the hydrolysis tower; c. The next step is kraft cooking process, with conditions as follows: Feeding the eucalyptus wood chips after hydrolysis with constant speed into the top of the digester; Effective alkali is 16-24% as NaOH basis and based on the oven dry weight of eucalyptus wood chips, the sulfidity is 20-40%; Cooking temperature of 140-170'C; Mass ratio of eucalyptus wood chips and water of 1:3 to 1:10; And cooking time of 1-4h.
    [2] 2. According to claim 1, the features of this method for producing dissolving pulp from eucalyptus lie in : eucalyptus wood chips with length of 25-40mm, width of
    [3] 20-30mm, and thickness of 5 mm. 3. According to claim 1 or 2, the features of this method for producing dissolving pulp from eucalyptus lie in the following steps: a: Select eucalyptus wood chips and pre-steaming; b: In accordance with the mass ratio of eucalyptus wood chips and water is 1:4 to 1:8, the aqueous solution of eucalyptus wood chips will be entered continuous hydrolysis tower from the top of the hydrolysis tower with a pump, with the time of hydrolysis reaction of 2-3h, the temperature of 130'C to 170'C, hydrolyzate is extracted from the bottom of the hydrolysis tower; c: The next step is kraft cooking process, with conditions as follows: Feeding the eucalyptus wood chips after hydrolysis with constant speed into the top of the digester; Effective alkali is 18-22% as NaOH basis and based on the oven dry weight of eucalyptus wood chips, the sulfidity is 25-35%; Cooking temperature of 150-160'C; Mass ratio of eucalyptus wood chips and water of 1:3 to 1:5, and cooking time of 2-3h. 4. According to claim 1 or 2, the features of this method for producing dissolving pulp from eucalyptus feature lie in the following steps: a: Select eucalyptus wood chips and pre-steaming; I b: In accordance with the mass ratio of eucalyptus wood chips and water is 1:4, the aqueous solution of eucalyptus wood chips will be entered continuous hydrolysis tower from the top of the hydrolysis tower with a pump, with the time of hydrolysis reaction of 2.5h, the temperature of 170'C, hydrolyzate is extracted from the bottom of the hydrolysis tower; c: The next step is kraft cooking process, with conditions as follows: Feeding the eucalyptus wood chips after hydrolysis with constant speed into the top of the digester; Effective alkali is 20% as NaOH basis and based on the oven dry weight of eucalyptus wood chips, the sulfidity is 28%; Cooking temperature of 150'C; Mass ratio of eucalyptus wood chips and water of 1:3.5; And cooking time of 3h. 2
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    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    CN1099501C|1999-09-21|2003-01-22|中国科学院广州化学研究所|Pulping technology by dissolving eucalyptus|
    DE10109502A1|2001-02-28|2002-09-12|Rhodia Acetow Gmbh|Removal of hemicellulose from biomaterial, especially wood pulp, involves extraction by treatment with an aqueous solution of metal complex, e.g. nickel tris-2-aminoethyl-amine di-hydroxide|
    JP4192565B2|2002-11-19|2008-12-10|日本製紙株式会社|Method for producing high whiteness bleached kraft pulp|
    NZ598528A|2007-08-31|2013-08-30|Vertichem Corp|Lignin and other products isolated from plant material, and methods and compositions therefor|
    CN101748630B|2009-12-14|2012-10-17|昆明理工大学|Acid-free pre-hydrolysis enzymolysis-free method for preparing bamboo pulp of Dendrocalamus giganteus Munro series|
    CN102587179B|2012-03-08|2014-10-22|山东太阳纸业股份有限公司|Preparation process for eucalyptus dissolving pulp|CN105442367B|2015-12-06|2017-06-20|东莞玖龙纸业有限公司|A kind of preparation technology and processing system of paper gradewood powder|
    KR102264268B1|2019-11-06|2021-06-10|충남대학교산학협력단|Manufacturing method of pillow covers that is eco-friendly|
    法律状态:
    2016-06-02| FGA| Letters patent sealed or granted (standard patent)|
    优先权:
    申请号 | 申请日 | 专利标题
    CN201210088433.8||2012-03-30||
    CN201210088433.8A|CN102587179B|2012-03-08|2012-03-30|Preparation process for eucalyptus dissolving pulp|
    PCT/CN2012/001746|WO2013143047A1|2012-03-30|2012-12-28|Preparation process of eucalyptus dissolving pulp|
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