硫酸盐竹浆制备人纤浆的研究
摘要
黏胶纤维的发展一直备受关注。长期以来,黏胶纤维的生产原料主要来自棉浆粕及木浆粕。众所周知,现今森林资源匮乏,而棉花产量锐减,造成了浆粕生产原料供不应求,黏胶纤维的生产企业生存发展受到威胁。因此,合理开发利用竹材制备人纤浆粕具有重要意义:一方面为粘胶纤维的生产原料开辟了新渠道,促进竹子产业化发展;另一方面也可进一步提高纺织产业的核心竞争力。
竹子在我国具有种植面积广、种类繁多、蓄积量大等特点,且生长周期短,种植3-5即可成林砍伐,可满足于粘胶纤维生产企业的原料需求。竹材纤维细长,纤维素含量接近木材,是制备人纤浆的优质原料。
本论文以福建省资源丰富的麻竹为原料,通过硫酸盐法制浆(KP),两段氧脱木素(OO)、木聚糖酶处理(X)、二氧化氯漂白(D)、碱处理(E)、酸处理(A)的无元素氯(ECF)漂白工艺制备出适用于黏胶纤维生产的高级溶解浆。论文对两段氧脱木素、木聚糖酶处理、二氧化氯漂白、冷碱处理、酸处理工艺进行优化;并对漂白过程中溶解浆化学组成、纤维形态及超分子结构进行了表征。
结果表明:(一)两段氧脱木素最佳工艺条件为:一段,NaOH用量3.0%、氧压0.9MPa、温度80℃、时间40min、MgSO40.5%、浆浓10%;二段,NaOH用量2.0%、氧压0.3MPa、温度100℃、时间60min、MgSO40.5%、浆浓10%。在此优化条件下的浆料性能:聚戊糖12.68%,α-纤维素90.83%,卡伯值7.2,白度44.2%ISO,黏度44.55mPa.s,灰分1.28%;(二)木聚糖酶处理最佳工艺条件为:酶用量127.2IU.g-1,浆浓4%,时间40min, pH值9.0,温度55℃。在此优化条件下的浆料性能是:聚戊糖13.77%,α-纤维素87.58%,白度87.74%ISO,黏度17.96mPa.s,灰分0.133%;(三)二氧化氯漂白最优工艺为:ClO2用量1.52%,NaOH用量0.76%,温度75℃,浆浓10%,时间120min。在此优化条件下的浆料性能:聚戊糖12.96%,α-纤维素93.92%,卡伯值1.34,白度76.9%ISO,黏度36.34mPa.s,灰分0.76%;(四)碱处理优化后的工艺为:用碱量10.0%,温度60℃,时间60min,浆浓10%。在此优化条件下的浆料性能为:聚戊糖8.80%,α-纤维素92.80%,卡伯值4.6,白度59.0%ISO,黏度14.15mPa.s,灰分0.45%;(五)酸处理优化后的工艺为:pH值3.0,温度50℃,时间30min,浆浓5%,DTPA用量0.5%。在此优化条件下的浆料性能:聚戊糖14.86%,α-纤维素86.45%,白度88.6%ISO,黏度11.41mPa.s,灰分0.013%。
硫酸盐竹浆经无元素氯漂白后,α-纤维素含量为95.19%,满足人纤浆粕要求,且聚戊糖降至6.52%、灰分有效降低至0.14%,白度提高至86.8%ISO,黏度下降至11.80mPa.s。氧脱木素、二氧化氯漂白能够高效的除去浆中的木素,木素下降率分别是62.5%、69.6%。X-ray分析结果表明,氧脱木素及漂白处理后竹浆粕晶型结构未发生改变,属于纤维素Ⅰ型;在KP-OO-X-D1-E处理的过程中,随着半纤维素、木素、树脂、果胶等杂质的除去,纤维素结晶度由59.77%提高至70.26%。
Recently, the development and utilization of bamboo materials has attracted great attention as the most abundant renewable biomass materials which can be used in viscose fiber production, Although, the cotton linters and wood pulp have been used as starting materials for production of viscose fiber for long time; nowadays, the shortage of cotton linters and wood materials puts the factory at the severe status. Consequently, research and development of bamboo pulp as viscose fiber materials could not only open a new way to produce cellulosic fiber, but also play a significant role in solving the wood fiber shortage problem and also improve the viscose fiber production technology and product quality.
As an abundant resource in China, bamboo has been used as an important raw material for production of viscose fiber for its unique characteristics, such as long fiber length, higher cellulose content which is close to wood materials.
In this paper, Dendrocalamus latiflorus Mnuro, which is abundant in Fujian province, was used as raw material to prepare high quality dissolving pulp by Kraft pulping and OO-X-D-E-A bleaching processes. Each bleaching stage was optimized and thus to produce high quality dissolving pulp.The two-stage oxygen delignification process was studied. The results showed that, the optimum conditions of two-stage oxygen delignification were as followed: NaOH consumption 3.0%, oxygen pressure 0.9MPa, temperature 60℃, reaction time 40min, MgSO4 consumption 0.5%, consistency 10% and NaOH consumption 2.0% , oxygen pressure 0.3MPa, temperature 100℃, reaction time 60min, MgSO4 consumption 0.5%, consistency 10%. The pulp properties under these optimum conditions were as followed: pentosan content 12.68%,α-cellulose content 90.83%, kappa number 7.2, brightness 44.2%ISO, viscosity 44.55mPa.s, ash content 1.28%. The enzyme treatment process was studied. The results showed that, the optimum parameters of enzyme treatment process were as followed: enzyme dosage 127.2IU.g-1, consistency of 4%, reaction time 30min, pH 9.0, reaction temperature 55℃. The pulp properties under these optimum conditions were as followed: pentosan content 13.77%,α-cellulose content 87.58%, brightness 87.74%ISO, viscosity 17.96mPa.s, ash content 0.133%. The chlorine dioxide bleaching process was studied. The results showed that, the optimum parameters of chlorine dioxide bleaching process were as followed: 1.52% of ClO2 consumption, 0.76% of NaOH consumption, reaction temperature 75℃, consistency of 10%, reaction time 30min. The pulp properties under these optimum conditions were as followed: pentosan content 12.96%,α-cellulose content 93.92%, kappa number 1.34, brightness 76.9%ISO, viscosity36.34mPa.s, ash content 0.76%. The alkaline treatment process was studied. The results showed that, the optimum parameters of alkaline treatment process were as followed: 10.0% of NaOH consumption, reaction temperature 60℃, reaction time 60min, consistency of 10%. The pulp properties under these optimum conditions were as followed: pentosan content 8.80%,α-cellulose content 92.80%, kappa number 4.6, brightness 59.0%ISO, viscosity14.15mPa.s, ash content 0.45%. The acid treatment process was studied. The results showed that, the optimum parameters of acid treatment process were as followed: pH 3.0, reaction temperature 30℃, reaction time 30min, consistency of 5%, 0.5% of DTPA consumption. The pulp properties under these optimum conditions were as followed: pentosan content 14.86%,α-cellulose content 86.45%, brightness 88.6%ISO, viscosity14.41mPa.s, ash content 0.013%.
The mechanism of dissolving pulp from Bamboo Kraft Pulp was shown. Bamboo Kraft Pulp upgraded to dissolving pulp by the Elemental Chlorine Free Bleaching stage.α-cellulose content reached 95.19% after bleaching and purification, which met the satisfaction of dissolving pulp production. And the pentosan content reduced to 6.52%、ash content dropped to 0.14%, brightness raised to 86.8%ISO, viscosity fell to 11.80mPa.s. Oxygen delignifation, chlorine dioxide bleaching were the high active delignification treatments, lignin reduction ratio 62.5% and 69.6%. The results of FT-IR and X-ray revealed that, characteristic absorption peaks about bamboo pulp fiber were belong to the typical absorption in cellulose; there was no crystalline transformation of the crystalline structure in the treated samples and showed cellulose I structure. After E bleaching, the degree of crystallization was up from 59.77% to 70.26%, indicated that hemicellulose, lignin, colophony, pectine and other amorphous materials were gradually removal.
竹子在我国具有种植面积广、种类繁多、蓄积量大等特点,且生长周期短,种植3-5即可成林砍伐,可满足于粘胶纤维生产企业的原料需求。竹材纤维细长,纤维素含量接近木材,是制备人纤浆的优质原料。
本论文以福建省资源丰富的麻竹为原料,通过硫酸盐法制浆(KP),两段氧脱木素(OO)、木聚糖酶处理(X)、二氧化氯漂白(D)、碱处理(E)、酸处理(A)的无元素氯(ECF)漂白工艺制备出适用于黏胶纤维生产的高级溶解浆。论文对两段氧脱木素、木聚糖酶处理、二氧化氯漂白、冷碱处理、酸处理工艺进行优化;并对漂白过程中溶解浆化学组成、纤维形态及超分子结构进行了表征。
结果表明:(一)两段氧脱木素最佳工艺条件为:一段,NaOH用量3.0%、氧压0.9MPa、温度80℃、时间40min、MgSO40.5%、浆浓10%;二段,NaOH用量2.0%、氧压0.3MPa、温度100℃、时间60min、MgSO40.5%、浆浓10%。在此优化条件下的浆料性能:聚戊糖12.68%,α-纤维素90.83%,卡伯值7.2,白度44.2%ISO,黏度44.55mPa.s,灰分1.28%;(二)木聚糖酶处理最佳工艺条件为:酶用量127.2IU.g-1,浆浓4%,时间40min, pH值9.0,温度55℃。在此优化条件下的浆料性能是:聚戊糖13.77%,α-纤维素87.58%,白度87.74%ISO,黏度17.96mPa.s,灰分0.133%;(三)二氧化氯漂白最优工艺为:ClO2用量1.52%,NaOH用量0.76%,温度75℃,浆浓10%,时间120min。在此优化条件下的浆料性能:聚戊糖12.96%,α-纤维素93.92%,卡伯值1.34,白度76.9%ISO,黏度36.34mPa.s,灰分0.76%;(四)碱处理优化后的工艺为:用碱量10.0%,温度60℃,时间60min,浆浓10%。在此优化条件下的浆料性能为:聚戊糖8.80%,α-纤维素92.80%,卡伯值4.6,白度59.0%ISO,黏度14.15mPa.s,灰分0.45%;(五)酸处理优化后的工艺为:pH值3.0,温度50℃,时间30min,浆浓5%,DTPA用量0.5%。在此优化条件下的浆料性能:聚戊糖14.86%,α-纤维素86.45%,白度88.6%ISO,黏度11.41mPa.s,灰分0.013%。
硫酸盐竹浆经无元素氯漂白后,α-纤维素含量为95.19%,满足人纤浆粕要求,且聚戊糖降至6.52%、灰分有效降低至0.14%,白度提高至86.8%ISO,黏度下降至11.80mPa.s。氧脱木素、二氧化氯漂白能够高效的除去浆中的木素,木素下降率分别是62.5%、69.6%。X-ray分析结果表明,氧脱木素及漂白处理后竹浆粕晶型结构未发生改变,属于纤维素Ⅰ型;在KP-OO-X-D1-E处理的过程中,随着半纤维素、木素、树脂、果胶等杂质的除去,纤维素结晶度由59.77%提高至70.26%。
Recently, the development and utilization of bamboo materials has attracted great attention as the most abundant renewable biomass materials which can be used in viscose fiber production, Although, the cotton linters and wood pulp have been used as starting materials for production of viscose fiber for long time; nowadays, the shortage of cotton linters and wood materials puts the factory at the severe status. Consequently, research and development of bamboo pulp as viscose fiber materials could not only open a new way to produce cellulosic fiber, but also play a significant role in solving the wood fiber shortage problem and also improve the viscose fiber production technology and product quality.
As an abundant resource in China, bamboo has been used as an important raw material for production of viscose fiber for its unique characteristics, such as long fiber length, higher cellulose content which is close to wood materials.
In this paper, Dendrocalamus latiflorus Mnuro, which is abundant in Fujian province, was used as raw material to prepare high quality dissolving pulp by Kraft pulping and OO-X-D-E-A bleaching processes. Each bleaching stage was optimized and thus to produce high quality dissolving pulp.The two-stage oxygen delignification process was studied. The results showed that, the optimum conditions of two-stage oxygen delignification were as followed: NaOH consumption 3.0%, oxygen pressure 0.9MPa, temperature 60℃, reaction time 40min, MgSO4 consumption 0.5%, consistency 10% and NaOH consumption 2.0% , oxygen pressure 0.3MPa, temperature 100℃, reaction time 60min, MgSO4 consumption 0.5%, consistency 10%. The pulp properties under these optimum conditions were as followed: pentosan content 12.68%,α-cellulose content 90.83%, kappa number 7.2, brightness 44.2%ISO, viscosity 44.55mPa.s, ash content 1.28%. The enzyme treatment process was studied. The results showed that, the optimum parameters of enzyme treatment process were as followed: enzyme dosage 127.2IU.g-1, consistency of 4%, reaction time 30min, pH 9.0, reaction temperature 55℃. The pulp properties under these optimum conditions were as followed: pentosan content 13.77%,α-cellulose content 87.58%, brightness 87.74%ISO, viscosity 17.96mPa.s, ash content 0.133%. The chlorine dioxide bleaching process was studied. The results showed that, the optimum parameters of chlorine dioxide bleaching process were as followed: 1.52% of ClO2 consumption, 0.76% of NaOH consumption, reaction temperature 75℃, consistency of 10%, reaction time 30min. The pulp properties under these optimum conditions were as followed: pentosan content 12.96%,α-cellulose content 93.92%, kappa number 1.34, brightness 76.9%ISO, viscosity36.34mPa.s, ash content 0.76%. The alkaline treatment process was studied. The results showed that, the optimum parameters of alkaline treatment process were as followed: 10.0% of NaOH consumption, reaction temperature 60℃, reaction time 60min, consistency of 10%. The pulp properties under these optimum conditions were as followed: pentosan content 8.80%,α-cellulose content 92.80%, kappa number 4.6, brightness 59.0%ISO, viscosity14.15mPa.s, ash content 0.45%. The acid treatment process was studied. The results showed that, the optimum parameters of acid treatment process were as followed: pH 3.0, reaction temperature 30℃, reaction time 30min, consistency of 5%, 0.5% of DTPA consumption. The pulp properties under these optimum conditions were as followed: pentosan content 14.86%,α-cellulose content 86.45%, brightness 88.6%ISO, viscosity14.41mPa.s, ash content 0.013%.
The mechanism of dissolving pulp from Bamboo Kraft Pulp was shown. Bamboo Kraft Pulp upgraded to dissolving pulp by the Elemental Chlorine Free Bleaching stage.α-cellulose content reached 95.19% after bleaching and purification, which met the satisfaction of dissolving pulp production. And the pentosan content reduced to 6.52%、ash content dropped to 0.14%, brightness raised to 86.8%ISO, viscosity fell to 11.80mPa.s. Oxygen delignifation, chlorine dioxide bleaching were the high active delignification treatments, lignin reduction ratio 62.5% and 69.6%. The results of FT-IR and X-ray revealed that, characteristic absorption peaks about bamboo pulp fiber were belong to the typical absorption in cellulose; there was no crystalline transformation of the crystalline structure in the treated samples and showed cellulose I structure. After E bleaching, the degree of crystallization was up from 59.77% to 70.26%, indicated that hemicellulose, lignin, colophony, pectine and other amorphous materials were gradually removal.
引文
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