CN116607344A - High-yield bamboo cellulose preparation method - Google Patents

High-yield bamboo cellulose preparation method Download PDF

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Publication number
CN116607344A
CN116607344A CN202310713755.5A CN202310713755A CN116607344A CN 116607344 A CN116607344 A CN 116607344A CN 202310713755 A CN202310713755 A CN 202310713755A CN 116607344 A CN116607344 A CN 116607344A
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bamboo
contact
cellulose
preparation
yield
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徐鼎峰
凌素芬
罗诗红
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Gannan Normal University
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Gannan Normal University
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    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21HPULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H11/00Pulp or paper, comprising cellulose or lignocellulose fibres of natural origin only
    • D21H11/12Pulp from non-woody plants or crops, e.g. cotton, flax, straw, bagasse
    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21CPRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C1/00Pretreatment of the finely-divided materials before digesting
    • D21C1/04Pretreatment of the finely-divided materials before digesting with acid reacting compounds
    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21CPRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C3/00Pulping cellulose-containing materials
    • D21C3/02Pulping cellulose-containing materials with inorganic bases or alkaline reacting compounds, e.g. sulfate processes

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  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Polysaccharides And Polysaccharide Derivatives (AREA)

Abstract

The application relates to the technical field of bamboo cellulose, in particular to a preparation method of high-yield bamboo cellulose. The method comprises the following steps: (1) Carrying out first contact on the bamboo material and the acid liquor to obtain a bamboo material product; (2) Carrying out at least one second contact on the bamboo product obtained in the step (1) and alkali liquor, washing and drying to obtain bamboo cellulose; the bamboo is moso bamboo with the bamboo age of 15-180 days; the second contact conditions include: the temperature is 60-80 ℃ and the time is 4-8h. By adopting the moso bamboo with the bamboo age within 6 months and combining the preparation method, the high fiber yield can be achieved by only simple acid treatment and alkali treatment, the quality of the bamboo cellulose can be controlled under mild conditions, the yield can be up to 51.3%, and the alpha-cellulose of the prepared bamboo cellulose can reach 90.08%.

Description

High-yield bamboo cellulose preparation method
Technical Field
The application relates to the technical field of bamboo cellulose, in particular to a preparation method of high-yield bamboo cellulose.
Background
Cellulose is a renewable natural polymer with the most abundant reserves on earth, is mainly derived from biomass, and is a main component of plant cell walls. The bamboo is rich in cellulose, and the content of the bamboo can reach 40-60% according to different ages of bamboo. China has rich bamboo resources, the area of the bamboo forest is 641.16 ten thousand hectares, and the area of the bamboo forest accounts for one third of the total area of the world, and has the reputation of bamboo kingdom. The bamboos are more than 700 species, wherein 467.78 ten thousand hectares of the phyllostachys pubescens occupy 72.96 percent of the area of the phyllostachys pubescens. In the cellulose extraction process, the cellulose in the bamboo plants is mostly medium and long fibers, and the quality of the bamboo cellulose is equivalent to or even better than that of conifer wood from the analysis of fiber morphology and chemical components. Therefore, developing cellulose dissolving pulp prepared from bamboo is an effective way to solve the problems of insufficient dissolving pulp and wood resource shortage in China. The method takes the bamboo as the second forest resource in the world as the raw material, develops a green new technology of bamboo pulp papermaking, realizes controllable quality of bamboo cellulose, is an effective way for realizing 'taking bamboo as a substitute for wood', and is also a sustainable development way of domestic pulping papermaking industry.
However, due to the fact that the bamboo wood contains more miscellaneous cells (20-50%), the wall thickness of fiber cells and the wall cavity ratio is small, the digestion time is long, the conditions are harsh, the yield of the prepared cellulose is low in the cellulose extraction process, and the impurity removal, refining and purification are difficult. Thus, the bamboo cellulose only accounts for about 2% of the total domestic pulping consumption. Therefore, the separation, extraction and functional modification of the bamboo cellulose are one of effective ways for developing high-added-value bamboo products and improving the technical content and market competitiveness of the bamboo products.
Bamboo cellulose has excellent performance and wide application prospect, and many scientific researchers have conducted related researches on the bamboo cellulose. Liu Yishan and the like, the bleached sulfate bamboo pulp is taken as a raw material, a Baol screening instrument is used for screening to remove the miscellaneous cell components, then the purity of the bleached sulfate bamboo pulp is further improved through hydrolysis treatment and cold alkali refining, and the alpha-cellulose of the obtained bamboo cellulose reaches 95.91 percent, so that the requirements of high-purity dissolving pulp (Paper and Paper Making Vol.39No.6Nov 2020) can be met. CN107988643B, CN101565906A, CN110965382A, CN111021123B et al propose a method for extracting bamboo cellulose. However, the existing bamboo cellulose extraction methods are not designed with control technology and method of cellulose yield, and most of the existing bamboo cellulose extraction methods need complex technologies such as sulfate digestion, bleaching and the like, and in addition, special high-temperature and high-pressure equipment is needed, so that the extraction efficiency is low, and the cost performance of the bamboo cellulose extraction methods is difficult to improve.
Disclosure of Invention
The application aims to provide a preparation method of high-yield bamboo cellulose, which adopts moso bamboos with the age of 6 months, and the yield of the bamboo cellulose can reach 51.3 percent by combining the preparation method of the application, and the alpha-cellulose content in the prepared bamboo cellulose can reach 90.08 percent.
In order to achieve the above object, according to one aspect of the present application, there is provided a method for preparing high yield bamboo cellulose, comprising:
(1) Carrying out first contact on the bamboo material and the acid liquor to obtain a bamboo material product;
(2) Carrying out at least one second contact on the bamboo product obtained in the step (1) and alkali liquor, washing and drying to obtain bamboo cellulose;
the bamboo is moso bamboo with the bamboo age of 15-180 days;
the second contact conditions include: the temperature is 60-80 ℃ and the time is 4-8h.
According to the technical scheme, the moso bamboo with the bamboo age within 6 months is adopted, and the preparation method provided by the application is combined, so that the high fiber yield can be achieved only by simple acid treatment and alkali treatment, the quality of the bamboo cellulose can be controlled under mild conditions, the yield can be up to 51.3%, and the prepared bamboo cellulose alpha-cellulose can reach 90.08%.
Drawings
FIG. 1 is an infrared spectrum of a bamboo fiber sample prepared in examples 1-3;
fig. 2 is an external view of a bamboo fiber sample prepared in example 1;
fig. 3 is an external view of a bamboo fiber sample prepared in example 2;
fig. 4 is an external view of a bamboo fiber sample prepared in example 3.
Detailed Description
The endpoints and any values of the ranges disclosed herein are not limited to the precise range or value, and are understood to encompass values approaching those ranges or values. For numerical ranges, one or more new numerical ranges may be found between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point value, in combination with each other, and are to be considered as specifically disclosed herein.
In the application, the age of the bamboo material refers to: the bamboo shoots are taken out of the soil until they are cut.
The application provides a preparation method of high-yield bamboo cellulose, which comprises the following steps:
(1) Carrying out first contact on the bamboo material and the acid liquor to obtain a bamboo material product;
(2) Carrying out at least one second contact on the bamboo product obtained in the step (1) and alkali liquor, washing and drying to obtain bamboo cellulose;
the bamboo is moso bamboo with the bamboo age of 15-180 days;
the second contact conditions include: the temperature is 60-80 ℃ and the time is 4-8h. By adopting the moso bamboo with the bamboo age within 6 months and combining the preparation method, the high fiber yield can be achieved by only simple acid treatment and alkali treatment, the quality of the bamboo cellulose can be controlled under mild conditions, the yield can be up to 51.3%, and the alpha-cellulose of the prepared bamboo cellulose can reach 90.08%.
In the present application, the conditions of the first contact are wide in the optional range, and according to a preferred embodiment of the present application, the conditions of the first contact include: the temperature is 15-40 ℃ and the time is 4-8h.
According to a preferred embodiment of the application, after the first contact and the second contact, the bamboo is washed to neutrality.
According to a preferred embodiment of the application, the bamboo is moso bamboo with the age of 10-90 days, which is beneficial to further improving the yield of bamboo cellulose and improving the alpha cellulose content of the bamboo cellulose.
According to a preferred embodiment of the application, the acid liquor has a mass concentration of 4-8wt%; in the acid liquid, the acid is at least one selected from hydrochloric acid and sulfuric acid.
According to a preferred embodiment of the application, the alkaline liquor has a mass concentration of 4-8 wt.%; in the alkaline solution, the base is selected from alkali metal hydroxide and/or alkaline earth metal hydroxide.
According to a preferred embodiment of the application, the base is selected from sodium hydroxide and/or potassium hydroxide.
In the application, the mass ratio of the bamboo wood to the acid liquor is wider in the optional range, and according to a preferred embodiment of the application, the mass ratio of the bamboo wood to the acid liquor is 1:8-20.
In the application, the mass ratio of the bamboo wood to the alkali liquor is wider in optional range, and according to a preferred embodiment of the application, the mass ratio of the bamboo wood to the alkali liquor is 1:5-15.
According to a preferred embodiment of the application, the bamboo product obtained in step (1) is subjected to 1-4 second contacts with alkali liquor.
According to a preferred embodiment of the application, the bamboo product obtained in step (1) is subjected to 3 second contacts with alkali liquor.
According to a preferred embodiment of the application, the 1 st second contact is carried out with a lye mass concentration of 6 to 8 wt.%.
According to a preferred embodiment of the application, the second contact is 2 nd, the concentration of lye is 5-6wt%.
According to a preferred embodiment of the application, the mass concentration of the lye is 4-5 wt.% in the 3 rd second contact.
According to a preferred embodiment of the application, the temperature of the 1 st second contact is 80-90℃for a period of 6-8 hours.
According to a preferred embodiment of the application, the temperature of the second contact 2 is 60-80℃for a period of 6-8 hours.
According to a preferred embodiment of the application, the temperature of the 3 rd second contact is 60-80 ℃ for 4-8 hours.
The present application is further illustrated by the following examples, which are not to be construed as limiting the scope of the application in any way.
The content testing methods of cellulose, hemicellulose and lignin are respectively determined according to the determination of cellulose (the ethanol nitrate method), the determination of pentose (the tetrabromo method) and the determination method of chemical pulp lignin in pulping and papermaking inspection technology.
The method for calculating the yield of the bamboo fiber comprises the following steps: omega Yield rate =(m 1 /m 2 ) 100% of formula m 2 Is the mass of the starting materials; m is m 1 The quality of the sample after the sample is dried.
In the following examples, the source of tender phyllostachys praecox is the autonomous felling phyllostachys praecox; the bamboo age is 30-35 days.
Example 1
(1) Pulverizing tender Phyllostachys Pubescens, oven drying, mixing with 5wt% hydrochloric acid aqueous solution at solid-liquid mass ratio of 1:10, and stirring at room temperature for 6 hr.
(2) Washing the product obtained in the step (1) to be neutral, mixing the product with a sodium hydroxide aqueous solution with the mass fraction of 5wt% in a solid-liquid mass ratio of 1:10, heating to 60 ℃, preserving heat and stirring for 7 hours. And washing with deionized water to neutrality and drying to obtain bamboo fiber.
The resulting bamboo fiber sample is shown in fig. 2. The yield of the bamboo cellulose is 51.3%.
The contents of alpha-cellulose, hemicellulose and lignin in the obtained bamboo fiber are shown in table 1.
Example 2
(1) Pulverizing tender Phyllostachys Pubescens, oven drying, mixing with 5wt% hydrochloric acid aqueous solution at solid-liquid mass ratio of 1:10, and stirring at low speed at room temperature for 7 hr.
(2) Washing the sample obtained in the step (1) to be neutral, mixing the sample with a sodium hydroxide aqueous solution with the mass fraction of 5wt% in a solid-liquid mass ratio of 1:10, heating to 60 ℃, preserving heat and stirring for 7 hours, and washing the sample with deionized water to be neutral;
(3) Mixing the product obtained in the step (2) with a sodium hydroxide aqueous solution with the mass fraction of 5wt% at a solid-liquid mass ratio of 1:10, heating to 60 ℃, preserving heat and stirring for 7 hours. Finally, deionized water is used for washing to be neutral and drying is carried out, thus obtaining the bamboo fiber.
The obtained bamboo fiber sample is shown in FIG. 3, and its infrared spectrum is shown in FIG. 1, which shows 1730cm -1 There is a distinct peak due to C=O stretching vibration with hemicellulose and lignin, 1730cm after 2 alkali treatments -1 The peak intensity was significantly reduced, indicating that hemicellulose and lignin were further removed after further alkali treatment.
The yield of the bamboo cellulose is 45.5%.
The contents of cellulose, hemicellulose and lignin in the obtained bamboo fiber are shown in table 1.
Example 3
(1) Pulverizing tender Phyllostachys Pubescens, oven drying, mixing with 5wt% hydrochloric acid aqueous solution at solid-liquid mass ratio of 1:10, and stirring at low speed at room temperature for 7 hr;
(2) Washing the sample obtained in the step (1) to be neutral, uniformly mixing the sample with a sodium hydroxide aqueous solution with the mass fraction of 5wt% in a solid-liquid ratio of 1:10, heating to 60 ℃, preserving heat and stirring for 7 hours; washing with deionized water to neutrality after completion;
(3) Mixing the product obtained in the step (2) with a sodium hydroxide aqueous solution with the mass fraction of 5wt% at a solid-liquid mass ratio of 1:10, heating to 60 ℃, preserving heat and stirring for 7 hours, and finally washing with deionized water to be neutral;
(4) Mixing the product obtained in the step (3) with 5wt% sodium hydroxide aqueous solution according to a solid-liquid mass ratio of 1:10, heating to 60 ℃, preserving heat and stirring for 7 hours.
Finally, deionized water is used for washing to be neutral, and the bamboo fiber is obtained after drying.
The obtained bamboo fiber sample is shown in FIG. 4, and its infrared spectrum is shown in FIG. 1, which shows that the sample is about 1730cm -1 There is a distinct peak due to C=O stretching vibration with hemicellulose and lignin, 1730cm after 3 alkali treatments -1 The peak intensity was significantly reduced, indicating that hemicellulose and lignin were further removed after further alkali treatment.
The yield of the bamboo fiber is 39.8%.
The contents of cellulose, hemicellulose and lignin in the obtained bamboo fiber are shown in table 1.
Example 4
(1) Pulverizing tender Phyllostachys Pubescens, oven drying, mixing with 5wt% hydrochloric acid aqueous solution at solid-liquid mass ratio of 1:10, and stirring at low speed at room temperature for 7 hr;
(2) Washing the sample obtained in the step (1) to be neutral, uniformly mixing the sample with a sodium hydroxide aqueous solution with the mass fraction of 4wt% in a solid-liquid ratio of 1:10, heating to 90 ℃, preserving heat and stirring for 6 hours; washing with deionized water to neutrality after completion;
(3) Mixing the product obtained in the step (2) with a sodium hydroxide aqueous solution with the mass fraction of 6wt% at a solid-liquid mass ratio of 1:10, heating to 70 ℃, preserving heat and stirring for 7 hours, and finally washing with deionized water to be neutral;
(4) Mixing the product obtained in the step (3) with a sodium hydroxide aqueous solution with the mass fraction of 4wt% at a solid-liquid mass ratio of 1:10, heating to 60 ℃, preserving heat and stirring for 6 hours.
Finally, deionized water is used for washing to be neutral, and the bamboo fiber is obtained after drying.
The yield of the bamboo fiber is 39.5%.
Example 5
(1) Pulverizing tender Phyllostachys Pubescens, oven drying, mixing with 5wt% hydrochloric acid aqueous solution at solid-liquid mass ratio of 1:10, and stirring at low speed at room temperature for 7 hr;
(2) Washing the sample obtained in the step (1) to be neutral, uniformly mixing the sample with a sodium hydroxide aqueous solution with the mass fraction of 7wt% in a solid-liquid ratio of 1:10, heating to 90 ℃, preserving heat and stirring for 6 hours; washing with deionized water to neutrality after completion;
(3) Mixing the product obtained in the step (2) with a sodium hydroxide aqueous solution with the mass fraction of 7wt% at a solid-liquid mass ratio of 1:10, heating to 70 ℃, preserving heat and stirring for 7 hours, and finally washing with deionized water to be neutral;
(4) Mixing the product obtained in the step (3) with a 7wt% sodium hydroxide aqueous solution according to a solid-liquid mass ratio of 1:10, heating to 60 ℃, preserving heat and stirring for 6 hours.
Finally, deionized water is used for washing to be neutral, and the bamboo fiber is obtained after drying.
The yield of the bamboo fiber is 39.2%.
Example 6
The method according to example 1 is different in that the source of tender phyllostachys pubescens is the autonomous felling phyllostachys pubescens; the bamboo age was 120-130 days, and the rest was the same as in example 1.
The yield of the bamboo fiber is 43.2%.
The contents of alpha-cellulose, hemicellulose and lignin in the obtained bamboo fiber are shown in table 1.
Comparative example 1
The procedure of example 1 was followed except that the bamboo age was 9 months, and the other conditions were the same as in example 1.
The yield of the bamboo cellulose is 39.4%.
The contents of alpha-cellulose, hemicellulose and lignin in the obtained bamboo fiber are shown in table 1.
TABLE 1
As can be seen from Table 1, the bamboo with a bamboo age of 180 days or less is used, and the preparation method of the application has high yield of bamboo cellulose and high alpha-cellulose content.
In particular, by the preferred embodiment of the present application, as in example 4, a high content of α -cellulose in the bamboo cellulose can be obtained while maintaining a high yield of bamboo cellulose.
The preferred embodiments of the present application have been described in detail above, but the present application is not limited thereto. Within the scope of the technical idea of the application, a number of simple variants of the technical solution of the application are possible, including combinations of the individual technical features in any other suitable way, which simple variants and combinations should likewise be regarded as being disclosed by the application, all falling within the scope of protection of the application.

Claims (10)

1. A preparation method of high-yield bamboo cellulose is characterized by comprising the following steps:
(1) Carrying out first contact on the bamboo material and the acid liquor to obtain a bamboo material product;
(2) Carrying out at least one second contact on the bamboo product obtained in the step (1) and alkali liquor, washing and drying to obtain bamboo cellulose;
the bamboo is moso bamboo with the bamboo age of 15-180 days;
the second contact conditions include: the temperature is 60-80 ℃ and the time is 4-8h.
2. The preparation method according to claim 1, wherein,
the conditions of the first contact include: the temperature is 15-40 ℃ and the time is 4-8h.
3. The preparation method according to claim 1 or 2, wherein,
after the first contact and the second contact, the bamboo materials are washed to be neutral respectively; and/or
The bamboo is moso bamboo with bamboo age of 10-90 days.
4. The preparation method according to claim 1 or 2, wherein,
the mass concentration of the acid liquor is 4-8wt%; in the acid liquid, the acid is at least one selected from hydrochloric acid and sulfuric acid.
5. The preparation method according to claim 1 or 2, wherein,
the mass concentration of the alkali liquor is 4-8wt%; in the alkaline solution, the base is selected from alkali metal hydroxide and/or alkaline earth metal hydroxide.
6. The process according to claim 5, wherein the base is sodium hydroxide and/or potassium hydroxide.
7. The preparation method according to claim 1 or 2, wherein,
the mass ratio of the bamboo wood to the acid liquor is 1:8-20 parts;
the mass ratio of the bamboo wood to the alkali liquor is 1:5-15.
8. The preparation method according to claim 1 or 2, wherein,
and (3) carrying out secondary contact on the bamboo product obtained in the step (1) and alkali liquor for 1-4 times.
9. The preparation method according to claim 8, wherein,
carrying out 3 times of second contact on the bamboo product obtained in the step (1) and alkali liquor; preferably, the method comprises the steps of,
the second contact is carried out for the 1 st time, and the mass concentration of the alkali liquor is 6-8wt%;
the second contact is carried out for the 2 nd time, and the mass concentration of the alkali liquor is 5-6wt%;
and (3) carrying out second contact, wherein the mass concentration of the alkali liquor is 4-5wt%.
10. The preparation method according to claim 8, wherein,
the temperature of the 1 st second contact is 80-90 ℃ and the time is 6-8h;
the temperature of the second contact for the 2 nd time is 60-80 ℃ and the time is 6-8h;
the temperature of the 3 rd second contact is 60-80 ℃ and the time is 4-8h.
CN202310713755.5A 2023-06-15 2023-06-15 High-yield bamboo cellulose preparation method Pending CN116607344A (en)

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Citations (6)

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Publication number Priority date Publication date Assignee Title
CN1390989A (en) * 2002-07-19 2003-01-15 徐奎元 Process for preparing natural bamboo fibres
CN103484948A (en) * 2013-09-11 2014-01-01 昆山市万丰制衣有限责任公司 Technology for extracting bamboo fibers by using caustic soda
JP2017043869A (en) * 2015-08-28 2017-03-02 日本製紙株式会社 Additive for paper making
CN111021123A (en) * 2019-12-11 2020-04-17 北京理工大学 Method for extracting bamboo cellulose by utilizing moso bamboos
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Publication number Priority date Publication date Assignee Title
CN1390989A (en) * 2002-07-19 2003-01-15 徐奎元 Process for preparing natural bamboo fibres
CN103484948A (en) * 2013-09-11 2014-01-01 昆山市万丰制衣有限责任公司 Technology for extracting bamboo fibers by using caustic soda
JP2017043869A (en) * 2015-08-28 2017-03-02 日本製紙株式会社 Additive for paper making
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