CN105568396A - Method combining inorganic alkali pretreatment, steam explosion and organic alkali ultrasonic-microwave detection to prepare cotton stalk bark fiber - Google Patents
Method combining inorganic alkali pretreatment, steam explosion and organic alkali ultrasonic-microwave detection to prepare cotton stalk bark fiber Download PDFInfo
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- CN105568396A CN105568396A CN201510956741.1A CN201510956741A CN105568396A CN 105568396 A CN105568396 A CN 105568396A CN 201510956741 A CN201510956741 A CN 201510956741A CN 105568396 A CN105568396 A CN 105568396A
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01C—CHEMICAL OR BIOLOGICAL TREATMENT OF NATURAL FILAMENTARY OR FIBROUS MATERIAL TO OBTAIN FILAMENTS OR FIBRES FOR SPINNING; CARBONISING RAGS TO RECOVER ANIMAL FIBRES
- D01C1/00—Treatment of vegetable material
Abstract
The invention relates to a method for preparing cotton stalk bark fiber. The method is characterized by including: bringing alkali liquid for steam explosion after cotton stalk bark is pre-treated by inorganic base sodium hydroxide, which is conducive to exposing hemicellulose and lignin in the process of steam explosion; for coarse fiber obtained after steam explosion, further using an organic base tetramethyl ammonium hydroxide solution as a solvent and using an ultrasonic wave-microwave combined method for extraction, separation and washing to further remove impurities like hemicellulose, lignin and pectin exploded during steam explosion while still adhered on the fiber. By using the method, cotton stalk bark fiber suitable for being used in textile industry and composite material industry can be prepared; the method is simple and environment friendly and has an industrialized application prospect, and utilization rate of the cotton stalk bark is increased.
Description
Technical field
The present invention relates to a kind of biomass resource utilization method, especially relate to a kind of inorganic base preliminary treatment, low pressure vapor dodges the quick-fried method preparing cotton stalk hide fiber with organic base ultrasonic-microwave coupling process, belong to biomass resource utilization field.
Background technology
Cotton stalk, as the byproduct of cotton planting, contains cellulose and the non-cellulosic material such as lignin, hemicellulose in its surperficial bast.Cotton stalk skin belongs to renewable resource, its content of cellulose about 40%, extracts the cotton stalk hide fiber being suitable for yarn, composite application, contribute to the value improving cotton crop from cotton stalk skin.At present, most of cotton stalk is burned, causes the significant wastage of biomass resource.So, better exploitation are carried out to cotton stalk bast particularly important.
At present, the patent relating to the utilization of cotton stalk skin mainly contains: patent of invention " a kind of cotton stalk hide fiber cleans Degumming method " (publication number: CN101008108A), adopts the quick-fried method combined with High Temperature High Pressure post processing of sudden strain of a muscle to prepare cotton stalk hide fiber; Patent of invention " a kind of steam explosion and alkali treatment combine and prepare the method for the cotton stalk hide fiber of weaving " (publication number: CN104047063A), steam explosion is first adopted to be separated cotton stalk skin, then process further with potassium hydroxide, finally use hydrogen peroxide bleaching.But adopt inorganic base NaOH to process under high temperature, high concentration, due to NaOH molecular weight, be difficult to control to the separation of fiber, prepared Fiber Aspect Ratio is less than normal, and namely length is partially short.
For head it off, the present invention adopts organic alkali TMAH, and its molecular weight is 91, be greater than the molecular weight 40 of NaOH, mainly to the cotton stalk bark surface action after steam explosion, hemicellulose and the lignin of fiber surface exposure can be removed, play " peeling " and centrifugation.Ultrasonic microwave synergic solvent extraction reaction instrument is combined ultrasonic with microwave technology, achieve the associated treatment of ultrasonic wave and microwave, suitable application area relates to the synthesis of the extraction of Chinese herb medicine active ingredient, organic-inorganic compound, pharmaceutical intermediate and nano material, the exploitation of energy fuel and new forms of energy product thereof, processing procedure has the features such as extraction efficiency is high, the time is short.The present invention is intended to the draw ratio of the cotton stalk hide fiber obtained by raising.
Summary of the invention
For improving the draw ratio of obtained cotton stalk hide fiber, and raising content of cellulose, the technical solution adopted in the present invention is a kind of inorganic base preliminary treatment, low pressure vapor dodges the quick-fried method preparing cotton stalk hide fiber with organic base ultrasonic-microwave Combined Treatment, it is characterized in that, the method comprises following processing step:
1) machine cuts: the cotton stalk skin of drying is cut into the section that 15 ~ 20cm is long.
2) oxygenation pretreatment: cotton stalk skin step (1) obtained is placed in the inorganic base sodium hydroxide solution that solid-to-liquid ratio is 1:30 ~ 1:40, and alkali consumption is 25 ~ 40g/L, and treatment temperature is 60 ~ 80 DEG C, and the processing time is 50 ~ 150min.Inorganic base NaOH molecular weight is 40, fully can penetrate into the fine structure of cotton stalk hide fiber, contributes to isolating the impurity such as hemicellulose in steam explosion process;
3) steam explosion: the pretreated cotton stalk skin of inorganic base does not wash, after circulating water is extruded, load and dodge in quick-fried tank, pass into saturated vapor, make saturated vapor pressure reach 1.5 ~ 2.5MPa, dodge quick-fried instantaneously with 0.0875s after maintaining saturated vapor pressure 60 ~ 300s;
4) extract: the crude fibre obtained after steam explosion is placed in organic base tetramethyl ammonium hydroxide solution, TMAH consumption is 20 ~ 30g/L, solid-to-liquid ratio is 1:30 ~ 1:60, Ultrasonic-microwave synergistic extraction reaction instrument is adopted to extract further, ultrasonic frequency is 25KHZ, and microwave frequency is 2450MHZ, and temperature is 60 ~ 90 DEG C, time is 15 ~ 60min, extracts 2 ~ 3 times.Organic base TMAH ultrasonic-microwave auxiliary under, fully can remove hemicellulose, the lignin impurity on cotton stalk hide fiber surface, make fiber softening.
5) wash: the sample after extraction is washed at normal temperatures.
6) neutralize: adopt mass percent be 10 ~ 36% acetic acid neutralize, cotton stalk hide fiber pH value is adjusted to neutrality;
7) dry: naturally to dry under fiber being placed in room temperature, obtain cotton stalk hide fiber.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the invention will be further described.
Specific embodiment 1: the method for cotton stalk hide fiber is prepared in a kind of inorganic base preliminary treatment, steam explosion, the coupling of organic base ultrasonic-microwave
1) machine cuts: the cotton stalk skin of drying is cut into the section that 15cm is long;
2) oxygenation pretreatment: cotton stalk skin step (1) obtained is placed in the inorganic base sodium hydroxide solution that solid-to-liquid ratio is 1:30, and alkali consumption is 25g/L, and treatment temperature is 70 DEG C, and the processing time is 50min;
3) steam explosion: the pretreated cotton stalk skin of inorganic base does not wash, after being extruded by circulating water, loads and dodges in quick-fried tank, pass into saturated vapor, make saturated vapor pressure reach 1.5MPa, dodges quick-fried instantaneously after maintaining saturated vapor pressure 180s with 0.0875s;
4) extract: the crude fibre obtained after steam explosion is placed in organic base tetramethyl ammonium hydroxide solution, TMAH consumption is 20g/L solid-to-liquid ratio is 1:30, Ultrasonic-microwave synergistic extraction reaction instrument is adopted to extract further, ultrasonic frequency is 25KHZ, microwave frequency is 2450MHZ, temperature is 60 DEG C, and the time is 20min, extracts 2 times;
5) wash: the sample after extraction is washed at normal temperatures;
6) neutralize: adopt mass percent be 20% acetic acid neutralize, cotton stalk hide fiber pH value is adjusted to neutrality;
7) naturally dry under fiber being placed in room temperature, obtain cotton stalk hide fiber.
Specific embodiment 2: the method for cotton stalk hide fiber is prepared in a kind of inorganic base preliminary treatment, steam explosion, the coupling of organic base ultrasonic-microwave
1) machine cuts: the cotton stalk skin of drying is cut into the section that 20cm is long;
2) oxygenation pretreatment: cotton stalk skin step (1) obtained is placed in the inorganic base sodium hydroxide solution that solid-to-liquid ratio is 1:20, and alkali consumption is 40g/L, and treatment temperature is 80 DEG C, and the processing time is 40min;
3) steam explosion: the pretreated cotton stalk skin of inorganic base does not wash, after being extruded by circulating water, loads and dodges in quick-fried tank, pass into saturated vapor, make saturated vapor pressure reach 2.3MPa, dodges quick-fried instantaneously after maintaining saturated vapor pressure 100s with 0.0875s;
4) extract: the crude fibre obtained after steam explosion is placed in organic base tetramethyl ammonium hydroxide solution, TMAH consumption is 25g/L solid-to-liquid ratio is 1:40, Ultrasonic-microwave synergistic extraction reaction instrument is adopted to extract further, ultrasonic frequency is 25KHZ, microwave frequency is 2450MHZ, temperature is 80 DEG C, and the time is 30min, extracts 1 time;
5) wash: the sample after extraction is washed at normal temperatures;
6) neutralize: adopt mass percent be 25% acetic acid neutralize, cotton stalk hide fiber pH value is adjusted to neutrality;
7) naturally dry under fiber being placed in room temperature, obtain cotton stalk hide fiber.
Claims (1)
1. inorganic base preliminary treatment, steam explosion and organic base ultrasonic-microwave Combined Treatment prepare a method for cotton stalk hide fiber, and it is characterized in that, the method comprises following processing step:
(1) machine cuts: the cotton stalk skin of drying is cut into the section that 15 ~ 20cm is long;
(2) oxygenation pretreatment: cotton stalk skin step (1) obtained is placed in the inorganic base sodium hydroxide solution that solid-to-liquid ratio is 1:30 ~ 1:40, and alkali consumption is 25 ~ 40g/L, and treatment temperature is 60 ~ 80 DEG C, and the processing time is 50 ~ 150min;
(3) steam explosion: the pretreated cotton stalk skin of inorganic base does not wash, after circulating water is extruded, load and dodge in quick-fried tank, pass into saturated vapor, make saturated vapor pressure reach 1.5 ~ 2.5MPa, dodge quick-fried instantaneously with 0.0875s after maintaining saturated vapor pressure 60 ~ 300s;
(4) extract: the crude fibre obtained after steam explosion is placed in organic base tetramethyl ammonium hydroxide solution, TMAH consumption is 20 ~ 30g/L, solid-to-liquid ratio is 1:30 ~ 1:60, Ultrasonic-microwave synergistic extraction reaction instrument is adopted to extract further, ultrasonic frequency is 25KHZ, and microwave frequency is 2450MHZ, and temperature is 60 ~ 90 DEG C, time is 15 ~ 60min, extracts 2 ~ 3 times;
(5) wash: the sample after extraction is washed at normal temperatures;
(6) neutralize: adopt mass percent be 10 ~ 36% acetic acid neutralize, cotton stalk hide fiber pH value is adjusted to neutrality;
(7) dry: naturally to dry under fiber being placed in room temperature, obtain cotton stalk hide fiber.
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| CN201510956741.1A CN105568396A (en) | 2015-12-18 | 2015-12-18 | Method combining inorganic alkali pretreatment, steam explosion and organic alkali ultrasonic-microwave detection to prepare cotton stalk bark fiber |
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| CN201510956741.1A CN105568396A (en) | 2015-12-18 | 2015-12-18 | Method combining inorganic alkali pretreatment, steam explosion and organic alkali ultrasonic-microwave detection to prepare cotton stalk bark fiber |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106319641A (en) * | 2016-10-27 | 2017-01-11 | 青岛大学 | High-gum-content raw hemp fiber degumming method |
| CN108004283A (en) * | 2016-10-27 | 2018-05-08 | Ptt全球化学股份有限公司 | Use alkaline solution and the preprocessing process of the lignocellulose biomass of vapour explosion |
| CN108329407A (en) * | 2017-12-28 | 2018-07-27 | 潍坊友容实业有限公司 | A method of extracting cellulose from Suaeda salsa |
| CN111823343A (en) * | 2020-07-17 | 2020-10-27 | 安徽三和工艺品有限公司 | Method for treating rubber wood to improve surface coating performance based on steam explosion method |
| CN113073485A (en) * | 2021-04-09 | 2021-07-06 | 黑龙江八一农垦大学 | Preparation method of nano cellulose fiber and product thereof |
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| CN102286789A (en) * | 2011-08-01 | 2011-12-21 | 西安工程大学 | Method for preparing cotton bast cellulose fibers by directly degumming cotton stalks |
| CN102492997A (en) * | 2011-12-09 | 2012-06-13 | 西南大学 | Flash explosion and base boiling combined degumming method of natural bamboo fiber |
| CN104762668A (en) * | 2015-01-21 | 2015-07-08 | 江南大学 | Method for steam explosion-sodium chlorite-alkali treatment combined preparation of cotton bast fibers |
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2015
- 2015-12-18 CN CN201510956741.1A patent/CN105568396A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102286789A (en) * | 2011-08-01 | 2011-12-21 | 西安工程大学 | Method for preparing cotton bast cellulose fibers by directly degumming cotton stalks |
| CN102492997A (en) * | 2011-12-09 | 2012-06-13 | 西南大学 | Flash explosion and base boiling combined degumming method of natural bamboo fiber |
| CN104762668A (en) * | 2015-01-21 | 2015-07-08 | 江南大学 | Method for steam explosion-sodium chlorite-alkali treatment combined preparation of cotton bast fibers |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106319641A (en) * | 2016-10-27 | 2017-01-11 | 青岛大学 | High-gum-content raw hemp fiber degumming method |
| CN108004283A (en) * | 2016-10-27 | 2018-05-08 | Ptt全球化学股份有限公司 | Use alkaline solution and the preprocessing process of the lignocellulose biomass of vapour explosion |
| CN106319641B (en) * | 2016-10-27 | 2019-01-18 | 青岛大学 | A kind of Degumming method of the raw ramie fiber of high gum level |
| CN108329407A (en) * | 2017-12-28 | 2018-07-27 | 潍坊友容实业有限公司 | A method of extracting cellulose from Suaeda salsa |
| CN111823343A (en) * | 2020-07-17 | 2020-10-27 | 安徽三和工艺品有限公司 | Method for treating rubber wood to improve surface coating performance based on steam explosion method |
| CN113073485A (en) * | 2021-04-09 | 2021-07-06 | 黑龙江八一农垦大学 | Preparation method of nano cellulose fiber and product thereof |
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Application publication date: 20160511 |