CN1955346A - Method for extracting ramie from supercritical CO2 media by enzyme method - Google Patents
Method for extracting ramie from supercritical CO2 media by enzyme method Download PDFInfo
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- CN1955346A CN1955346A CN 200510118278 CN200510118278A CN1955346A CN 1955346 A CN1955346 A CN 1955346A CN 200510118278 CN200510118278 CN 200510118278 CN 200510118278 A CN200510118278 A CN 200510118278A CN 1955346 A CN1955346 A CN 1955346A
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Abstract
A process for extracting ramie fibers by enzyme method in the condition of supercritical CO2 includes such steps as providing raw ramie, pre-treating by Na2CO3, preparing the solution of pectinase and xylanase, immersing raw ramie in said solution, supercritical enzyme treating, baking, washing, bleaching with H2O2, dewatering, applying oil, removing oil and water, shaking the ramie fibers, and baking.
Description
One, technical field
The present invention relates to the new method that ramee extracts in the textile industry, particularly adopt Chemical Pretreatment and supercritical CO
2The ramee extracting method that enzymic catalytic reaction combines in the medium.
Two, background technology
The bast-fibre goods are China's characteristic export-oriented commodities.2004, China's bast-fibre goods foreign exchange earning reached 9.3 hundred million dollars, is 20 times before 20 years.Particularly after China joined WTO, bast-fibre and goods thereof with national characters are just showing bigger vigor.
Ramie is a kind of high yield, high-quality, efficient bast fiber crop that originates in China.Agricultural product-ramie that the peasant obtains by decorticating (raw ramie), must be through coming unstuck, remove its non-cellulose material and (comprise pectin, hemicellulose, lignin, cerolipoid, the hydrotrope etc., general designation ramie colloid, account for the 22-30% of raw ramie weight), could obtain ramee loose, pure white, that can be used for weaving.At present, the ramie degumming method that generally adopts is the conventional chemical processing technology both at home and abroad, and the basic principle of this process acts is to adopt strong acid, highly basic to separate the non-cellulose material in high temperature, high drops.Its technology path is generally: raw ramie → bundle boils (vapour pressure 2.0-2.5kg/cm to dress cage → pickling (bath raio 1: 8-10, sulfuric acid 4.5g/l, about 50 ℃, 30 minutes) →
2, 1.5h, bath raio 1: 10, NaOH concentration 6-8g/L) → wash fiber crops (60 ℃ of hot water, bath raio 1: 10) → two to boil (vapour pressure 2.0-2.5kg/cm
2, 2.5h, bath raio 1: 10, NaOH concentration 14-18g/L, auxiliary agent about 2%) → wash fiber crops (60-80 ℃ of hot water, bath raio 1: 10) → beat fine → float pickling (combination machine) → oil supply → dehydration → oven dry (degummed ramie).The subject matter that this method exists is: consume a large amount of industrial chemicals and the energy, one ton of raw ramie consumption of every processing solid caustic soda 150-200kg, concentrated sulfuric acid 45kg, the about 2.5T of raw coal, water 600m
3, about electricity 350 degree; Damage the intrinsic good characteristic of ramee and reduce fiber production, high temperature, high pressure and strong acid, when separating colloid, strong lye make the microfiber of original intersection, twisted arrangement become straight, and hydrolysis the low cellulosic molecule end of degree of crystallinity, cause that the resultant yarn cohesive force is poor, the fabric prodding and itching feeling is obvious, the row yielding of coming unstuck is generally 62-65%; Contaminated environment is serious, and these pollute except a large amount of inputs from degumming tech energy consumption, industrial chemicals, and also from raw ramie itself, the COD value is on average up to about 10000mg/L in its high-concentration waste water; The factory cost height, raw ramie per ton to the processing charges of degummed ramie about 3000 yuan.
For this reason, extensively carried out ramie biological degumming technology research both at home and abroad, Sun Qingxiang etc. (1985) utilize bacillus subtilis, Chen Fuxing (1991), Liu Zirong (1992) and Liu Zhengchu (1995) to utilize bacterium and fungi crude enzyme liquid, Li Fengming (1994) preparation pectase pulvis, He Shaojiang (1995), Hu state's congruence (2003) to utilize anaerobic bacteria to handle ramie after several hours to tens hours, finish China grass degumming with the sig water kiering again.These researchs have reducing production costs, improve fiber production, improve characteristics such as fiber quality and reduction environmental pollution, but occur two kinds of reaction mechanisms in same production technology, and technical difficulty is bigger; Simultaneously, the enzymatic degradation of ramie non-cellulose material is reflected in the aqueous solution and carries out, and environment is caused certain pollution.
Three, the quasi-solution key issue of determining
The subject matter that purpose of the present invention is come unstuck at the ramie conventional chemical and the biochemistry combined degum method exists combines modern biotechnology and supercritical fluid technique, provides a kind of the ramie raw ramie is carried out Chemical Pretreatment and supercritical CO
2The ramee extracting method that enzymic catalytic reaction combines.That is: pass through Na
2CO
3With boil-off assistant osmosises such as sodium polyphosphates, can the tough skin structure of loose to a certain extent raw ramie, make pectase, zytase be easier to enter between fibre bundle and in conjunction with the interfascicular colloid; Supercritical CO
2Reaction medium can quicken the catalytic reaction of enzyme; The H that bleaching is used
2O
2Be a kind of free of contamination bleaching agent, can dispose the old root of intractable that degummase can't decompose, spot etc.Compared with the prior art, have the textile performance that improves bast-fibre, shorten the cycle of coming unstuck, thoroughly solve the characteristics such as environmental pollution of China grass degumming.
Four, technical scheme
The technical scheme that the present invention intends adopting comprises: get the raw materials ready, the preparation of Chemical Pretreatment, enzyme liquid, enzyme liquid are soaked, overcritical enzyme is handled, copy fiber crops, wash fiber crops, bleaching, dehydration, oil supply, de-oiled water, tremble operations such as fiber crops and oven dry.
(1) get the raw materials ready the raw ramie removal of impurities, be curled into the fiber crops handle of 5cm ± 0.5cm, standby.
(2) Chemical Pretreatment is in the ratio preparation Na of raw ramie dry weight 1: 10-15
2CO
3Solution, Na
2CO
3Consumption is 2.0% ± 0.25% of a raw ramie dry weight, and the sodium polyphosphate consumption is 0.5% ± 0.1% of a raw ramie dry measure; Then, raw ramie is immersed in Na
2CO
3Solution boils and boils 1.0h ± 0.5h; At last, residual Na in the water flushing fiber crops
2CO
3Solution gets final product.
(3) preparation of enzyme liquid presses 1 with pectase and zytase: the proportioning mixing of 3-5,20 times (make pectase concentration is 5% to thin up, zytase concentration 15%-25%), add 1.5 ‰ ± 0.5 ‰ glycerine (stabilizing agent) again, with HCl or NaOH adjust pH 5.0 ~ 6.0, heat to 45 ℃ ± 5 ℃.
(4) enzyme liquid soaks in 1: the ratio of 5-10 (the raw ramie dry weight is to the weight of water), and will be soaked in the enzyme liquid through pretreated raw ramie and handle 20min-40min, make numb moisture content reach 65% ± 5% and get final product.
(5) supercritical CO
2Enzyme is handled the reaction under high pressure reactor that the ramie material of adsorptive enzyme liquid is placed 2L in the medium, heats to 45 ℃ ± 5 ℃, uses CO
2Medium is forced into 8MPa-10MPa and handles 2.0h ± 0.5h.
(6) bleaching H
2O
2Amount is for handling the 15%-25% of fibre weight, and the NaOH amount is for handling 2.0% ± 0.5% of fibre weight, control bath raio 1: 10-15, temperature 95-100 ℃, processing time 20min-40min.
(7) copy fiber crops, wash fiber crops, dehydration, oil supply, de-oiled water, tremble fiber crops and dry routinely technology and carry out.
Five, embodiment
(1) technical scheme
The technical scheme that the present invention intends adopting comprises: get the raw materials ready, the preparation of Chemical Pretreatment, enzyme liquid, enzyme liquid are soaked, supercritical CO
2Enzyme is handled, copies fiber crops, is washed fiber crops, bleaching, dehydration, oil supply, de-oiled water, trembles operations such as fiber crops and oven dry in the medium.
Embodiment 1
1, get the raw materials ready the raw ramie removal of impurities, be curled into the fiber crops handle of 5cm ± 0.5cm, standby.
2, Chemical Pretreatment is in 1: 10 ratio of raw ramie dry weight preparation Na
2CO
3Solution, Na
2CO
3Consumption is 1.5% of a raw ramie dry weight, and the sodium polyphosphate consumption is 0.5% ± 0.1% of a raw ramie dry measure; Then, raw ramie is immersed in Na
2CO
3Solution boils and boils 0.5h; At last, residual Na in the water flushing fiber crops
2CO
3Solution gets final product.
3, the preparation of enzyme liquid is pressed 1: 3 proportioning mixing with pectase and the 5000IU/ml zytase of active 2000IU/ml, 20 times (make pectase concentration is 5% to thin up, zytase concentration 15%), add 1.0 ‰ glycerine again, with HCl or NaOH adjust pH 5.0-6.0, heat to 45 ℃ ± 5 ℃.
4, enzyme liquid soaks the ratio (the raw ramie dry weight is to the weight of water) in 1: 5, will be soaked in the enzyme liquid through pretreated raw ramie and handle 20min-40min.
5, supercritical CO
2Enzyme is handled the reaction under high pressure reactor that the ramie material of adsorptive enzyme liquid is placed 2L in the medium, heats to 45 ℃ ± 5 ℃, uses CO
2Medium is forced into 8MPa and handles 1.5h.
6, bleaching H
2O
2Amount is for handling 15% of fibre weight, and the NaOH amount is for handling 1.5% of fibre weight, control bath raio 1: 10, temperature 95-100 ℃, processing time 20min.
7, copy fiber crops, wash fiber crops, dehydration, oil supply, de-oiled water, tremble fiber crops and dry routinely technology and carry out.
Embodiment 2
1, get the raw materials ready the raw ramie removal of impurities, be curled into the fiber crops handle of 5cm ± 0.5cm, standby.
2, Chemical Pretreatment is in 1: 15 ratio of raw ramie dry weight preparation Na
2CO
3Solution, Na
2CO
3Consumption is 2.25% of a raw ramie dry weight, and the sodium polyphosphate consumption is 0.5% ± 0.1% of a raw ramie dry measure; Then, raw ramie is immersed in Na
2CO
3Solution boils and boils 1.5h; At last, residual Na in the water flushing fiber crops
2CO
3Solution gets final product.
3, the preparation of enzyme liquid is pressed 1: 5 proportioning mixing with the pectase of active 2240IU/ml and the zytase of 5150IU/ml, 20 times (make pectase concentration is 5% to thin up, zytase concentration 25%), add 2.0 ‰ glycerine again, with HCl or NaOH adjust pH 5.0-6.0, heat to 45 ℃ ± 5 ℃.
4, enzyme liquid soaks the ratio (the raw ramie dry weight is to the weight of water) by 1: 10, will be soaked in that processing 20min-40min gets final product in the enzyme liquid through pretreated raw ramie.
5, supercritical CO
2Enzyme is handled the reaction under high pressure reactor that the ramie material of adsorptive enzyme liquid is placed 2L in the medium, heats to 45 ℃ ± 5 ℃, uses CO
2Medium is forced into 10MPa and handles 2.5h.
6, bleaching H
2O
2Amount is for handling 25% of fibre weight, and the NaOH amount is for handling 2.5% of fibre weight, control bath raio 1: 15,95 ~ 100 ℃ of temperature, processing time 40min.
7, copy fiber crops, wash fiber crops, dehydration, oil supply, de-oiled water, tremble fiber crops and dry routinely technology and carry out.
Embodiment 3
1, get the raw materials ready the raw ramie removal of impurities, be curled into the fiber crops handle of 5cm ± 0.5cm, standby.
2, Chemical Pretreatment is in 1: 12.5 ratio of raw ramie dry weight preparation Na
2CO
3Solution, Na
2CO
3Consumption is 1.875% of a raw ramie dry weight, and the sodium polyphosphate consumption is 0.4% ± 0.1% of a raw ramie dry measure; Then, raw ramie is immersed in Na
2CO
3Solution boils and boils 1.0h; At last, residual Na in the water flushing fiber crops
2CO
3Solution gets final product.
3, the preparation of enzyme liquid is pressed 1: 4 proportioning mixing with pectase and the 5000IU/ml zytase of active 2000IU/ml, 20 times (make pectase concentration is 5% to thin up, zytase concentration 20%), add 1.0 ‰ glycerine again, with HCl or NaOH adjust pH 5.0～6.0, heat to 45 ℃ ± 5 ℃.
4, enzyme liquid soaks the ratio (the raw ramie dry weight is to the weight of water) in 1: 7.5, will be soaked in the enzyme liquid through pretreated raw ramie and handle 20min-40min.
5, supercritical CO
2Enzyme is handled the reaction under high pressure reactor that the ramie material of adsorptive enzyme liquid is placed 2L in the medium, heats to 45 ℃ ± 5 ℃, uses CO
2Medium is forced into 9MPa and handles 2.0h.
6, bleaching H
2O
2Amount is for handling 20% of fibre weight, and the NaOH amount is for handling 2.0% of fibre weight, control bath raio 1: 12.5, temperature 95-100 ℃, processing time 30min.
7, copy fiber crops, wash fiber crops, dehydration, oil supply, de-oiled water, tremble fiber crops and dry routinely technology and carry out.
(2) implementation result
The present invention adopts the scale of 50g, 500g and 2kg raw ramie to implement above-mentioned technological process, and result of implementation shows that present technique can be processed into the raw ramie of different cultivars, different brackets the degummed ramie of pure white softness.The row yielding of coming unstuck is stabilized between the 70%-75%, and the cycle of coming unstuck, monofilament strength was at 4.2g/D-4.7g/D in 8h.Compare with conventional method, it is short, evenly to have a processing time, quality better, pollutes characteristics such as light.Solve that the environmental pollution that the conventional chemical degumming tech exists is heavy, fibre percentage is low and problem such as poor quality.
Claims (7)
1, a kind of supercritical CO
2The method of Enzymatic Extraction ramee in the medium is characterized in that adopting Na
2CO
3After carrying out preliminary treatment, at supercritical CO
2Carry out pectase and zytase catalytic reaction under the condition and extract ramee, utilize H
2O
2Bleach.
2, a kind of supercritical CO according to claim 1
2The method of Enzymatic Extraction ramee in the medium is characterized in that technological process comprises: raw ramie is prepared (getting the raw materials ready), preliminary treatment, the preparation of enzyme liquid, the immersion of enzyme liquid, supercritical CO
2Enzyme is handled, copies fiber crops, washes fiber crops, is bleached, washes fiber crops, dehydration, oil supply, de-oiled water, tremble operations such as fiber crops and oven dry.
3, a kind of supercritical CO according to claim 1
2The method of Enzymatic Extraction ramee in the medium, the Na that adds when it is characterized in that preliminary treatment
2CO
3Amount is 2.0% ± 0.25% of raw ramie weight, and the sodium polyphosphate amount is the 0.4%-0.6% of raw ramie weight, bath raio 1: 10-15, Na
2CO
3Solution boils and boils 1.0h ± 0.5h.
4, a kind of supercritical CO according to claim 1
2The method of Enzymatic Extraction ramee in the medium, the proportioning 1 of pectase and zytase when it is characterized in that the preparation of enzyme liquid: 3-5, pectase concentration 5%, zytase concentration 15%-25%, glycerine (stabilizing agent) concentration 1.5 ‰ ± 0.5 ‰, pH value 5.0-6.0,45 ℃ ± 5 ℃ of temperature; Bath raio was 1 when enzyme liquid soaked: 5-10, soak time 20min-40min.
5, a kind of supercritical CO according to claim 1
2The method of Enzymatic Extraction ramee is characterized in that CO in the medium
2Carry out 45 ℃ ± 5 ℃ of the temperature of pectase and zytase catalytic reaction under the super critical condition, CO
2Pressure is 8MPa-10MPa, reaction time 2.0h ± 0.5h.
6, CO according to claim 1
2Overcritical Enzymatic Extraction ramee technology, the H that adds when it is characterized in that bleaching
2O
2Amount is for handling the 15%-25% of fibre weight, and the NaOH amount is for handling 2.0% ± 0.5% of fibre weight, control bath raio 1: 10-15, temperature 95-100 ℃, processing time 20min-40min.
7, according to claim 1 or 3 described CO
2Overcritical Enzymatic Extraction ramee technology is characterized in that pectinase activity＞2000IU/ml of adding, xylanase activity＞5000IU/ml.
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| CN 200510118278 CN1955346A (en) | 2005-10-24 | 2005-10-24 | Method for extracting ramie from supercritical CO2 media by enzyme method |
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| CN102533936A (en) * | 2012-01-06 | 2012-07-04 | 东华大学 | Method for measuring enzyme activity of special pectinase for textile by taking bast-fibre pectin as substrate |
| CN103835005A (en) * | 2013-12-08 | 2014-06-04 | 姜著川 | Explosion and supercritical carbon dioxide fluid combined degumming method for apocynum venetum |
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| CN102533936B (en) * | 2012-01-06 | 2014-07-02 | 东华大学 | Method for measuring enzyme activity of special pectinase for textile by taking bast-fibre pectin as substrate |
| CN102533936A (en) * | 2012-01-06 | 2012-07-04 | 东华大学 | Method for measuring enzyme activity of special pectinase for textile by taking bast-fibre pectin as substrate |
| CN103835005A (en) * | 2013-12-08 | 2014-06-04 | 姜著川 | Explosion and supercritical carbon dioxide fluid combined degumming method for apocynum venetum |
| CN104032611B (en) * | 2014-06-23 | 2016-04-20 | 广西大学 | A kind of dioxde pulp bleaching process |
| CN104032611A (en) * | 2014-06-23 | 2014-09-10 | 广西大学 | Paper pulp bleaching method |
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| CN104313891A (en) * | 2014-10-17 | 2015-01-28 | 苏州大学 | Starch slurry desizing method adopting supercritical carbon dioxide as medium |
| CN104372598A (en) * | 2014-10-17 | 2015-02-25 | 苏州大学 | Supercritical carbon dioxide fluid desizing method by use of combined enzyme |
| CN104389153A (en) * | 2014-10-17 | 2015-03-04 | 苏州大学 | Method for enzymatic desizing of cotton in supercritical carbon dioxide fluid |
| WO2016058252A1 (en) * | 2014-10-17 | 2016-04-21 | 苏州大学 | Method for enzyme desizing cotton in a supercritical carbon dioxide fluid |
| WO2016058257A1 (en) * | 2014-10-17 | 2016-04-21 | 苏州大学 | Textile desizing pretreatment method |
| CN105154995A (en) * | 2015-08-14 | 2015-12-16 | 辽宁轻工职业学院 | Method for chemically degumming apocynum venetum bast fibers through supercritical carbon dioxide |
| CN105040117A (en) * | 2015-08-14 | 2015-11-11 | 辽宁轻工职业学院 | Supercritical carbon dioxide extraction degumming method for apocynum venetum bast fiber |
| CN105040118A (en) * | 2015-08-14 | 2015-11-11 | 辽宁轻工职业学院 | Apocynum venetum bast fiber supercritical carbon dioxide biochemical degumming method |
| CN105040117B (en) * | 2015-08-14 | 2017-04-26 | 辽宁轻工职业学院 | Supercritical carbon dioxide extraction degumming method for apocynum venetum bast fiber |
| CN105154995B (en) * | 2015-08-14 | 2017-07-18 | 辽宁轻工职业学院 | Apocynum bast fiber Chemistry of Carbon Dioxide in Supercritical Degumming method |
| CN105651719A (en) * | 2016-01-21 | 2016-06-08 | 苏州大学 | Supercritical fluid processing method for improving activity and stability of pectinase |
| CN107881644A (en) * | 2017-11-07 | 2018-04-06 | 中国农业科学院麻类研究所 | A kind of flaxen fiber Oil Guide film and preparation method thereof |
| CN107881644B (en) * | 2017-11-07 | 2019-11-08 | 中国农业科学院麻类研究所 | A kind of flaxen fiber Oil Guide film and preparation method thereof |
| CN107916460A (en) * | 2017-11-28 | 2018-04-17 | 黄桂凤 | A kind of Degumming method of hemp |
| CN113550137A (en) * | 2021-07-12 | 2021-10-26 | 武汉纺织大学 | Method for preparing non-woven fabric through multi-effect composite bleaching |
| CN113550137B (en) * | 2021-07-12 | 2022-04-22 | 武汉纺织大学 | Method for preparing non-woven fabric through multi-effect composite bleaching |
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