CN102492058A - Preparation method of straw hemicellulose A - Google Patents

Preparation method of straw hemicellulose A Download PDF

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Publication number
CN102492058A
CN102492058A CN2011103639352A CN201110363935A CN102492058A CN 102492058 A CN102492058 A CN 102492058A CN 2011103639352 A CN2011103639352 A CN 2011103639352A CN 201110363935 A CN201110363935 A CN 201110363935A CN 102492058 A CN102492058 A CN 102492058A
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straw
preparation
semicellulose
hours
supernatant
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CN2011103639352A
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CN102492058B (en
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胡国华
王伟
王飞
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Shanghai Normal University
University of Shanghai for Science and Technology
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Shanghai Normal University
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Abstract

The invention discloses a preparation method of straw hemicellulose A. The preparation method comprises the following steps: 1, carrying out alkaline treatment through mixing straws with a sodium hydroxide solution with the mass concentration of 2-4%, wherein the alkaline treatment temperature is 70-90DEG C, the alkaline treatment time is 1.5-3.5h, and the ratio of the mass of the straws to the volume of the sodium hydroxide solution is 1:10-1:16kg/L; 2, removing residue, taking the supernatant, and adjusting the pH value of the supernatant to 4-8; and 3, allowing the supernatant to stand for 6-14h at 0-6DEG C, and taking the obtained precipitate. The preparation method of the invention, which has the advantages of simple process, high product purity, low production cost and the like, is very suitable for industrialized production. According to the obtained straw hemicellulose A, the dietary fiber content is higher than 92%, the yield is 7.2-9.7%, and physical and chemical performances, the viscosity, the swelling force and the water holding capacity are good.

Description

The preparation method of a kind of straw semicellulose A
Technical field
The invention belongs to chemical field and biotechnology, the working method of food fibre especially relates to the working method of a kind of semicellulose A, is specifically related to a kind of working method of from straw, extracting semicellulose A.
Background technology
Along with the raising day by day of standard of living, people's diet is abundant day by day.Because most crowds prefer to the food of selecting protein-high, higher fatty acid, high calorie, thereby have caused large quantities of obesities, mellitus, hyperlipidemia and sub-health state crowd's appearance.Changing one of mode of this situation, is exactly often to eat some to be rich in the food of food fibre.The outstanding nourishing function of edible fiber products is familiar with by people gradually.Passed through 30 years of researches and development, food fibre has become the pandemic protective foods of developed country.2002, edible fiber products in American-European sales volume above 5,000,000,000 dollars; In Japan, nearly 10,000,000,000 dollars of the annual sales amount of edible fiber products, and formally as after protein, fat, glucide, water, mineral substance " the seventh-largest nutrient substance " of classifying.On November 2nd, 1999, the annual meeting of U.S. clinical chemistry association defined food fibre: food fibre is meant and can anti-human small intestine digests and assimilates; And the summation of edible vegetalitas composition, glucide and the similar substance that can partly or entirely ferment at human body knot rectum mainly is made up of Mierocrystalline cellulose, pectic substance, semicellulose and xylogen.
China's straw YO reaches about several hundred million tons, and southern rice straw is particularly abundant, and its staple is Mierocrystalline cellulose, semicellulose and xylogen, be enrich, cheap renewable resources.Straw accounts for about 60% of paddy by quality, is the main sub product at paddy rice plantation family.But at present people also rest on the lower stage to the utilization of straw, like the feed of the herbivore of fertilizing the soil, do, burn or with it abandonment.This has not only caused the serious environmental pollution, and is the significant wastage to resource.The development and use purposes of straw does not seldom all really form industrial scaleization.
Though at present existing many learning studied rice straw; But focus mostly on aspect energy development; Research to extracting semicellulose A in the rice straw is less; And traditional exploitation is confined to use the technology of physics or chemical more, and the employing biotechnology is carried out deep development and utilized then less polysaccharide wherein.
More about the research report of hemicellulose B both at home and abroad at present, but very few to the report of semicellulose A both at home and abroad, the monose composition of semicellulose A is generally monose such as pectinose, wood sugar, glucose and semi-lactosi.And almost not research of structure to semicellulose A in the straw.If can the semicellulose in the straw be developed to product, good application market and research prospect should be arranged then.
Summary of the invention
The object of the present invention is to provide a kind of producing and manufacturing technique for preparing straw semicellulose A, this method technology is simple relatively, the content of semicellulose A is high, and production cost is low, is suitable for suitability for industrialized production.
Goal of the invention of the present invention realizes through following technical scheme:
(1) with after the rice straw drying and crushing, mix with the NaOH solution of mass concentration 2%~4%, carry out alkaline purification, its alkali purification temp is 70~90 ℃, 1.5~3.5 hours alkaline purification time;
In this step, the mass volume ratio of rice straw and NaOH solution is 1: 10~1: 16kg/L;
Preferably, 70~95 ℃ of dryings of rice straw 3~6 hours are ground into 20~100 order particles; Exsiccant rice straw water cut is 8%~12%;
(2) remove residue, get supernatant and the pH value is adjusted to 4~8; Remove residue with filtering with centrifugation method, with the filtration of 100~200 orders, and centrifugal 10~30 minutes of 3000~6000rpm;
Placed 6~14 hours, and got deposition for (3) 0~6 ℃; The pH value is preferably 5~6; Preferably regulate supernatant pH value with acetate; Get deposition with centrifugation method, centrifugal speed 3000~6000rpm, centrifugation time are 10~30 minutes.
Resulting deposition is dry; The exsiccant optimal process does, in 40~55 ℃ of following vacuum-dryings 14~18 hours and pulverizing.
Preparing method of the present invention has advantages such as technology is simple, product purity is high, production cost is low, is fit to very much suitability for industrialized production.Dietary fiber content is higher than 92% in the products obtained therefrom; The productive rate of straw stalk hemicellulose A is 7.2%~9.7%, and the product physicochemical property is good, and viscosity is low, and swelling power and retention ability are good.
Embodiment
Through embodiment the present invention is described further below, its purpose only is better to understand content of the present invention and unrestricted protection scope of the present invention:
Embodiment 1
Rice straw is cut off, and 80 ℃ of forced air dryings 4 hours (water cut is 10%) are pulverized 40 orders and are sieved.
Take by weighing the rice straw that 1000 grams are pulverized, add the 14L mass concentration and be 2% the NaOH aqueous solution, 85 ℃ of water-baths are 3 hours then;
300 order nylon cloths filter, and remove filter residue; The centrifugal 15min of 4500r/min that will filtrate, using acetate adjustment supernatant PH is 5.5, and 4 ℃ of refrigerations 10 hours;
The centrifugal 15min of 4500r/min, abandoning supernatant must precipitate, and 55 ℃ of room temperature vacuum-drying 16 hours is pulverized fine grinding and is got straw semicellulose A 76g, productive rate 7.6%, wherein dietary fiber content is greater than 93%.
Product is a pale powder, and mouthfeel does not have rough sense, and is soluble in water; 2% soltion viscosity (25 ℃) is 8.5cps, retention ability 5.7ml/g; Swelling power 6.5ml/g.
Embodiment 2
Rice straw is cut off, and 80 ℃ of forced air dryings 4 hours (water cut is 9%) are pulverized 40 orders and are sieved.
Take by weighing the rice straw that 1000 grams are pulverized, add the 14L mass concentration and be 2.5% the NaOH aqueous solution, 85 ℃ of water-baths are 3 hours then;
300 order nylon cloths filter, and remove filter residue; The centrifugal 15min of 4500r/min that will filtrate, using acetate adjustment supernatant PH is 5.5, and 4 ℃ of refrigerations 10 hours;
The centrifugal 15min of 4500r/min, abandoning supernatant must precipitate, and 55 ℃ of room temperature vacuum-drying 16 hours is pulverized fine grinding and is got straw semicellulose A 91g, productive rate 9.1%, wherein dietary fiber content is greater than 93%.
Product is a pale powder, and mouthfeel does not have rough sense, and is soluble in water; 2% soltion viscosity (25 ℃) is 8.4cps, retention ability 5.8ml/g; Swelling power 6.4ml/g.
Embodiment 3
Rice straw is cut off, and 80 ℃ of forced air dryings 4 hours (water cut is 9%) are pulverized 40 orders and are sieved.
Take by weighing the rice straw that 1000 grams are pulverized, add the 14L mass concentration and be 3% the NaOH aqueous solution, 85 ℃ of water-baths are 3 hours then;
300 order nylon cloths filter, and remove filter residue, the centrifugal 15min of 4500r/min that will filtrate, and using acetate adjustment supernatant PH is 5.5, and 4 ℃ of refrigerations 10 hours;
The centrifugal 15min of 4500r/min, abandoning supernatant must precipitate, and 55 ℃ of room temperature vacuum-drying 16 hours is pulverized fine grinding and is got straw semicellulose A 93g, productive rate 9.3%, wherein dietary fiber content is greater than 93%.
Product is a pale powder, and mouthfeel does not have rough sense, and is soluble in water; 2% soltion viscosity (25 ℃) is 8.5cps, retention ability 5.6ml/g; Swelling power 6.5ml/g.
Embodiment 4
Rice straw is cut off, and 80 ℃ of forced air dryings 4 hours (water cut is 10%) are pulverized 40 orders and are sieved.
Take by weighing the rice straw that 1000 grams are pulverized, add the 14L mass concentration and be 3.5% the NaOH aqueous solution, 85 ℃ of water-baths are 3 hours then;
300 order nylon cloths filter, and remove filter residue, the centrifugal 15min of 4500r/min that will filtrate, and using acetate adjustment supernatant PH is 5.5, and refrigerates 10 hours down at 4 ℃;
The centrifugal 15min of 4500r/min, abandoning supernatant must precipitate, and 55 ℃ of room temperature vacuum-drying 16 hours is pulverized fine grinding and is got straw semicellulose A 92g, productive rate 9.2%, wherein dietary fiber content is greater than 93%.
Product is a pale powder, and mouthfeel does not have rough sense, and is soluble in water; 2% soltion viscosity (25 ℃) is 8.5cps, retention ability 5.7ml/g; Swelling power 6.6ml/g.
Embodiment 5
Rice straw is cut off, and 80 ℃ of forced air dryings 4 hours (water cut is 11%) are pulverized 40 orders and are sieved.
Take by weighing the rice straw that 1000 grams are pulverized, add the 14L mass concentration and be 4% the NaOH aqueous solution, 85 ℃ of water-baths are 3 hours then;
300 order nylon cloths filter, and remove filter residue, the centrifugal 15min of 4500r/min that will filtrate, and using acetate adjustment supernatant PH is 5.5, and refrigerates 10 hours down at 4 ℃;
The centrifugal 15min of 4500r/min, abandoning supernatant must precipitate, and 55 ℃ of room temperature vacuum-drying 16 hours is pulverized fine grinding and is got straw semicellulose A 89g, productive rate 8.9%, wherein dietary fiber content is greater than 93%.
Product is a pale powder, and mouthfeel does not have rough sense, and is soluble in water; 2% soltion viscosity (25 ℃) is 8.4cps, retention ability 5.5ml/g; Swelling power 6.4ml/g.
Embodiment 6
Rice straw is cut off, and 80 ℃ of forced air dryings 4 hours (water cut is 10%) are pulverized 40 orders and are sieved.
Take by weighing the rice straw that 1000 grams are pulverized, add the 10L mass concentration and be 2.5% the NaOH aqueous solution, 85 ℃ of water-baths are 3 hours then;
300 order nylon cloths filter, and remove filter residue, the centrifugal 15min of 4500r/min that will filtrate, and using acetate adjustment supernatant PH is 5.5, and refrigerates 10 hours down at 4 ℃;
The centrifugal 15min of 4500r/min, abandoning supernatant must precipitate, and 55 ℃ of room temperature vacuum-drying 16 hours is pulverized fine grinding and is got straw semicellulose A 61g, productive rate 6.1%, wherein dietary fiber content is greater than 93%.
Product is a pale powder, and mouthfeel does not have rough sense, and is soluble in water; 2% soltion viscosity (25 ℃) is 8.5cps, retention ability 5.7ml/g; Swelling power 6.6ml/g.
Embodiment 7
Straw is cut off, and 80 ℃ of forced air dryings 4 hours (water cut is 10%) are pulverized 40 orders and are sieved.
Take by weighing the straw that 1000 grams are pulverized, add the 12L mass concentration and be 2.5% the NaOH aqueous solution, 85 ℃ of water-baths are 3 hours then;
300 order nylon cloths filter, and remove filter residue, the centrifugal 15min of 4500r/min that will filtrate, and using acetate adjustment supernatant PH is 5.5, and refrigerates 10 hours down at 4 ℃;
The centrifugal 15min of 4500r/min, abandoning supernatant must precipitate, and 55 ℃ of room temperature vacuum-drying 16 hours is pulverized fine grinding and is got straw semicellulose A 87g, productive rate 8.7%, wherein dietary fiber content is greater than 93%.
Product is a pale powder, and mouthfeel does not have rough sense, and is soluble in water; 2% soltion viscosity (25 ℃) is 8.6cps, retention ability 5.3ml/g; Swelling power 6.7ml/g.

Claims (7)

1. the preparation method of a straw semicellulose A is characterized in that, may further comprise the steps:
(1) with after the rice straw drying and crushing, to mix with the NaOH solution of mass concentration 2%~4% and to carry out alkaline purification, its alkali purification temp is 70~90 ℃, 1.5~3.5 hours alkaline purification time; The mass volume ratio of rice straw and NaOH solution is 1: 10~1: 16kg/L;
(2) remove residue, get supernatant and the pH value is adjusted to 4~8;
Placed 6~14 hours, and got deposition for (3) 0~6 ℃.
2. the preparation method of the said straw semicellulose of claim 1 A is characterized in that, in the step (1) with rice straw 70~95 ℃ of dryings 3~6 hours, and be ground into 20~100 order particles.
3. the preparation method of the said straw semicellulose of claim 1 A is characterized in that, dried rice straw water cut is 8%~12% in the step (1).
4. the preparation method of the said straw semicellulose of claim 1 A is characterized in that, the method for removing residue in the step (2) is filtration and centrifugal.
5. the preparation method of the said straw semicellulose of claim 1 A is characterized in that, regulates the pH value of supernatant in the step (2) with acetate.
6. the preparation method of the said straw semicellulose of claim 1 A is characterized in that, the pH value of supernatant is adjusted to 5~6 in the step (2).
7. the preparation method of the said straw semicellulose of claim 1 A is characterized in that, the deposition that step (3) obtains is carried out drying, and technology is: 40~55 ℃ of following vacuum-dryings 14~18 hours.
CN201110363935.2A 2011-11-16 2011-11-16 Preparation method of straw hemicellulose A Expired - Fee Related CN102492058B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103145881A (en) * 2013-03-29 2013-06-12 南开大学 Method for preparing hemicellulose from maize straws by adopting solid base catalyst
CN103467627A (en) * 2013-09-14 2013-12-25 大连工业大学 Preparation method for corn stalk hemicellulose

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1850866A (en) * 2006-05-26 2006-10-25 上海师范大学 Method for preparing tikitiki hemicellulose B
CN101628948A (en) * 2009-07-31 2010-01-20 上海师范大学 Straw stalk hemicellulose B preparation method

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1850866A (en) * 2006-05-26 2006-10-25 上海师范大学 Method for preparing tikitiki hemicellulose B
CN101628948A (en) * 2009-07-31 2010-01-20 上海师范大学 Straw stalk hemicellulose B preparation method

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103145881A (en) * 2013-03-29 2013-06-12 南开大学 Method for preparing hemicellulose from maize straws by adopting solid base catalyst
CN103467627A (en) * 2013-09-14 2013-12-25 大连工业大学 Preparation method for corn stalk hemicellulose

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