CN106617111A - Method for preparing dietary fiber from liquid ammonia steam exploded straw - Google Patents
Method for preparing dietary fiber from liquid ammonia steam exploded straw Download PDFInfo
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- CN106617111A CN106617111A CN201710040534.0A CN201710040534A CN106617111A CN 106617111 A CN106617111 A CN 106617111A CN 201710040534 A CN201710040534 A CN 201710040534A CN 106617111 A CN106617111 A CN 106617111A
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- dietary fiber
- hemicellulose
- lignin
- liquefied ammonia
- filtrate
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Abstract
The invention discloses a method for preparing dietary fiber from liquid ammonia steam exploded straw. The method comprises steps as follows: 1) liquid ammonia is added to straw at 80-90 DEG C for steam explosion, and a steam exploded product is obtained; 2) the steam exploded product is washed and filtered, and filtrate containing hemicellulose and filter residues containing cellulose and lignin are obtained; 3) ethanol is added to the filtrate obtained in step 2), soluble hemicellulose precipitates, filtration is performed, and hemicellulose is obtained; 4) the filter residues obtained in step 2) are cooked with ethanol, filtration is performed, and filtrate containing ethanol and lignin and filter residues containing cellulose are obtained; 5) the filtrate obtained in step 4) and monosaccharide are subjected to graft copolymerization under the acid condition, filtration is performed, and filter residues are a lignin copolymer; 6) the lignin copolymer, cellulose, hemicellulose and starch are mixed, and the dietary fiber is obtained. The problem that higher temperature is required for steam explosion of straw now is solved, and the prepared dietary fiber tastes good.
Description
Technical field
The present invention relates to the preparing technical field of dietary fiber, and in particular to liquefied ammonia steam puffed stalk prepares the side of dietary fiber
Method.
Background technology
Dietary fiber is a kind of current functional food ingredient generally acknowledged in the world, is referred to as except water, protein, sugar
" the 7th nutrient " outside class, lipid, vitamin, the big nutrient of mineral matter 6, and be described as most being received in 21 century food industry
Concern, a kind of food additives with special health care and food modifying function.Dietary fiber can be used as a kind of effective
Functional health-care food prevention of various diseases, and with water-retaining property, Oil keeping, improve the special work(such as food color and local flavor
Effect, can improve human consumption's absorption, strengthen body discharges function, promote the diet structure balance of human body, hinder human body to one
A little eutrophic excessive absorptions, keep function equilibrium, prevent all kinds of calculus etc. to make with anticancer, step-down, reducing blood lipid, reducing slimming machine
With.
Contain dietary fiber in the crops such as stalk, water fruits and vegetables, but dietary fiber is extracted from water fruits and vegetables
It is relatively costly.And not only containing abundant dietary fiber in the crops such as stalk, forming preparation cost is relatively low, so adopting
It is a kind of industry development trend to prepare dietary fiber with stalk, and dietary fiber mainly includes cellulose, hemicellulose and lignin.
Dietary fiber compacted mass in stalk, comparison is inflexible, not only affects mouthfeel but also band is gone away when through human body
The efficiency of body enteron aisle rubbish is reduced.Therefore, the dietary fiber in stalk is needed after cellulose, hemicellulose and lignin separation
Mixed again.
At present, using acetic acid boiling and steam blasting in the isolation technics of dietary fiber, acetic acid boiling is easily caused preparation
Dietary fiber poor taste, many steam blastings need to carry out explosion at high temperature to obtain more preferable mouthfeel, quick-fried under high temperature
It is broken all can equipment requirement it is of a relatively high, and danger is also relatively large.
The content of the invention
It is an object of the invention to provide the method that liquefied ammonia steam puffed stalk prepares dietary fiber, solves existing steam blasting straw
Stalk needs the problem of higher temperature, while the dietary fiber for preparing has good mouthfeel.
The present invention is achieved through the following technical solutions：
The method that liquefied ammonia steam puffed stalk prepares dietary fiber, comprises the following steps：
1), stalk adds liquefied ammonia to carry out steam explosion at 80-90 DEG C and obtains steam explosion product；
2), liquid ammonia recovery, steam explosion product is washed, and takes off hemicellulose, is filtered, and obtains the filter containing hemicellulose
The filter residue of liquid, containing cellulose and lignin；
3), to step 2) in the filtrate that obtains add ethanol, soluble hemicellulose precipitation is filtered, and obtains hemicellulose；
4), by step 2) obtain filter residue ethanol boiling, filter, obtain the filtrate containing ethanol and lignin, contain
The filter residue of cellulose；
5), by step 4) obtain filtrate in acid condition with monose graft copolymerization, filter, filter residue be lignin copolymerization
Thing；
6), by step 5) obtain lignin copolymer, step 4) obtain cellulose, step 3 obtain hemicellulose
And starch carries out mixing and obtains dietary fiber.
At present, using acetic acid boiling and steam blasting in the isolation technics of dietary fiber, acetic acid boiling is without steam explosion skill
Art, directly uses acetic acid boiling stalk, filters, and containing hemicellulose and lignin in filtrate, filter residue is cellulose, then by filtrate
Containing hemicellulose and lignin separation, finally hemicellulose, lignin and cellulose are mixed into into dietary fiber, acetic acid boiling
Be easily caused the dietary fiber poor taste of preparation, many steam blastings in order to obtain more preferable mouthfeel need to carry out at high temperature it is quick-fried
It is broken, under high temperature explosion all can equipment requirement it is of a relatively high, and danger is also relatively large.
Liquefied ammonia steam explosion of the present invention specifically refers to add the steam blasting of liquefied ammonia, and specifically, steam blasting is by stalk
It is sealed in the container with uniform temperature and pressure, when the evaporation right pressure release of processus aboralis to a certain extent, stalk just struts explosion, class
Like puffed rice.In the reasonable scope the higher demolition effect of temperature is better, and common steam explosion temperature carries out ability under 150 DEG C or so
Obtain the weight ratio preferably 1 of preferable mouthfeel, liquefied ammonia and stalk:1-3.
The present invention can effectively lower temperature during steam explosion by adding liquefied ammonia, liquefied ammonia during steam explosion, and can
Guarantee the mouthfeel of the dietary fiber of demolition effect and preparation, because temperature during liquefied ammonia steam explosion is less than 100 DEG C, equipment is wanted
Reduction is asked, and improves the security of steam explosion.
The principle of the present invention：Hemicellulose dissolving during washing (explosion thing is soluble in water), in explosion thing
In water, in filter residue, by filter residue ethanol boiling, lignin dissolution is obtained in ethanol solution for lignin and cellulose
To the filtrate containing lignin.
Lignin of the present invention has aldehyde radical, and monose is partly ring-type in aqueous, is partly chain, in monose
Phenolic hydroxyl group and lignin in aldehyde radical carry out phenol formaldehyde condensation reaction, then, the strand of lignin increases, molecular weight increase,
Filament with certain lines is changed into from original unbodied granular structure, chewy texture can not only be increased, strengthen mouthfeel,
And hydrophobicity can be improved, it is macromolecule that the lignin after improvement improves material, not easily digested, by human body
When directly take away rubbish and toxin in enteron aisle, play a part of toxicant elimination and fat cleanness.
To sum up, the lignin copolymer of preparation, cellulose, hemicellulose and starch are carried out mixing and obtain meals by the present invention
Food fiber not only increases the gas porosity of dietary fiber in stalk, and prepares lignin copolymer because by original unbodied
Granular structure is changed into the filament with certain lines and improves mouthfeel, and then, the dietary fiber prepared by the present invention has
Good mouthfeel.
Further, acid be hydrochloric acid, step 5) in acid condition be pH value be 5.0-6.0.
Further, liquid ammonia recovery with step：Heating liquefied ammonia is changed into ammonia, and then hot blast removes deammoniation, uses water absorbing ammonia.
Further, step 5) in the weight ratio of filtrate and monose be 20-30：5-8.
Applicant proves that filtrate is 20-30 with the weight ratio of monose by lot of experiments：During 5-8, lignin copolymerization is formed
The mouthfeel of thing is optimal.
Further, step 6) in adjust pH to 4.5-6.0 with sodium carbonate or sodium acid carbonate.
Further, step 6) in lignin copolymer, cellulose, hemicellulose and starch mixed proportion be 1:1.3-
1.8:1.5-2.0:2.5-3.0。
Aforementioned proportion mixing enables to prepare dietary fiber mouth and see reach most preferably.
The present invention compared with prior art, has the following advantages and advantages：
1 present invention can effectively lower temperature during steam explosion by adding liquefied ammonia, liquefied ammonia during steam explosion, and can
Guarantee the mouthfeel of the dietary fiber of demolition effect and preparation, because temperature during liquefied ammonia steam explosion is less than 100 DEG C, equipment is wanted
Reduction is asked, and improves the security of steam explosion.
2nd, the present invention forms lignin copolymer, the strand of lignin by the way that lignin and monose are carried out into polycondensation reaction
Increase, molecular weight increase is changed into the filament with certain lines from original unbodied granular structure, can not only increase
Plus chewy texture, strengthen mouthfeel, and hydrophobicity can be improved.
3rd, the lignin copolymer of preparation, cellulose, hemicellulose and starch are carried out mixing and obtain meals by the present invention
Fiber not only increases the gas porosity of dietary fiber in stalk, and prepares lignin copolymer because by original unbodied powder
Shape structure is changed into the filament with certain lines and improves mouthfeel, and then, the dietary fiber prepared by the present invention has very
Good mouthfeel.
Specific embodiment
To make the object, technical solutions and advantages of the present invention become more apparent, with reference to embodiment, to present invention work
Further to describe in detail, exemplary embodiment and its explanation of the invention is only used for explaining the present invention, is not intended as to this
The restriction of invention.
Embodiment 1：
The method that liquefied ammonia steam puffed stalk prepares dietary fiber, comprises the following steps：
1), stalk adds liquefied ammonia to carry out steam explosion at 80 DEG C and obtains steam explosion product；
2), liquid ammonia recovery, steam explosion product is washed, and takes off hemicellulose, is filtered, and obtains the filter containing hemicellulose
The filter residue of liquid, containing cellulose and lignin；
Liquid ammonia recovery with step：Heating liquefied ammonia is changed into ammonia, and then hot blast removes deammoniation, uses water absorbing ammonia；
3), to step 2) in the filtrate that obtains add ethanol, soluble hemicellulose precipitation is filtered, and obtains hemicellulose；
4), by step 2) obtain filter residue ethanol boiling, filter, obtain the filtrate containing ethanol and lignin, contain
The filter residue of cellulose；
5), by step 4) filtrate that obtains adds hydrochloric acid, and it is 5.0 to adjust pH value, adds monose graft copolymerization, is filtered, filter residue
For lignin copolymer, wherein, filtrate is 20 with the weight ratio of monose：8；
6), by step 5) obtain lignin copolymer, step 4) obtain cellulose, step 3 obtain hemicellulose
And starch carries out mixing and obtains dietary fiber, and pH is adjusted to 4.5 with sodium carbonate or sodium acid carbonate, wherein, lignin copolymer,
The mixed proportion of cellulose, hemicellulose and starch is 1:1.3:1.5:2.5.
Embodiment 2：
The method that liquefied ammonia steam puffed stalk prepares dietary fiber, comprises the following steps：
1), stalk adds liquefied ammonia to carry out steam explosion at 90 DEG C and obtains steam explosion product；
2), liquid ammonia recovery, steam explosion product is washed, and takes off hemicellulose, is filtered, and obtains the filter containing hemicellulose
The filter residue of liquid, containing cellulose and lignin；
Liquid ammonia recovery with step：Heating liquefied ammonia is changed into ammonia, and then hot blast removes deammoniation, uses water absorbing ammonia；
3), to step 2) in the filtrate that obtains add ethanol, soluble hemicellulose precipitation is filtered, and obtains hemicellulose；
4), by step 2) obtain filter residue ethanol boiling, filter, obtain the filtrate containing ethanol and lignin, contain
The filter residue of cellulose；
5), by step 4) filtrate that obtains adds hydrochloric acid, and it is 6.0 to adjust pH value, adds monose graft copolymerization, is filtered, filter residue
For lignin copolymer, wherein, filtrate is 30 with the weight ratio of monose：5；
6), by step 5) obtain lignin copolymer, step 4) obtain cellulose, step 3 obtain hemicellulose
And starch carries out mixing and obtains dietary fiber, and pH is adjusted to 6.0 with sodium carbonate or sodium acid carbonate, wherein, lignin copolymer,
The mixed proportion of cellulose, hemicellulose and starch is 1:1.8:2.0:3.0.
Embodiment 3：
The method that liquefied ammonia steam puffed stalk prepares dietary fiber, comprises the following steps：
1), stalk adds liquefied ammonia to carry out steam explosion at 85 DEG C and obtains steam explosion product；
2), liquid ammonia recovery, steam explosion product is washed, and takes off hemicellulose, is filtered, and obtains the filter containing hemicellulose
The filter residue of liquid, containing cellulose and lignin；
Liquid ammonia recovery with step：Heating liquefied ammonia is changed into ammonia, and then hot blast removes deammoniation, uses water absorbing ammonia；
3), to step 2) in the filtrate that obtains add ethanol, soluble hemicellulose precipitation is filtered, and obtains hemicellulose；
4), by step 2) obtain filter residue ethanol boiling, filter, obtain the filtrate containing ethanol and lignin, contain
The filter residue of cellulose；
5), by step 4) filtrate that obtains adds hydrochloric acid, and it is 5.5 to adjust pH value, adds monose graft copolymerization, is filtered, filter residue
For lignin copolymer, wherein, filtrate is 25 with the weight ratio of monose：6；
6), by step 5) obtain lignin copolymer, step 4) obtain cellulose, step 3 obtain hemicellulose
And starch carries out mixing and obtains dietary fiber, and pH is adjusted to 5.0 with sodium carbonate or sodium acid carbonate, wherein, lignin copolymer,
The mixed proportion of cellulose, hemicellulose and starch is 1:1.5:1.8:2.8.
Above-described specific embodiment, has been carried out further to the purpose of the present invention, technical scheme and beneficial effect
Describe in detail, should be understood that the specific embodiment that the foregoing is only the present invention, be not intended to limit the present invention
Protection domain, all any modification, equivalent substitution and improvements within the spirit and principles in the present invention, done etc. all should include
Within protection scope of the present invention.
Claims (6)
1. the method that liquefied ammonia steam puffed stalk prepares dietary fiber, it is characterised in that comprise the following steps：
1), stalk adds liquefied ammonia to carry out steam explosion at 80-90 DEG C and obtains steam explosion product；
2), liquid ammonia recovery, steam explosion product is washed, and takes off hemicellulose, is filtered, and is obtained the filtrate containing hemicellulose, is contained
The filter residue of cellulose and lignin；
3), to step 2) in the filtrate that obtains add ethanol, soluble hemicellulose precipitation is filtered, and obtains hemicellulose；
4), by step 2) obtain filter residue ethanol boiling, filter, obtain the filtrate containing ethanol and lignin, contain fiber
The filter residue of element；
5), by step 4) obtain filtrate in acid condition with monose graft copolymerization, filter, filter residue be lignin copolymer；
6), by step 5) obtain lignin copolymer, step 4) obtain cellulose, step 3 obtain hemicellulose and
Starch carries out mixing and obtains dietary fiber.
2. the method that liquefied ammonia steam puffed stalk according to claim 1 prepares dietary fiber, it is characterised in that the acid is salt
Acid, step 5) in acid condition be pH value be 5.0-6.0.
3. the method that liquefied ammonia steam puffed stalk according to claim 1 prepares dietary fiber, it is characterised in that liquid ammonia recovery
With step：Heating liquefied ammonia is changed into ammonia, and then hot blast removes deammoniation, uses water absorbing ammonia.
4. the method that liquefied ammonia steam puffed stalk according to claim 1 prepares dietary fiber, it is characterised in that step 5) middle filter
Liquid is 20-30 with the weight ratio of monose：5-8.
5. the method that liquefied ammonia steam puffed stalk according to claim 1 prepares dietary fiber, it is characterised in that step 6) middle use
Sodium carbonate or sodium acid carbonate adjust pH to 4.5-6.0.
6. the method that liquefied ammonia steam puffed stalk according to claim 1 prepares dietary fiber, it is characterised in that step 6) in wood
The mixed proportion of quality copolymer, cellulose, hemicellulose and starch is 1:1.3-1.8:1.5-2.0:2.5-3.0.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201710040534.0A CN106617111A (en) | 2017-01-20 | 2017-01-20 | Method for preparing dietary fiber from liquid ammonia steam exploded straw |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710040534.0A CN106617111A (en) | 2017-01-20 | 2017-01-20 | Method for preparing dietary fiber from liquid ammonia steam exploded straw |
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| CN201710040534.0A Withdrawn CN106617111A (en) | 2017-01-20 | 2017-01-20 | Method for preparing dietary fiber from liquid ammonia steam exploded straw |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106962949A (en) * | 2017-05-18 | 2017-07-21 | 成都衔石科技有限公司 | A kind of wash-off method of the stalk dietary fiber based on alkali cleaning |
| CN107125777A (en) * | 2017-05-18 | 2017-09-05 | 成都衔石科技有限公司 | A kind of preprocess method for preparing stalk dietary fiber |
| CN107411105A (en) * | 2017-05-18 | 2017-12-01 | 成都衔石科技有限公司 | A kind of wash-off method of the stalk dietary fiber based on pickling |
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| CN101463091A (en) * | 2009-01-16 | 2009-06-24 | 中国科学院过程工程研究所 | Method for separating stalk carboxymethylation components and preparing stalk carboxymethyl cellulose |
| CN102660884A (en) * | 2012-05-11 | 2012-09-12 | 南开大学 | Method for producing hemicellulose by treating straw by ammonia water steam explosion technology |
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| CN101463091A (en) * | 2009-01-16 | 2009-06-24 | 中国科学院过程工程研究所 | Method for separating stalk carboxymethylation components and preparing stalk carboxymethyl cellulose |
| CN102660884A (en) * | 2012-05-11 | 2012-09-12 | 南开大学 | Method for producing hemicellulose by treating straw by ammonia water steam explosion technology |
| CN105431466A (en) * | 2013-06-26 | 2016-03-23 | 植物材料工业公司 | Phenolic resin obtained by polycondensation of formaldehyde, phenol and lignin |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106962949A (en) * | 2017-05-18 | 2017-07-21 | 成都衔石科技有限公司 | A kind of wash-off method of the stalk dietary fiber based on alkali cleaning |
| CN107125777A (en) * | 2017-05-18 | 2017-09-05 | 成都衔石科技有限公司 | A kind of preprocess method for preparing stalk dietary fiber |
| CN107411105A (en) * | 2017-05-18 | 2017-12-01 | 成都衔石科技有限公司 | A kind of wash-off method of the stalk dietary fiber based on pickling |
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Application publication date: 20170510 |