CN103965365B - A kind of preparation method of apple residue Microcrystalline Cellulose - Google Patents
A kind of preparation method of apple residue Microcrystalline Cellulose Download PDFInfo
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Abstract
The present invention relates to a kind of preparation method of apple residue Microcrystalline Cellulose, the method comprises the following steps: (1) that apple residue raw material hydrochloric acid soln swelling treatment is centrifugal, obtains supernatant A and throw out A respectively; (2) supernatant A obtains crude pectin through concentrating under reduced pressure, precipitation, dry separation; (3) adding distil water after throw out A is washed to pH value neutrality, glacial acetic acid-Textone be pre-mixed liquid, drain solution and obtain filter residue; (4) after filter residue is washed to pH value neutrality, centrifugal by sodium hydroxide solution swelling treatment, obtain supernatant liquor B and sediment B respectively; (5) supernatant liquor B is through concentrating under reduced pressure, precipitation, crushed after being dried, obtains hemicellulose; (6) sediment B is centrifugal, dry after decolouring, swelling treatment, obtains water-insoluble apple residue Mierocrystalline cellulose; (7) the swelling rear enzymolysis of water-insoluble apple residue Mierocrystalline cellulose, obtains enzymolysis Mierocrystalline cellulose; (8) enzymolysis Mierocrystalline cellulose is through dehydration, dry, pulverizing, gets product.Present invention process is simple, cost is low, the products obtained therefrom polymerization degree is good.
Description
Technical field
The present invention relates to a kind of preparation method of Microcrystalline Cellulose, particularly relate to a kind of preparation method of apple residue Microcrystalline Cellulose.
Background technology
Apple residue is the by product of fruit juice production industry, and protein content is low, and crude fiber content is high, and containing abundant carbohydrate and mineral substance.Fresh fruit slag has the biological degradability of height, if do not processed, rapidly fermentation rotting and give out a foul smell, as wantonly entered in physical environment, can cause water pollution, destruction ecotope, therefore rationally dispose, to fully utilize apple residue resource extremely urgent.China produces fresh fruit per year and has exceeded 2,000 ten thousand tons, and apple residue accounts for 20% ~ 25% of processing apple, and the pomace produced in processing has just exceeded more than 100 ten thousand tons.If this reward for writing or painting source can obtain Appropriate application, not only can stop environmental pollution, also will bring considerable economic benefit.
Developed country's research apple deep processing time is longer, utilizes apple residue to produce pectin, produces alcohol, citric acid, Mierocrystalline cellulose and dietary fiber food, fermentation production of protein matter etc.In recent years, China had also recognized that apple residue resource is to the importance of comprehensive utilization, had dropped into a large amount of manpower and materials, utilized with the diversity realizing resource and obtained maximum economic benefit.Especially from apple residue, extract Mierocrystalline cellulose be prepared into Microcrystalline Cellulose, apple residue resource gives an important channel of comprehensive utilization especially.
Microcrystalline Cellulose (Microcrystallinestallinecellulose; MCC) be native cellulolytic to the free flowable imperceptible corynebacterium of levelling-off DP or powdery porous shape particle; color is white or near-white; odorless, tasteless; granular size is generally at 20 ~ 80 μm; levelling-off DP (LODP) is 15 ~ 375; water insoluble, diluted acid, organic solvent and grease; be partly dissolved in dilute alkaline soln, moisten and rise, in carboxymethylation, acetylize, esterification process, there is higher reactivity worth.
Microcrystalline cellulose have fine powder and colloidal two kinds of principal modes, and the former is for sorbent material or tackiness agent, and the latter is as the dispersion agent in liquid.Powdered Microcrystalline Cellulose, as anti-caking agent, having the effect of anti-caking and help flowing, being also used as the carrier of essence and spice oil because having oil absorbency.The multifunctionality of colloidal Microcrystalline Cellulose shows: control ice crystal in the stable and peptizing agent of emulsification and froth stability, high temperatures, non-nutritive weighting material and thickening material, liquid, suspension agent, frozen food confection and formed.In addition, Microcrystalline Cellulose can be used as the food fiber in heath food, also can be used as function food fiber.Due to the multiple character of Microcrystalline Cellulose, medicine, food, makeup and light industry industry are widely used at present.
Multidigit investigator is had to be studied Microcrystalline Cellulose at present, as beautiful in Russell is that raw material produces Microcrystalline Cellulose through hydrochloric acid hydrolysis preparation with bagasse pulp, the requirement of quality product conformance with standard, wherein yield is 82.18%, the polymerization degree is 120, its amounts of particles distribution uniform, particle diameter is less, respond well through application test.Lv Yanbei is that material acidolysis prepares Microcrystalline Cellulose with soybean hulls, obtains good Microcrystalline Cellulose product.Yuan Yi etc. are to extract the Dioscorea nipponica Mak. Ningpo Yam Rhizome residue after saponin(e for raw material, and separation and purification obtains Mierocrystalline cellulose, then through the obtained Microcrystalline Cellulose of hydrolysis.After measured, in sample, MCC is 91.7%, and the polymerization degree is 164, and degree of crystallinity is 77.1%, and mean particle size is 23.21 μm.
Summary of the invention
Technical problem to be solved by this invention is to provide the preparation method of the apple residue Microcrystalline Cellulose that a kind of technique is simple, cost is low, the products obtained therefrom polymerization degree is good.
For solving the problem, the preparation method of a kind of apple residue Microcrystalline Cellulose of the present invention, comprises the following steps:
By apple residue raw material by the liquid ratio massfraction of 16 ~ 18mL/g be 1.5% ~ 2.5% hydrochloric acid soln swelling, obtain solute A; Described solute A is centrifugal after constant temperature process 63.5min ~ 66.5min at 77 ~ 79 DEG C of temperature, obtains supernatant A and throw out A respectively;
(2) described supernatant A is separated obtains crude pectin through concentrating under reduced pressure, dehydrated alcohol precipitation, spraying dry successively;
(3) described throw out A is washed to pH value neutrality, then distilled water is added with the solid-liquid ratio of 1g:8 ~ 12mL, what add 15mL glacial acetic acid and 16g Textone by every 1L mixed system again to be pre-mixed after liquid at 70 ~ 80 DEG C of constant temperature process 1 ~ 2h, obtains filter residue after draining solution;
(4) described filter residue drains away the water after being washed to pH value neutrality, swelling by the liquid ratio of 11 ~ 13mL/g with the sodium hydroxide solution of massfraction 7% ~ 9%, obtains solute B; Described solute B is centrifugal after isothermal holding 88min ~ 92min at 88 DEG C ~ 92 DEG C temperature, obtains supernatant liquor B and sediment B respectively;
Described supernatant liquor B successively through concentrating under reduced pressure, dehydrated alcohol precipitation, 55 ~ 65 DEG C be dried to constant weight after pulverize, obtaining granularity is 150 ~ 200 object hemicelluloses;
(6) described sediment B is the H of 4 ~ 5% with the stirring velocity of 45 ~ 55r/min, by the liquid ratio volumetric concentration of 3 ~ 5mL/g
2o
2in the decolouring of 75 ~ 85 DEG C of heating in water bath, be the H of 4 ~ 5% by volumetric concentration after 5min
2o
2swelling by the liquid ratio of 3mL/g ~ 5mL/g, obtain solute C; Described solute C is centrifugal process 175min ~ 185min at 79 DEG C ~ 81 DEG C temperature after, at 35 ~ 50 DEG C of drying 8 ~ 12h, obtains water-insoluble apple residue Mierocrystalline cellulose;
(7) the solid-liquid ratio adding distil water pressing 1g:40 ~ 60mL in described water-insoluble apple residue Mierocrystalline cellulose is swelling, obtains solute D; The glacial acetic acid solution that pH value is 2.0 ~ 2.8 is dropwise added in described solute D, make its pH value to 4.1 ~ 5.0, then according to the water-insoluble apple residue Mierocrystalline cellulose quality weighed, 18 ~ 35U cellulose complex enzyme is added by every gram of dried fibres element, this cellulose complex enzyme pH is the citric acid/sodium citrate buffer solution of 4.0 ~ 5.0, then mix with described water-insoluble apple residue Mierocrystalline cellulose, again at 45 ~ 55 DEG C of insulation enzymolysis 5 ~ 7h, and enzymolysis process stirs once every 15 ~ 20min, obtains enzymolysis Mierocrystalline cellulose;
(8) described enzymolysis Mierocrystalline cellulose is pulverized successively after centrifuge dehydration, 40 ~ 60 DEG C of drying 8 ~ 12h, and obtaining granularity is 150 ~ 250 object finished product Microcrystalline Celluloses.
Described step (1) in apple residue raw material refer to the pomace of the broken rear mistake 40 mesh sieve gained of the biffins ground-slag of water content less than 8%; Or the apple wet slag of water content less than 10% is after temperature is the distilled water submergence 3 ~ 8min of 25 ~ 35 DEG C, and the pomace of the gained that dewaters with the centrifugal 8 ~ 12min of the speed of 3000 ~ 5000r/min.
Described step (2) or described step (5) in the condition of concentrating under reduced pressure refer to that vacuum tightness is 0.5 ~ 0.7MPa, vaporization temperature is 35 DEG C of insulations, and solvent recuperation volume ratio is 0.80 ~ 0.85.
Described step (2) in spray-dired condition be feeding temperature 198 DEG C ~ 221 DEG C, drop temperature 153 DEG C ~ 156 DEG C.
Described step (7) in pH be 4.0 ~ 5.0 citric acid/sodium citrate damping fluid refer to first by 21.01 grams of citric acid (C
6h
8o
7.H
2o) dissolve in 1L pure water and obtain 0.1mol/L citric acid solution; Then by 29.41 grams of Trisodium Citrate (Na
3c
6h
5o
7.2H
2o) dissolve in 1L pure water and obtain 0.1mol/L sodium citrate solution; Finally described 7.2mL ~ 12.7mL citric acid solution and described 7.3mL ~ 12.8mL sodium citrate solution are mixed and get final product.
The present invention compared with prior art has the following advantages:
1, products obtained therefrom of the present invention is best in quality, and the Microcrystalline Cellulose of infrared spectra display preparation has typical cellulose character peak, and chemical constitution is similar to the finished product Microcrystalline Cellulose as standard substance; There are depression and crackle in ultrastructure surface, and its short texture is little with standard substance difference; Its color, structural state, carbohydrate content, loss on drying, pH, ignition residue, the water solubles, all in the scope that standard specifies, reach the quality standard of commodity cotton Microcrystalline Cellulose substantially.
(1) SEM can observe the surface tissue of material:
Can find out that commodity cotton Microcrystalline Cellulose is long narrow shape fiber linear structure by Fig. 1 ~ 2, apple residue Microcrystalline Cellulose is irregular fibrous texture, and the profile of two kinds of particulates has similarity.
The microcrystalline cellulose crude granule of the cotton Microcrystalline Cellulose of Fig. 3 ~ 4 display of commodity is bar-shaped to the length of microcrystalline cellulose crude granule all in similar of apple residue Microcrystalline Cellulose, and concave-convex surface is more similar.
In Fig. 5, the fiber grain of commodity cotton Microcrystalline Cellulose is larger, smooth surface, caves in less; Scanning electron microscope (SEM) photograph display in apple residue Microcrystalline Cellulose × 10000 in Fig. 6, there are a small amount of depression and crackle in surface, illustrates that cellulose treatment changes the surface tissue of sample, and specific surface area increases, and its short texture is little with commodity cotton Microcrystalline Cellulose difference.
(2) infrared spectra display apple residue Microcrystalline Cellulose has typical cellulose character peak, chemical constitution similar to commodity cotton Microcrystalline Cellulose (see Fig. 7 ~ 8).
As can be seen from Fig. 7 ~ 8, all there are two main absorption sections in all samples, and one is 700 ~ 1800cm of low wavelength
-1, another is 2700 ~ 3500cm
-1slightly high wavelength period.Meanwhile, commodity cotton Microcrystalline Cellulose and apple residue Microcrystalline Cellulose sample all have typical cellulose character peak.
3352 ~ 3419cm-1 is O-H stretching vibration absorption band, the O-H absorption band of commodity Microcrystalline Cellulose appears at 3352cm-1 place, and apple residue Microcrystalline Cellulose is near 3418cm-1, illustrate that the O-H absorption band of apple residue Microcrystalline Cellulose is wider than commodity cotton Microcrystalline Cellulose.The uronic acid carbonyl absorption peak at 1730cm-1 place is the characteristic peak of hemicellulose, and as can be seen from the figure, commodity cotton Microcrystalline Cellulose and apple residue Microcrystalline Cellulose are herein all without absorption peak, therefore two kinds of Microcrystalline Celluloses are not containing hemicellulose; 1640cm-1 place absorption band is the stretching vibration of-C=O conjugation substituted aroma ketone, for lignin degradation produces; 1430cm-1 place is the vibration of-CH2, and above-mentioned two kinds of absorption peak commodity cotton Microcrystalline Celluloses and apple residue Microcrystalline Cellulose all exist.The symmetrical C-H flexural vibration peak of methoxyl group appears at 1370cm-1 place, and commodity cotton Microcrystalline Cellulose is stronger than this absorption peak of apple residue Microcrystalline Cellulose.The stretching vibration of what 1060 ~ 1032cm-1 represented is C-O ether, methoxyl group and β-O-4, commodity cotton Microcrystalline Cellulose absorption peak in contrast appears at 1060cm-1, and apple residue Microcrystalline Cellulose is near 1032cm-1, slightly different.
In sum, the apple residue Microcrystalline Cellulose sample that obtains of enzymolysis and commodity cotton Microcrystalline Cellulose chemical structure basic simlarity.
(3) the foodstuff additive Microcrystalline Cellulose product standard (in March, 2011 bulletin) formulated with reference to the People's Republic of China Ministry of Health is tested to the apple residue Microcrystalline Cellulose of gained of the present invention, its color, structural state, carbohydrate content, loss on drying, pH, ignition residue, the water solubles are all in the scope that standard specifies, quality reaches standard substantially, and result is as table 1.
Table 1 Microcrystalline Cellulose evaluation index
As can be seen from Table 1, apple residue Microcrystalline Cellulose meets the foodstuff additive standard that Ministry of Health of the People's Republic of China formulates substantially, can be used as foodstuff additive.
2, because enzymatic hydrolysis condition has been carried out reasonably optimizing by the present invention, therefore, make the products obtained therefrom polymerization degree compared with the polymerization degree close to commodity cotton Microcrystalline Cellulose, retention ability, swelling property are better, make it have good suspension stability after adding fruit juice, thus make fruit juice system even.
3, because product of the present invention is by the control of the conditions such as solid-liquid ratio, enzymolysis time, enzyme class, enzyme concentration, therefore, products obtained therefrom uniform particles, stable in properties, color and luster are better, free from extraneous odour.
4, present invention process and simple to operate, easily grasp, production cost is low, pollutes little.Products obtained therefrom can be used as non-nutritive part in food, as the food fiber in heath food.In addition, also can be used to ice crystal in the glidant of some ertruding food product, non-nutritive weighting material and thickening material, the stable and peptizing agent of liquid, suspension agent, control frozen food confection formed.
Accompanying drawing explanation
Below in conjunction with accompanying drawing, the specific embodiment of the present invention is described in further detail.
Fig. 1 is commodity cotton Microcrystalline Cellulose × 50 scanning electron microscope (SEM) photographs.
Fig. 2 is apple residue Microcrystalline Cellulose × 50 of the present invention scanning electron microscope (SEM) photographs.
Fig. 3 is commodity cotton Microcrystalline Cellulose × 5000 scanning electron microscope (SEM) photographs.
Fig. 4 is apple residue Microcrystalline Cellulose × 5000 of the present invention scanning electron microscope (SEM) photographs.
Fig. 5 is commodity cotton Microcrystalline Cellulose × 10000 scanning electron microscope (SEM) photographs.
Fig. 6 is apple residue Microcrystalline Cellulose × 10000 of the present invention scanning electron microscope (SEM) photographs.
Fig. 7 is the infrared sight spectrogram of commodity cotton Microcrystalline Cellulose.
Fig. 8 is the infrared sight spectrogram of apple residue Microcrystalline Cellulose of the present invention.
Embodiment
embodiment 1a preparation method for apple residue Microcrystalline Cellulose, comprises the following steps:
By apple residue raw material by the liquid ratio massfraction of 16mL/g be 1.5% hydrochloric acid soln swelling, obtain solute A; Solute A is constant temperature process 66.5min at 77 DEG C of temperature, then after the centrifugal 6min of 3000r/min, obtains supernatant A and throw out A respectively.
Wherein: apple residue raw material refers to the pomace of the broken rear mistake 40 mesh sieve gained of the biffins ground-slag of water content 6 ~ 8%.
Supernatant A vacuum tightness be 0.5MPa, vaporization temperature is 35 DEG C of insulations, solvent recuperation volume ratio be the condition of 0.80 under concentrating under reduced pressure, obtain concentrated solution A, the dehydrated alcohol of its 3 times of volumes is added in this concentrated solution A, carry out solid-liquid separation with the centrifugal 8min of the rotating speed of 1400rpm after left at room temperature precipitation 8min, obtain solids A; Solids A carries out spraying dry to constant weight under the condition of feeding temperature 198 DEG C, drop temperature 153 DEG C, obtains crude pectin.
(3) throw out A is washed to pH value neutrality, then adds distilled water with the solid-liquid ratio of 1g:8mL, then add 15mL glacial acetic acid and 16g Textone by every 1L mixed system to be pre-mixed after liquid at 70 DEG C of constant temperature process 2h, remove xylogen, after draining solution, obtain filter residue.
(4) filter residue drains away the water after being washed to pH value neutrality, and the liquid ratio of pressing 11mL/g with the sodium hydroxide solution of massfraction 7% is swelling, obtains solute B; Solute B is isothermal holding 92min at 88 DEG C of temperature, then after the centrifugal 6min of 3000r/min, obtains supernatant liquor B and sediment B respectively.
Supernatant liquor B vacuum tightness be 0.5MPa, vaporization temperature is 35 DEG C of insulations, solvent recuperation volume ratio be the condition of 0.80 under concentrating under reduced pressure, obtain concentrated solution B, the dehydrated alcohol of its 3 times of volumes is added in this concentrated solution B, carry out solid-liquid separation with the centrifugal 8min of the rotating speed of 1400rpm after left at room temperature precipitation 8min, obtain solids B; Solids B pulverizes after being dried to constant weight at 55 DEG C, and obtaining granularity is 150 object hemicelluloses.
(6) sediment B is the H of 4% with the stirring velocity of 45r/min, by the liquid ratio volumetric concentration of 3mL/g
2o
2in the decolouring of 75 DEG C of heating in water bath, be the H of 4% by volumetric concentration after 5min
2o
2swelling by the liquid ratio of 3mL/g, obtain solute C; Solute C processes 185min at 79 DEG C of temperature, then after the centrifugal 6min of 3000r/min, at 35 DEG C of dry 12h, obtains water-insoluble apple residue Mierocrystalline cellulose.
(7) the solid-liquid ratio adding distil water pressing 1g:40mL in water-insoluble apple residue Mierocrystalline cellulose is swelling, obtains solute D; The glacial acetic acid solution that pH value is 2.0 is dropwise added in solute D, make its pH value to 4.1, then according to the water-insoluble apple residue Mierocrystalline cellulose quality weighed, 18U cellulose complex enzyme is added by every gram of dried fibres element, this cellulose complex enzyme pH is the citric acid/sodium citrate buffer solution of 4.0, then mixes with water-insoluble apple residue Mierocrystalline cellulose, then at 45 DEG C of insulation enzymolysis 7h, and enzymolysis process stirs once every 15min, obtains enzymolysis Mierocrystalline cellulose.
Wherein: pH be 4.0 citric acid/sodium citrate damping fluid refer to first by 21.01 grams of citric acid (C
6h
8o
7.H
2o) dissolve in 1L pure water and obtain 0.1mol/L citric acid solution; Then by 29.41 grams of Trisodium Citrate (Na
3c
6h
5o
7.2H
2o) dissolve in 1L pure water and obtain 0.1mol/L sodium citrate solution; Finally 12.7mL citric acid solution and 7.3mL sodium citrate solution are mixed and get final product.
(8) enzymolysis Mierocrystalline cellulose is pulverized successively after 3000r/min centrifugal 6min dehydration, 40 DEG C of dry 12h, and obtaining granularity is 150 object finished product Microcrystalline Celluloses.
embodiment 2a preparation method for apple residue Microcrystalline Cellulose, comprises the following steps:
By apple residue raw material by the liquid ratio massfraction of 18mL/g be 2.5% hydrochloric acid soln swelling, obtain solute A; Solute A is constant temperature process 63.5min at 79 DEG C of temperature, then after the centrifugal 4min of 5000r/min, obtains supernatant A and throw out A respectively.
Wherein: apple residue raw material refers to the pomace of the broken rear mistake 40 mesh sieve gained of the biffins ground-slag of water content 4 ~ 6%.
Supernatant A vacuum tightness be 0.7MPa, vaporization temperature is 35 DEG C of insulations, solvent recuperation volume ratio be the condition of 0.85 under concentrating under reduced pressure, obtain concentrated solution A, the dehydrated alcohol of its 6 times of volumes is added in this concentrated solution A, carry out solid-liquid separation with the centrifugal 3min of the rotating speed of 1600rpm after left at room temperature precipitation 12min, obtain solids A; Solids A carries out spraying dry to constant weight under the condition of feeding temperature 221 DEG C, drop temperature 156 DEG C, obtains crude pectin.
(3) throw out A is washed to pH value neutrality, then distilled water is added with the solid-liquid ratio of 1g:12mL, what add 15mL glacial acetic acid and 16g Textone by every 1L mixed system again to be pre-mixed after liquid at 80 DEG C of constant temperature process 1h, removes xylogen, obtains filter residue after draining solution.
(4) filter residue drains away the water after being washed to pH value neutrality, and the liquid ratio of pressing 13mL/g with the sodium hydroxide solution of massfraction 9% is swelling, obtains solute B; Solute B is isothermal holding 88min at 92 DEG C of temperature, then after the centrifugal 4min of 5000r/min, obtains supernatant liquor B and sediment B respectively.
Supernatant liquor B vacuum tightness be 0.7MPa, vaporization temperature is 35 DEG C of insulations, solvent recuperation volume ratio be the condition of 0.85 under concentrating under reduced pressure, obtain concentrated solution B, the dehydrated alcohol of its 6 times of volumes is added in this concentrated solution B, carry out solid-liquid separation with the centrifugal 3min of the rotating speed of 1600rpm after left at room temperature precipitation 12min, obtain solids B; Solids B pulverizes after being dried to constant weight at 65 DEG C, and obtaining granularity is 200 object hemicelluloses.
(6) sediment B is the H of 5% with the stirring velocity of 55r/min, by the liquid ratio volumetric concentration of 5mL/g
2o
2in the decolouring of 85 DEG C of heating in water bath, be the H of 5% by volumetric concentration after 5min
2o
2swelling by the liquid ratio of 5mL/g, obtain solute C; Solute C is centrifugal process 175min at 81 DEG C of temperature after, at 50 DEG C of dry 8h, obtains water-insoluble apple residue Mierocrystalline cellulose.
(7) the solid-liquid ratio adding distil water pressing 1g:60mL in water-insoluble apple residue Mierocrystalline cellulose is swelling, obtains solute D; The glacial acetic acid solution that pH value is 2.8 is dropwise added in solute D, make its pH value to 5.0, then according to the water-insoluble apple residue Mierocrystalline cellulose quality weighed, 35U cellulose complex enzyme is added by every gram of dried fibres element, this cellulose complex enzyme pH is the citric acid/sodium citrate buffer solution of 5.0, then mixes with water-insoluble apple residue Mierocrystalline cellulose, then at 55 DEG C of insulation enzymolysis 5h, and enzymolysis process stirs once every 20min, obtains enzymolysis Mierocrystalline cellulose.
Wherein: pH be 5.0 citric acid/sodium citrate damping fluid refer to first by 21.01 grams of citric acid (C
6h
8o
7.H
2o) dissolve in 1L pure water and obtain 0.1mol/L citric acid solution; Then by 29.41 grams of Trisodium Citrate (Na
3c
6h
5o
7.2H
2o) dissolve in 1L pure water and obtain 0.1mol/L sodium citrate solution; Finally 7.2mL citric acid solution and 12.8mL sodium citrate solution are mixed and get final product.
(8) enzymolysis Mierocrystalline cellulose is pulverized successively after 5000r/min centrifugal 4min dehydration, 60 DEG C of dry 8h, and obtaining granularity is 250 object finished product Microcrystalline Celluloses.
embodiment 3a preparation method for apple residue Microcrystalline Cellulose, comprises the following steps:
By apple residue raw material by the liquid ratio massfraction of 17mL/g be 2% hydrochloric acid soln swelling, obtain solute A; Solute A is constant temperature process 65.5min at 78 DEG C of temperature, then after the centrifugal 5min of 4000r/min, obtains supernatant A and throw out A respectively.
Wherein: apple residue raw material refers to the pomace of the broken rear mistake 40 mesh sieve gained of the biffins ground-slag of water content less than 4%.
Supernatant A vacuum tightness be 0.6MPa, vaporization temperature is 35 DEG C of insulations, solvent recuperation volume ratio be the condition of 0.82 under concentrating under reduced pressure, obtain concentrated solution A, the dehydrated alcohol of its 4 times of volumes is added in this concentrated solution A, carry out solid-liquid separation with the centrifugal 5min of the rotating speed of 1500rpm after left at room temperature precipitation 10min, obtain solids A; Solids A carries out spraying dry to constant weight under the condition of feeding temperature 210 DEG C, drop temperature 154 DEG C, obtains crude pectin.
(3) throw out A is washed to pH value neutrality, then distilled water is added with the solid-liquid ratio of 1g:10mL, what add 15mL glacial acetic acid and 16g Textone by every 1L mixed system again to be pre-mixed after liquid at 75 DEG C of constant temperature process 1.5h, removes xylogen, obtains filter residue after draining solution.
(4) filter residue drains away the water after being washed to pH value neutrality, and the liquid ratio of pressing 12mL/g with the sodium hydroxide solution of massfraction 8% is swelling, obtains solute B; Solute B is isothermal holding 90min at 90 DEG C of temperature, then after the centrifugal 5min of 4000r/min, obtains supernatant liquor B and sediment B respectively.
Supernatant liquor B vacuum tightness be 0.6MPa, vaporization temperature is 35 DEG C of insulations, solvent recuperation volume ratio be the condition of 0.82 under concentrating under reduced pressure, obtain concentrated solution B, the dehydrated alcohol of its 4 times of volumes is added in this concentrated solution B, carry out solid-liquid separation with the centrifugal 5min of the rotating speed of 1500rpm after left at room temperature precipitation 10min, obtain solids B; Solids B pulverizes after being dried to constant weight at 60 DEG C, and obtaining granularity is 180 object hemicelluloses.
(6) sediment B is the H of 4.5% with the stirring velocity of 50r/min, by the liquid ratio volumetric concentration of 4mL/g
2o
2in the decolouring of 80 DEG C of heating in water bath, be the H of 4.5% by volumetric concentration after 5min
2o
2swelling by the liquid ratio of 4mL/g, obtain solute C; Solute C is centrifugal process 180min at 80 DEG C of temperature after, at 40 DEG C of dry 10h, obtains water-insoluble apple residue Mierocrystalline cellulose.
(7) the solid-liquid ratio adding distil water pressing 1g:50mL in water-insoluble apple residue Mierocrystalline cellulose is swelling, obtains solute D; The glacial acetic acid solution that pH value is 2.4 is dropwise added in solute D, make its pH value to 4.5, then according to the water-insoluble apple residue Mierocrystalline cellulose quality weighed, 26U cellulose complex enzyme is added by every gram of dried fibres element, this cellulose complex enzyme pH is the citric acid/sodium citrate buffer solution of 4.5, then mixes with water-insoluble apple residue Mierocrystalline cellulose, then at 50 DEG C of insulation enzymolysis 6h, and enzymolysis process stirs once every 18min, obtains enzymolysis Mierocrystalline cellulose.
Wherein: pH be 4.5 citric acid/sodium citrate damping fluid refer to first by 21.01 grams of citric acid (C
6h
8o
7.H
2o) dissolve in 1L pure water and obtain 0.1mol/L citric acid solution; Then by 29.41 grams of Trisodium Citrate (Na
3c
6h
5o
7.2H
2o) dissolve in 1L pure water and obtain 0.1mol/L sodium citrate solution; Finally 9.9mL citric acid solution and 10.1mL sodium citrate solution are mixed and get final product.
(8) enzymolysis Mierocrystalline cellulose is pulverized successively after 4000r/min centrifugal 5min dehydration, 50 DEG C of dry 10h, and obtaining granularity is 200 object finished product Microcrystalline Celluloses.
embodiment 4a preparation method for apple residue Microcrystalline Cellulose, comprises the following steps:
By apple residue raw material by the liquid ratio massfraction of 16.5mL/g be 1.8% hydrochloric acid soln swelling, obtain solute A; Solute A is constant temperature process 64.5min at 77.5 DEG C of temperature, then after the centrifugal 6min of 3000r/min, obtains supernatant A and throw out A respectively.
Wherein: the apple wet slag of water content less than 10% is after the distilled water submergence 8min of 25 DEG C in temperature, and with the centrifugal 12min dehydration of the speed of 3000r/min, the pomace of the impurity such as soluble sugar and tannin gained in removing pomace.
Supernatant A vacuum tightness be 0.55MPa, vaporization temperature is 35 DEG C of insulations, solvent recuperation volume ratio be the condition of 0.81 under concentrating under reduced pressure, obtain concentrated solution A, the dehydrated alcohol of its 3.5 times of volumes is added in this concentrated solution A, carry out solid-liquid separation with the centrifugal 8min of the rotating speed of 1400rpm after left at room temperature precipitation 8min, obtain solids A; Solids A carries out spraying dry to constant weight under the condition of feeding temperature 200 DEG C, drop temperature 153 DEG C, obtains crude pectin.
(3) throw out A is washed to pH value neutrality, then adds distilled water with the solid-liquid ratio of 1g:9mL, then add 15mL glacial acetic acid and 16g Textone by every 1L mixed system to be pre-mixed after liquid at 72 DEG C of constant temperature process 1h, remove xylogen, after draining solution, obtain filter residue.
(4) filter residue drains away the water after being washed to pH value neutrality, and the liquid ratio of pressing 11.5mL/g with the sodium hydroxide solution of massfraction 7.5% is swelling, obtains solute B; Solute B is isothermal holding 89min at 89 DEG C of temperature, then after the centrifugal 6min of 3000r/min, obtains supernatant liquor B and sediment B respectively.
Supernatant liquor B vacuum tightness be 0.55MPa, vaporization temperature is 35 DEG C of insulations, solvent recuperation volume ratio be the condition of 0.81 under concentrating under reduced pressure, obtain concentrated solution B, the dehydrated alcohol of its 3.5 times of volumes is added in this concentrated solution B, carry out solid-liquid separation with the centrifugal 8min of the rotating speed of 1400rpm after left at room temperature precipitation 8min, obtain solids B; Solids B pulverizes after being dried to constant weight at 56 DEG C, and obtaining granularity is 150 object hemicelluloses.
(6) sediment B is the H of 4% with the stirring velocity of 45r/min, by the liquid ratio volumetric concentration of 3.5mL/g
2o
2in the decolouring of 75 DEG C of heating in water bath, be the H of 4% by volumetric concentration after 5min
2o
2swelling by the liquid ratio of 3.5mL/g, obtain solute C; Solute C is centrifugal process 178min at 79.5 DEG C of temperature after, at 35 DEG C of dry 12h, obtains water-insoluble apple residue Mierocrystalline cellulose.
(7) the solid-liquid ratio adding distil water pressing 1g:45mL in water-insoluble apple residue Mierocrystalline cellulose is swelling, obtains solute D; The glacial acetic acid solution that pH value is 2.2 is dropwise added in solute D, make its pH value to 4.3, then according to the water-insoluble apple residue Mierocrystalline cellulose quality weighed, 20U cellulose complex enzyme is added by every gram of dried fibres element, this cellulose complex enzyme pH is the citric acid/sodium citrate buffer solution of 4.0, then mixes with water-insoluble apple residue Mierocrystalline cellulose, then at 45 DEG C of insulation enzymolysis 7h, and enzymolysis process stirs once every 15min, obtains enzymolysis Mierocrystalline cellulose.
Wherein: pH be 4.0 citric acid/sodium citrate damping fluid refer to first by 21.01 grams of citric acid (C
6h
8o
7.H
2o) dissolve in 1L pure water and obtain 0.1mol/L citric acid solution; Then by 29.41 grams of Trisodium Citrate (Na
3c
6h
5o
7.2H
2o) dissolve in 1L pure water and obtain 0.1mol/L sodium citrate solution; Finally 12.7mL citric acid solution and 7.3mL sodium citrate solution are mixed and get final product.
(8) enzymolysis Mierocrystalline cellulose is pulverized successively after 3000r/min centrifugal 6min dehydration, 40 DEG C of dry 12h, and obtaining granularity is 150 object finished product Microcrystalline Celluloses.
embodiment 5a preparation method for apple residue Microcrystalline Cellulose, comprises the following steps:
By apple residue raw material by the liquid ratio massfraction of 17.5mL/g be 2.2% hydrochloric acid soln swelling, obtain solute A; Solute A is constant temperature process 66min at 78.5 DEG C of temperature, then after the centrifugal 4min of 5000r/min, obtains supernatant A and throw out A respectively.
Wherein: the apple wet slag of water content less than 10% is after the distilled water submergence 3min of 35 DEG C in temperature, and with the centrifugal 8min dehydration of the speed of 5000r/min, the pomace of the impurity such as soluble sugar and tannin gained in removing pomace.
Supernatant A vacuum tightness be 0.65MPa, vaporization temperature is 35 DEG C of insulations, solvent recuperation volume ratio be the condition of 0.83 under concentrating under reduced pressure, obtain concentrated solution A, the dehydrated alcohol of its 4.5 times of volumes is added in this concentrated solution A, carry out solid-liquid separation with the centrifugal 3min of the rotating speed of 1600rpm after left at room temperature precipitation 12min, obtain solids A; Solids A carries out spraying dry to constant weight under the condition of feeding temperature 215 DEG C, drop temperature 154.5 DEG C, obtains crude pectin.
(3) throw out A is washed to pH value neutrality, then distilled water is added with the solid-liquid ratio of 1g:11mL, what add 15mL glacial acetic acid and 16g Textone by every 1L mixed system again to be pre-mixed after liquid at 78 DEG C of constant temperature process 1.5h, removes xylogen, obtains filter residue after draining solution.
(4) filter residue drains away the water after being washed to pH value neutrality, and the liquid ratio of pressing 12.5mL/g with the sodium hydroxide solution of massfraction 8.5% is swelling, obtains solute B; Solute B is isothermal holding 91min at 91 DEG C of temperature, then after the centrifugal 5min of 4000r/min, obtains supernatant liquor B and sediment B respectively.
Supernatant liquor B vacuum tightness be 0.65MPa, vaporization temperature is 35 DEG C of insulations, solvent recuperation volume ratio be the condition of 0.83 under concentrating under reduced pressure, obtain concentrated solution B, the dehydrated alcohol of its 4.5 times of volumes is added in this concentrated solution B, carry out solid-liquid separation with the centrifugal 3min of the rotating speed of 1600rpm after left at room temperature precipitation 12min, obtain solids B; Solids B pulverizes after being dried to constant weight at 62 DEG C, and obtaining granularity is 200 object hemicelluloses.
(6) sediment B is the H of 5% with the stirring velocity of 55r/min, by the liquid ratio volumetric concentration of 5mL/g
2o
2in the decolouring of 85 DEG C of heating in water bath, be the H of 5% by volumetric concentration after 5min
2o
2swelling by the liquid ratio of 5mL/g, obtain solute C; Solute C is centrifugal process 182min at 80.5 DEG C of temperature after, at 50 DEG C of dry 8h, obtains water-insoluble apple residue Mierocrystalline cellulose.
(7) the solid-liquid ratio adding distil water pressing 1g:55mL in water-insoluble apple residue Mierocrystalline cellulose is swelling, obtains solute D; The glacial acetic acid solution that pH value is 2.6 is dropwise added in solute D, make its pH value to 4.8, then according to the water-insoluble apple residue Mierocrystalline cellulose quality weighed, 30U cellulose complex enzyme is added by every gram of dried fibres element, this cellulose complex enzyme pH is the citric acid/sodium citrate buffer solution of 5.0, then mixes with water-insoluble apple residue Mierocrystalline cellulose, then at 55 DEG C of insulation enzymolysis 5h, and enzymolysis process stirs once every 20min, obtains enzymolysis Mierocrystalline cellulose.
Wherein: pH be 5.0 citric acid/sodium citrate damping fluid refer to first by 21.01 grams of citric acid (C
6h
8o
7.H
2o) dissolve in 1L pure water and obtain 0.1mol/L citric acid solution; Then by 29.41 grams of Trisodium Citrate (Na
3c
6h
5o
7.2H
2o) dissolve in 1L pure water and obtain 0.1mol/L sodium citrate solution; Finally 7.2mL citric acid solution and 12.8mL sodium citrate solution are mixed and get final product.
(8) enzymolysis Mierocrystalline cellulose is pulverized successively after 5000r/min centrifugal 4min dehydration, 60 DEG C of dry 8h, and obtaining granularity is 250 object finished product Microcrystalline Celluloses.
embodiment 6a preparation method for apple residue Microcrystalline Cellulose, comprises the following steps:
By apple residue raw material by the liquid ratio massfraction of 18mL/g be 2.5% hydrochloric acid soln swelling, obtain solute A; Solute A is constant temperature process 63.5minmin at 79 DEG C of temperature, then after the centrifugal 5min of 4000r/min, obtains supernatant A and throw out A respectively.
Wherein: the apple wet slag of water content less than 10% is after the distilled water submergence 5min of 30 DEG C in temperature, and with the centrifugal 10min dehydration of the speed of 4000r/min, the pomace of the impurity such as soluble sugar and tannin gained in removing pomace.
Supernatant A vacuum tightness be 0.7MPa, vaporization temperature is 35 DEG C of insulations, solvent recuperation volume ratio be the condition of 0.85 under concentrating under reduced pressure, obtain concentrated solution A, the dehydrated alcohol of its 6 times of volumes is added in this concentrated solution A, carry out solid-liquid separation with the centrifugal 3min of the rotating speed of 1600rpm after left at room temperature precipitation 12min, obtain solids A; Solids A carries out spraying dry to constant weight under the condition of feeding temperature 220 DEG C, drop temperature 155.5 DEG C, obtains crude pectin.
(3) throw out A is washed to pH value neutrality, then distilled water is added with the solid-liquid ratio of 1g:12mL, what add 15mL glacial acetic acid and 16g Textone by every 1L mixed system again to be pre-mixed after liquid at 80 DEG C of constant temperature process 1h, removes xylogen, obtains filter residue after draining solution.
(4) filter residue drains away the water after being washed to pH value neutrality, and the liquid ratio of pressing 113mL/g with the sodium hydroxide solution of massfraction 9% is swelling, obtains solute B; Solute B is isothermal holding 88min at 92 DEG C of temperature, then after the centrifugal 4min of 5000r/min, obtains supernatant liquor B and sediment B respectively.
Supernatant liquor B vacuum tightness be 0.7MPa, vaporization temperature is 35 DEG C of insulations, solvent recuperation volume ratio be the condition of 0.85 under concentrating under reduced pressure, obtain concentrated solution B, the dehydrated alcohol of its 6 times of volumes is added in this concentrated solution B, carry out solid-liquid separation with the centrifugal 3min of the rotating speed of 1600rpm after left at room temperature precipitation 12min, obtain solids B; Solids B pulverizes after being dried to constant weight at 65 DEG C, and obtaining granularity is 200 object hemicelluloses.
(6) sediment B is the H of 5% with the stirring velocity of 55r/min, by the liquid ratio volumetric concentration of 5mL/g
2o
2in the decolouring of 85 DEG C of heating in water bath, be the H of 5% by volumetric concentration after 5min
2o
2swelling by the liquid ratio of 5mL/g, obtain solute C; Solute C is centrifugal process 185min at 81 DEG C of temperature after, at 50 DEG C of dry 8h, obtains water-insoluble apple residue Mierocrystalline cellulose.
(7) the solid-liquid ratio adding distil water pressing 1g:60mL in water-insoluble apple residue Mierocrystalline cellulose is swelling, obtains solute D; The glacial acetic acid solution that pH value is 2.8 is dropwise added in solute D, make its pH value to 5.0, then according to the water-insoluble apple residue Mierocrystalline cellulose quality weighed, 25U cellulose complex enzyme is added by every gram of dried fibres element, this cellulose complex enzyme pH is the citric acid/sodium citrate buffer solution of 4.5, then mixes with water-insoluble apple residue Mierocrystalline cellulose, then at 50 DEG C of insulation enzymolysis 6h, and enzymolysis process stirs once every 18min, obtains enzymolysis Mierocrystalline cellulose.
Wherein: pH be 4.5 citric acid/sodium citrate damping fluid refer to first by 21.01 grams of citric acid (C
6h
8o
7.H
2o) dissolve in 1L pure water and obtain 0.1mol/L citric acid solution; Then by 29.41 grams of Trisodium Citrate (Na
3c
6h
5o
7.2H
2o) dissolve in 1L pure water and obtain 0.1mol/L sodium citrate solution; Finally 9.9mL citric acid solution and 10.1mL sodium citrate solution are mixed and get final product.
(8) enzymolysis Mierocrystalline cellulose is pulverized successively after 4000r/min centrifugal 5min dehydration, 50 DEG C of dry 10h, and obtaining granularity is 200 object finished product Microcrystalline Celluloses.
Above-mentioned
embodiment 1 ~ 6in, cellulose complex enzyme, purchased from Beijing Science and Technology Ltd. of Tianrui, is U.S. SIGMA cellulase packing product.
Claims (5)
1. a preparation method for apple residue Microcrystalline Cellulose, comprises the following steps:
By apple residue raw material by the liquid ratio massfraction of 16 ~ 18mL/g be 1.5% ~ 2.5% hydrochloric acid soln swelling, obtain solute A; Described solute A is centrifugal after constant temperature process 63.5min ~ 66.5min at 77 ~ 79 DEG C of temperature, obtains supernatant A and throw out A respectively;
(2) described supernatant A is separated obtains crude pectin through concentrating under reduced pressure, dehydrated alcohol precipitation, spraying dry successively;
(3) described throw out A is washed to pH value neutrality, then distilled water is added with the solid-liquid ratio of 1g:8 ~ 12mL, what add 15mL glacial acetic acid and 16g Textone by every 1L mixed system again to be pre-mixed after liquid at 70 ~ 80 DEG C of constant temperature process 1 ~ 2h, obtains filter residue after draining solution;
(4) described filter residue drains away the water after being washed to pH value neutrality, swelling by the liquid ratio of 11 ~ 13mL/g with the sodium hydroxide solution of massfraction 7% ~ 9%, obtains solute B; Described solute B is centrifugal after isothermal holding 88min ~ 92min at 88 DEG C ~ 92 DEG C temperature, obtains supernatant liquor B and sediment B respectively;
Described supernatant liquor B successively through concentrating under reduced pressure, dehydrated alcohol precipitation, 55 ~ 65 DEG C be dried to constant weight after pulverize, obtaining granularity is 150 ~ 200 object hemicelluloses;
(6) described sediment B is the H of 4 ~ 5% with the stirring velocity of 45 ~ 55r/min, by the liquid ratio volumetric concentration of 3 ~ 5mL/g
2o
2in the decolouring of 75 ~ 85 DEG C of heating in water bath, be the H of 4 ~ 5% by volumetric concentration after 5min
2o
2swelling by the liquid ratio of 3mL/g ~ 5mL/g, obtain solute C; Described solute C is centrifugal process 175min ~ 185min at 79 DEG C ~ 81 DEG C temperature after, at 35 ~ 50 DEG C of drying 8 ~ 12h, obtains water-insoluble apple residue Mierocrystalline cellulose;
(7) the solid-liquid ratio adding distil water pressing 1g:40 ~ 60mL in described water-insoluble apple residue Mierocrystalline cellulose is swelling, obtains solute D; The glacial acetic acid solution that pH value is 2.0 ~ 2.8 is dropwise added in described solute D, make its pH value to 4.1 ~ 5.0, then according to the water-insoluble apple residue Mierocrystalline cellulose quality weighed, 18 ~ 35U cellulose complex enzyme is added by every gram of dried fibres element, this cellulose complex enzyme pH is the citric acid/sodium citrate buffer solution of 4.0 ~ 5.0, then mix with described water-insoluble apple residue Mierocrystalline cellulose, again at 45 ~ 55 DEG C of insulation enzymolysis 5 ~ 7h, and enzymolysis process stirs once every 15 ~ 20min, obtains enzymolysis Mierocrystalline cellulose;
(8) described enzymolysis Mierocrystalline cellulose is pulverized successively after centrifuge dehydration, 40 ~ 60 DEG C of drying 8 ~ 12h, and obtaining granularity is 150 ~ 250 object finished product Microcrystalline Celluloses.
2. the preparation method of a kind of apple residue Microcrystalline Cellulose as claimed in claim 1, is characterized in that: described step (1) in apple residue raw material refer to the pomace of the broken rear mistake 40 mesh sieve gained of the biffins ground-slag of water content less than 8%; Or the apple wet slag of water content less than 10% is after temperature is the distilled water submergence 3 ~ 8min of 25 ~ 35 DEG C, and the pomace of the gained that dewaters with the centrifugal 8 ~ 12min of the speed of 3000 ~ 5000r/min.
3. the preparation method of a kind of apple residue Microcrystalline Cellulose as claimed in claim 1, it is characterized in that: described step (2) or described step (5) in the condition of concentrating under reduced pressure refer to that vacuum tightness is 0.5 ~ 0.7MPa, vaporization temperature is 35 DEG C of insulations, and solvent recuperation volume ratio is 0.80 ~ 0.85.
4. the preparation method of a kind of apple residue Microcrystalline Cellulose as claimed in claim 1, is characterized in that: described step (2) in spray-dired condition be feeding temperature 198 DEG C ~ 221 DEG C, drop temperature 153 DEG C ~ 156 DEG C.
5. the preparation method of a kind of apple residue Microcrystalline Cellulose as claimed in claim 1, is characterized in that: described step (7) in pH be 4.0 ~ 5.0 citric acid/sodium citrate damping fluid refer to and obtain 0.1mol/L citric acid solution first being dissolved in 1L pure water by 21.01 grams of citric acids; Then 29.41 grams of Trisodium Citrates are dissolved in 1L pure water and obtain 0.1mol/L sodium citrate solution; Finally described 7.2mL ~ 12.7mL citric acid solution and described 7.3mL ~ 12.8mL sodium citrate solution are mixed and get final product.
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| CN106916231B (en) * | 2017-05-08 | 2019-07-16 | 兰州理工大学 | A kind of method that Chinese medicine slag prepares microcrystalline cellulose |
| CN109336986B (en) * | 2018-10-31 | 2021-02-19 | 梧州学院 | Method for preparing nanocrystalline cellulose by utilizing cassava residues |
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| CN114249841B (en) * | 2021-11-25 | 2023-04-21 | 集美大学 | Preparation method and application of microcrystalline cellulose of honey pomelo young fruits |
| CN115874481A (en) * | 2022-11-24 | 2023-03-31 | 新疆金色果园农林科技有限公司 | Microcrystalline cellulose extracted from grape skin residues and preparation method thereof |
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| EP0531486A1 (en) * | 1991-02-21 | 1993-03-17 | Genencor International, Inc. | Crystalline cellulose production |
| CN101153293A (en) * | 2007-08-28 | 2008-04-02 | 陕西省微生物研究所 | Method for producing malic acid and mlcrocrystalline cellulose with apple pomace as raw material |
| CN103102419A (en) * | 2013-01-25 | 2013-05-15 | 浙江理工大学 | Method for preparing nano microcrystalline cellulose by hydrolyzing phyllostachys edulis fiber with cellulase |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| EP0531486A1 (en) * | 1991-02-21 | 1993-03-17 | Genencor International, Inc. | Crystalline cellulose production |
| CN101153293A (en) * | 2007-08-28 | 2008-04-02 | 陕西省微生物研究所 | Method for producing malic acid and mlcrocrystalline cellulose with apple pomace as raw material |
| CN103102419A (en) * | 2013-01-25 | 2013-05-15 | 浙江理工大学 | Method for preparing nano microcrystalline cellulose by hydrolyzing phyllostachys edulis fiber with cellulase |
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