CN106916231B - A kind of method that Chinese medicine slag prepares microcrystalline cellulose - Google Patents
A kind of method that Chinese medicine slag prepares microcrystalline cellulose Download PDFInfo
- Publication number
- CN106916231B CN106916231B CN201710316191.6A CN201710316191A CN106916231B CN 106916231 B CN106916231 B CN 106916231B CN 201710316191 A CN201710316191 A CN 201710316191A CN 106916231 B CN106916231 B CN 106916231B
- Authority
- CN
- China
- Prior art keywords
- chinese medicine
- medicine slag
- microcrystalline cellulose
- filter residue
- added
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B15/00—Preparation of other cellulose derivatives or modified cellulose, e.g. complexes
- C08B15/02—Oxycellulose; Hydrocellulose; Cellulosehydrate, e.g. microcrystalline cellulose
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Biochemistry (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Cosmetics (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The invention discloses a kind of methods that Chinese medicine slag prepares microcrystalline cellulose, comprising the following steps: a, mixes Chinese medicine slag and distilled water, slightly boiled, centrifugation obtains filter residue；B, alkali process: sodium hydroxide solution, water bath processing is added in filter residue, centrifugation, washing are precipitated to neutrality, collect filter residue；C, acid processing: adding distilled water for gained filter residue, adjusts pH to 1-2, and water bath processing is centrifuged to obtain filter residue, washing to neutrality, drying；D, Chinese medicine slag crude fibre extracts: bleaching liquid is added in gained filter residue, water bath processing filters, and washing obtains Chinese medicine slag crude fibre to neutral, drying to constant weight；E, it prepares microcrystalline cellulose: hydrochloric acid solution is added in obtained Chinese medicine slag crude fibre and carries out sour water solution, filter, wash to neutral, drying to constant weight, microcrystalline cellulose is made.Preparation method of the invention is conducive to improve the processing utilization rate of discarded Chinese medicine slag resource, provides a kind of safe, cheap, convenient raw material resources for the production of microcrystalline cellulose.
Description
Technical field
The present invention relates to a kind of method for preparing microcrystalline cellulose, more particularly to a kind of Chinese medicine slag prepare pharmaceutic adjuvant and
The method of food additives microcrystalline cellulose.
Background technique
Chinese medicine is under instruction of Chinese Medicine theory for preventing, diagnosing, treating disease or adjusting the drug of function of human body.In
Medicinal material is mostly botanical medicine, also there is Some Animals medicine, mineral drug and chemistry, biological species medicine.The fast development of Chinese herbal medicine industry is to people
Bring economic interests, but the processing of Chinese medicine slag and to recycle be a great problem.The Chinese medicine slag yield that China generates every year
It is very big, up to as many as a few kiloton.Currently, people are not very environmentally friendly to the processing of Chinese medicine slag, early stage is mostly to burn, fill
The mode of hostile environment and human health is handled.Crude fibre component rich in, mislays in plant source Chinese medicine slag
Natural reproducible resource.Therefore, concern of the recycling of Chinese medicine slag by more and more professional persons, if can will be huge in
Dregs of a decoction resource carries out trans-utilization and deep development, had not only avoided the waste of resource but also had protected the health of environment and human body.
Microcrystalline cellulose (Microcrystalline cellulose, abbreviation MCC) is natural plant cellulose, through diluted acid
Made from hydrolysis and a variety of post-processings, the product with levelling off degree of polymerization (LOOP), with line made of β-Isosorbide-5-Nitrae glucosides key connection
Type molecule.Microcrystalline cellulose is free flowable imperceptible corynebacterium or powdery porous shape particle, color be white or
Near-white, odorless, tasteless, granular size is generally in 20-80nm, and levelling off degree of polymerization (LODP) is in 15-375.Microcrystalline cellulose
The degree of polymerization has differences with its crystallinity because its raw material type is different, the degree of polymerization for the microcrystalline cellulose that different material is produced
Difference is larger, high between 200-250, mainly natural purified cotton production, between low 15-30.Microcrystalline cellulose is molten
Solution property poor, not soluble in water, diluted acid, organic solvent and grease, are partly dissolved in dilute alkaline soln, moisten and rise, in carboxy methylation, second
Reactivity worth with higher in acylated, esterification process.Due to the particularity such as low degree and biggish specific surface area
Matter, microcrystalline cellulose are widely used in medicine, food, cosmetics and light industry industry.
In the prior art, someone prepares crystallite fibre using soybean skin, peanut shell, reed, wheat straw waste, corn stover etc.
Dimension element, but yet there are no the report in relation to preparing microcrystalline cellulose using Chinese medicine slag resource, crystallite fibre is prepared according to Chinese medicine slag
Dimension element is succeeded in developing, and opens a new way for utilizing for the deep development of Chinese medicine slag resource.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of method that Chinese medicine slag prepares microcrystalline cellulose, make full use of
Dregs of a decoction resource avoids the wastings of resources such as burning, landfill and environmental pollution, improves effective benefit of Chinese medicine processing enterprise waste residue
With, and a kind of low in cost, convenient raw material resources in source are provided for new material microcrystalline cellulose.
In order to solve the above technical problems, the present invention provides a kind of methods that Chinese medicine slag prepares microcrystalline cellulose, including with
Lower step:
A, Chinese medicine slag and deionized water are mixed with solid-to-liquid ratio 1:15-1:30 (g/mL), slightly boiled 100-120min, centrifugation,
Filter residue, slightly boiled in the present invention refer to temperature close to boiling point, be 92-95 DEG C, liquid is just in fluidized state, occurs first
When bubble starts；
B, 0.02-0.08 (g/ml) hydrogen alkali process: is added with solid-to-liquid ratio 1:10-1:15 (g/ml) in filter residue obtained by step a
Sodium hydroxide solution, 50-80 DEG C of water bath processing 60-120min are centrifuged and wash and be precipitated to neutrality, collect filter residue；
C, acid processing: by filter residue obtained by step b with solid-to-liquid ratio 1:2-1:10 (g/ml) plus distilled water, it is with mass concentration
Hydrochloric acid, nitric acid, sulfuric acid or the phosphoric acid tune pH value of 1%-5% to 1-2,50-80 DEG C of constant temperature water bath handles 60-90min, is centrifuged to obtain filter
Slag, washing to neutrality, dewatered drying；
D, Chinese medicine slag crude fibre extracts: filter residue obtained by step c being added with solid-to-liquid ratio 1:20-1:50 (g/ml) and is bleached
Liquid, 50-80 DEG C of water bath processing 60-90min are filtered, and washing obtains Chinese medicine slag crude fibre to neutral, dewatered drying to constant weight；
E, microcrystalline cellulose processed: Chinese medicine slag crude fibre obtained by step d is added with solid-to-liquid ratio 1:10-1:20 (g/ml)
Entering mass concentration is 1%-6% hydrochloric acid solution, and 50-90 DEG C of water bath processing 65-115min is filtered, washed to neutral, dewatered drying
To constant weight, microcrystalline cellulose is made.
The method that above-mentioned Chinese medicine slag prepares microcrystalline cellulose, wherein in the step d, the bleaching liquid is mass concentration
The H that NaOH solution and mass fraction for 2%-5% are 3%-5%2O2The mixed bleach liquid of isometric mixing composition, preferably
The H that 3% NaOH solution and mass fraction is 4%2O2The mixed bleach liquid of isometric mixing composition.
The method that above-mentioned Chinese medicine slag prepares microcrystalline cellulose, wherein in the step d, the bleaching liquid is mass concentration
The liquor natrii hypochloritis that sodium sulfite solution and available chlorine content for 1%-4% are 3%-5% mixes the mixed of composition in equal volume
The bodies such as the liquor natrii hypochloritis that the sodium sulfite solution and available chlorine content that conjunction bleaching liquid, preferably mass concentration are 3% are 5%
The mixed bleach liquid of product mixing composition.
The method that above-mentioned Chinese medicine slag prepares microcrystalline cellulose, wherein in the step e, by Chinese medicine slag obtained by step d
Crude fibre with solid-to-liquid ratio 1:12-1:16 (g/ml) be added mass concentration be 3%-5% hydrochloric acid solution, 60-80 DEG C of water bath processing
65-85min filters, washs to neutral, dewatered drying to constant weight, microcrystalline cellulose is made.
The method that above-mentioned Chinese medicine slag prepares microcrystalline cellulose, wherein in the step e, by Chinese medicine slag obtained by step d
Mass concentration is added with solid-to-liquid ratio 1:14g/ml as 3% hydrochloric acid solution in crude fibre, and 70 DEG C of water bath processing 65min are filtered, washing
To neutral, dewatered drying to constant weight, microcrystalline cellulose is made.
The method that above-mentioned Chinese medicine slag prepares microcrystalline cellulose, wherein use mass concentration for 1-5%'s in the step c
Nitric acid.
The method that above-mentioned Chinese medicine slag prepares microcrystalline cellulose, wherein the Chinese medicine slag type is unlimited, excellent in the step a
Selection of land, the cellulose mass fraction in Chinese medicine slag is 15% or more.
The method that above-mentioned Chinese medicine slag prepares microcrystalline cellulose, wherein in the step a, the Chinese medicine slag is Radix Ophiopogonis, the five tastes
The Chinese medicine slag generated after the processing of the Chinese materia medica preparations such as son, Rehmannia glutinosa, wine-prepared fructus corni, cortex moutan, Chinese yam, Poria cocos, rhizoma alismatis.
The method that above-mentioned Chinese medicine slag prepares microcrystalline cellulose, wherein in the step a, the Chinese medicine slag is cortex cinnamomi, monkshood
The Chinese medicine slag generated after the processing of the Chinese materia medica preparations such as (system), Rehmannia glutinosa, Fructus Corni (system).
The method that Chinese medicine slag of the invention prepares microcrystalline cellulose has the following beneficial effects:
1, the present invention uses Chinese medicine slag to prepare microcrystalline cellulose for raw material, takes full advantage of Chinese medicine slag resource, avoids and burn
The wastings of resources and the environmental pollutions such as burning, landfill improve the effective use of Chinese medicine processing enterprise waste residue, and are new material
Microcrystalline cellulose provides a kind of safe, cheap, convenient raw material resources；
2, the obtained microcrystalline cellulose purity of the present invention is up to 98% or more, and for the degree of polymerization between 220-270, particle size is suitable
In, it measures indices and meets " Chinese Pharmacopoeia " microcrystalline cellulose quality standard, can be used for field of medicaments, and the present invention
Obtained microcrystalline cellulose also complies with GB1886.103-2015 national standard, is readily applicable to food additives industry；
3, microcrystalline cellulose is prepared using treatment process sour after first alkali in preparation method of the invention, be obviously improved micro-
The purity and whiteness of crystalline cellulose, and saved great lot of water resources；
4, mixed bleach agent is used in preparation method of the invention, compared with using single bleaching agent, can significantly be mentioned
Yield, purity and the whiteness of microcrystalline cellulose obtained are risen, and shortens bleaching time.
5, the preparation method of microcrystalline cellulose of the invention is simple, easily operated, environmentally protective.
Specific embodiment
Below with reference to embodiment the present invention is described in detail.
Chinese medicine slag in following embodiment and comparative examples is provided by Lanzhou Tai Bao pharmaceutcal corporation, Ltd, Chinese medicine slag be Radix Ophiopogonis,
The Chinese medicine slag formed after the processing of the Chinese medicines such as Schisandra chinensis, Rehmannia glutinosa, wine-prepared fructus corni, cortex moutan, Chinese yam, Poria cocos, rhizoma alismatis, cellulose material
Measuring score is 30% or more.
Embodiment 1
A, it weighs 10g Chinese medicine slag to boil in bottle in disappearing, be mixed Chinese medicine slag and deionized water with solid-to-liquid ratio 1:20g/mL, i.e. 1g
20ml deionized water is added in Chinese medicine slag, and slightly boiled 120min, 3500r/min are centrifuged 10min, obtain filter residue；
B, alkali process: being added 0.04g/ml sodium hydroxide solution for filter residue obtained by step a with solid-to-liquid ratio 1:10g/ml, and 60 DEG C
Water bath processing 100min is centrifuged to obtain filter residue, and washing is precipitated to neutrality, collects filter residue；
C, acid processing: filter residue obtained by step b is added into distilled water with solid-to-liquid ratio 1:10g/ml, the salt for being 3% with mass concentration
Acid adjusts pH value to 1.5,80 DEG C of constant temperature water baths to handle 60min, is centrifuged to obtain filter residue, washing to neutrality, dewatered drying；
D, Chinese medicine slag crude fibre extracts: bleaching liquid, bleaching liquid is added with solid-to-liquid ratio 1:40g/ml in filter residue obtained by step c
For mass concentration be 3% sodium sulfite solution and available chlorine content be 5% liquor natrii hypochloritis in equal volume mix composition
Mixed bleach liquid, 80 DEG C of water bath processing 60min are filtered, and washing obtains Chinese medicine slag crude fibre to neutral, dewatered drying to constant weight
Element；
E, quality microcrystalline cellulose processed: is added with solid-to-liquid ratio 1:14g/ml in Chinese medicine slag crude fibre obtained by step d
Concentration is 4% hydrochloric acid solution, and 70 DEG C of water bath processing 65min filter, wash to neutral, dewatered drying to constant weight, it is fine that crystallite is made
Dimension element.
The yield of microcrystalline cellulose made from the present embodiment is 35.43%, purity 98.77%, and whiteness 92.51 is gathered
Right is 256.43.
Embodiment 2
A, it weighs 10g Chinese medicine slag to boil in bottle in disappearing, be mixed Chinese medicine slag and deionized water with solid-to-liquid ratio 1:15g/mL, i.e. 1g
15ml deionized water is added in Chinese medicine slag, and slightly boiled 120min, 3500r/min are centrifuged 5min, obtain filter residue；
B, alkali process: being added 0.08g/ml sodium hydroxide solution for filter residue obtained by step a with solid-to-liquid ratio 1:15g/ml, and 80 DEG C
Water bath processing 60min is centrifuged to obtain filter residue, and washing is precipitated to neutrality, collects filter residue；
C, acid processing: filter residue obtained by step b is added into distilled water with solid-to-liquid ratio 1:2g/ml, the sulfuric acid for being 5% with mass concentration
It adjusts pH value to 1,60 DEG C of constant temperature water bath to handle 80min, is centrifuged to obtain filter residue, washing to neutrality, dewatered drying；
D, Chinese medicine slag crude fibre extracts: bleaching liquid, bleaching liquid is added with solid-to-liquid ratio 1:20g/ml in filter residue obtained by step c
The liquor natrii hypochloritis that sodium sulfite solution and available chlorine content for 3% are 5% mixes the mixed bleach liquid of composition in equal volume,
60 DEG C of water bath processing 80min are filtered, and washing obtains Chinese medicine slag crude fibre to neutral, dewatered drying to constant weight；
E, quality microcrystalline cellulose processed: is added with solid-to-liquid ratio 1:10g/ml in Chinese medicine slag crude fibre obtained by step d
Concentration is 4% hydrochloric acid solution, and 70 DEG C of water bath processing 75min filter, wash to neutral, dewatered drying to constant weight, it is fine that crystallite is made
Dimension element.
The yield of microcrystalline cellulose made from the present embodiment is 36.33%, purity 98.94%, whiteness 91.23, polymerization
Degree is 269.47.
Embodiment 3
A, it weighs 10g Chinese medicine slag to boil in bottle in disappearing, be mixed Chinese medicine slag and deionized water with solid-to-liquid ratio 1:30g/mL, i.e. 1g
30ml deionized water is added in Chinese medicine slag, and slightly boiled 100min, 3000r/min are centrifuged 20min, obtain filter residue；
B, alkali process: being added 0.02g/ml sodium hydroxide solution for filter residue obtained by step a with solid-to-liquid ratio 1:12g/ml, and 50 DEG C
Water bath processing 120min is centrifuged to obtain filter residue, and washing is precipitated to neutrality, collects filter residue；
C, acid processing: filter residue obtained by step b is added into distilled water with solid-to-liquid ratio 1:5g/ml, the phosphoric acid for being 5% with mass concentration
It adjusts pH value to 2,50 DEG C of constant temperature water baths to handle 90min, is centrifuged to obtain filter residue, washing to neutrality, dewatered drying；
D, Chinese medicine slag crude fibre extracts: bleaching liquid, bleaching liquid is added with solid-to-liquid ratio 1:50g/ml in filter residue obtained by step c
For mass concentration be 1% sodium sulfite solution and available chlorine content be 3% liquor natrii hypochloritis in equal volume mix composition
Mixed bleach liquid, 50 DEG C of water bath processing 90min are filtered, and washing obtains Chinese medicine slag crude fibre to neutral, dewatered drying to constant weight
Element；
E, quality microcrystalline cellulose processed: is added with solid-to-liquid ratio 1:14g/ml in Chinese medicine slag crude fibre obtained by step d
Concentration is 3% hydrochloric acid solution, and 60 DEG C of water bath processing 75min filter, wash to neutral, dewatered drying to constant weight, it is fine that crystallite is made
Dimension element.
The yield of microcrystalline cellulose made from the present embodiment is 39.55%, purity 98.55%, whiteness 90.63, the degree of polymerization
It is 249.28.
Embodiment 4
A, it weighs 10g Chinese medicine slag to boil in bottle in disappearing, be mixed Chinese medicine slag and deionized water with solid-to-liquid ratio 1:20g/mL, i.e. 1g
20ml deionized water is added in Chinese medicine slag, and slightly boiled 120min, 3500r/min are centrifuged 10min, obtain filter residue；
B, alkali process: being added 0.04g/ml sodium hydroxide solution for filter residue obtained by step a with solid-to-liquid ratio 1:12g/ml, and 60 DEG C
Water bath processing 100min is centrifuged to obtain filter residue, and washing is precipitated to neutrality, collects filter residue；
C, acid processing: filter residue obtained by step b is added into distilled water with solid-to-liquid ratio 1:8g/ml, the nitric acid for being 3% with mass concentration
It adjusts pH value to 1.5,80 DEG C of constant temperature water baths to handle 60min, is centrifuged to obtain filter residue, washing to neutrality, dewatered drying；
D, Chinese medicine slag crude fibre extracts: bleaching liquid, bleaching liquid is added with solid-to-liquid ratio 1:25g/ml in filter residue obtained by step c
The liquor natrii hypochloritis that for mass concentration be 3% sodium sulfite solution and available chlorine content is 5% mixes the mixed of composition in equal volume
Bleaching liquid is closed, 80 DEG C of water bath processing 60min are filtered, and washing obtains Chinese medicine slag crude fibre to neutral, dewatered drying to constant weight；
E, quality microcrystalline cellulose processed: is added with solid-to-liquid ratio 1:14g/ml in Chinese medicine slag crude fibre obtained by step d
Concentration is 4% hydrochloric acid solution, and 70 DEG C of water bath processing 65min filter, wash to neutral, dewatered drying to constant weight, it is fine that crystallite is made
Dimension element.
The yield of microcrystalline cellulose made from the present embodiment is 41.63%, purity 98.93%, whiteness 93.34, the degree of polymerization
It is 253.15.
Embodiment 5
A, it weighs 10g Chinese medicine slag to boil in bottle in disappearing, be mixed Chinese medicine slag and deionized water with solid-to-liquid ratio 1:20g/mL, i.e. 1g
20ml deionized water is added in Chinese medicine slag, and slightly boiled 120min, 3500r/min are centrifuged 10min, obtain filter residue；
B, alkali process: being added 0.04g/ml sodium hydroxide solution for filter residue obtained by step a with solid-to-liquid ratio 1:12g/ml, and 60 DEG C
Water bath processing 100min is centrifuged to obtain filter residue, and washing is precipitated to neutrality, collects filter residue；
C, acid processing: filter residue obtained by step b is added into distilled water with solid-to-liquid ratio 1:8g/ml, the nitric acid for being 3% with mass concentration
It adjusts pH value to 1.5,80 DEG C of constant temperature water baths to handle 60min, is centrifuged to obtain filter residue, washing to neutrality, dewatered drying；
D, Chinese medicine slag crude fibre extracts: bleaching liquid, bleaching liquid is added with solid-to-liquid ratio 1:25g/ml in filter residue obtained by step c
The liquor natrii hypochloritis that for mass concentration be 4% sodium sulfite solution and available chlorine content is 4% mixes the mixed of composition in equal volume
Bleaching liquid is closed, 80 DEG C of water bath processing 60min are filtered, and washing obtains Chinese medicine slag crude fibre to neutral, dewatered drying to constant weight；
E, quality microcrystalline cellulose processed: is added with solid-to-liquid ratio 1:12g/ml in Chinese medicine slag crude fibre obtained by step d
Concentration is 5% hydrochloric acid solution, and 70 DEG C of water bath processing 85min filter, wash to neutral, dewatered drying to constant weight, it is fine that crystallite is made
Dimension element.
The yield of microcrystalline cellulose made from the present embodiment is 40.05%, purity 98.53%, whiteness 91.67, the degree of polymerization
It is 263.14.
Embodiment 6
A, it weighs 10g Chinese medicine slag to boil in bottle in disappearing, be mixed Chinese medicine slag and deionized water with solid-to-liquid ratio 1:20g/mL, i.e. 1g
20ml deionized water is added in Chinese medicine slag, and slightly boiled 120min, 3500r/min are centrifuged 10min, obtain filter residue；
B, alkali process: being added 0.04g/ml sodium hydroxide solution for filter residue obtained by step a with solid-to-liquid ratio 1:12g/ml, and 60 DEG C
Water bath processing 100min is centrifuged to obtain filter residue, and washing is precipitated to neutrality, collects filter residue；
C, acid processing: filter residue obtained by step b is added into distilled water with solid-to-liquid ratio 1:8g/ml, the nitric acid for being 5% with mass concentration
It adjusts pH value to 1.5,80 DEG C of constant temperature water baths to handle 60min, is centrifuged to obtain filter residue, washing to neutrality, dewatered drying；
D, Chinese medicine slag crude fibre extracts: bleaching liquid, bleaching liquid is added with solid-to-liquid ratio 1:25g/ml in filter residue obtained by step c
For mass concentration be 3% NaOH solution and mass fraction be 4% H2O2The mixed bleach liquid of isometric mixing composition, 80 DEG C
Water bath processing 90min is filtered, and washing obtains Chinese medicine slag crude fibre to neutral, dewatered drying to constant weight；
E, quality microcrystalline cellulose processed: is added with solid-to-liquid ratio 1:14g/ml in Chinese medicine slag crude fibre obtained by step d
Concentration is 4% hydrochloric acid solution, and 70 DEG C of water bath processing 65min filter, wash to neutral, dewatered drying to constant weight, it is fine that crystallite is made
Dimension element.
The yield of microcrystalline cellulose made from the present embodiment is 36.4%, purity 98.48%, whiteness 93.53, and the degree of polymerization is
247.29。
Embodiment 7
A, it weighs 10g Chinese medicine slag to boil in bottle in disappearing, be mixed Chinese medicine slag and deionized water with solid-to-liquid ratio 1:20g/mL, i.e. 1g
20ml deionized water is added in Chinese medicine slag, and slightly boiled 120min, 3500r/min are centrifuged 10min, obtain filter residue；
B, alkali process: being added 0.04g/ml sodium hydroxide solution for filter residue obtained by step a with solid-to-liquid ratio 1:12g/ml, and 60 DEG C
Water bath processing 100min is centrifuged to obtain filter residue, and washing is precipitated to neutrality, collects filter residue；
C, acid processing: filter residue obtained by step b is added into distilled water with solid-to-liquid ratio 1:8g/ml, the nitric acid for being 1% with mass concentration
It adjusts pH value to 1.5,80 DEG C of constant temperature water baths to handle 60min, is centrifuged to obtain filter residue, washing to neutrality, dewatered drying；
D, Chinese medicine slag crude fibre extracts: bleaching liquid, bleaching liquid is added with solid-to-liquid ratio 1:25g/ml in filter residue obtained by step c
For mass concentration be 4% NaOH solution and mass fraction be 4% H2O2The mixed bleach liquid of isometric mixing composition, 80 DEG C
Water bath processing 90min is filtered, and washing obtains Chinese medicine slag crude fibre to neutral, dewatered drying to constant weight；
E, quality microcrystalline cellulose processed: is added with solid-to-liquid ratio 1:20g/ml in Chinese medicine slag crude fibre obtained by step d
Concentration is 4% hydrochloric acid solution, and 80 DEG C of water bath processing 65min filter, wash to neutral, dewatered drying to constant weight, it is fine that crystallite is made
Dimension element.
The yield of microcrystalline cellulose made from the present embodiment is 34.36%, purity 98.31%, whiteness 92.13, the degree of polymerization
It is 241.11.
Embodiment 8
A, it weighs 10g Chinese medicine slag to boil in bottle in disappearing, be mixed Chinese medicine slag and deionized water with solid-to-liquid ratio 1:20g/mL, i.e. 1g
20ml deionized water is added in Chinese medicine slag, and slightly boiled 120min, 3500r/min are centrifuged 10min, obtain filter residue；
B, alkali process: being added 0.04g/ml sodium hydroxide solution for filter residue obtained by step a with solid-to-liquid ratio 1:12g/ml, and 60 DEG C
Water bath processing 100min is centrifuged to obtain filter residue, and washing is precipitated to neutrality, collects filter residue；
C, acid processing: filter residue obtained by step b is added into distilled water with solid-to-liquid ratio 1:8g/ml, the nitric acid for being 5% with mass concentration
It adjusts pH value to 1.5,80 DEG C of constant temperature water baths to handle 60min, is centrifuged to obtain filter residue, washing to neutrality, dewatered drying；
D, Chinese medicine slag crude fibre extracts: bleaching liquid, bleaching liquid is added with solid-to-liquid ratio 1:25g/ml in filter residue obtained by step c
For mass concentration be 2% NaOH solution and mass fraction be 5% H2O2The mixed bleach liquid of isometric mixing composition, 80 DEG C
Water bath processing 90min is filtered, and washing obtains Chinese medicine slag crude fibre to neutral, dewatered drying to constant weight；
E, quality microcrystalline cellulose processed: is added with solid-to-liquid ratio 1:14g/ml in Chinese medicine slag crude fibre obtained by step d
Concentration is 6% hydrochloric acid solution, and 50 DEG C of water bath processing 115min filter, wash to neutral, dewatered drying to constant weight, crystallite is made
Cellulose.
The yield of microcrystalline cellulose made from the present embodiment is 32.32%, purity 97.39%, whiteness 92.33, the degree of polymerization
It is 227.22.
Embodiment 9
A, it weighs 10g Chinese medicine slag to boil in bottle in disappearing, be mixed Chinese medicine slag and deionized water with solid-to-liquid ratio 1:20g/mL, i.e. 1g
20ml deionized water is added in Chinese medicine slag, and slightly boiled 120min, 3500r/min are centrifuged 10min, obtain filter residue；
B, alkali process: being added 0.04g/ml sodium hydroxide solution for filter residue obtained by step a with solid-to-liquid ratio 1:12g/ml, and 60 DEG C
Water bath processing 100min is centrifuged to obtain filter residue, and washing is precipitated to neutrality, collects filter residue；
C, acid processing: filter residue obtained by step b is added into distilled water with solid-to-liquid ratio 1:8g/ml, the nitric acid for being 3% with mass concentration
It adjusts pH value to 1.5,80 DEG C of constant temperature water baths to handle 60min, is centrifuged to obtain filter residue, washing to neutrality, dewatered drying；
D, Chinese medicine slag crude fibre extracts: bleaching liquid, bleaching liquid is added with solid-to-liquid ratio 1:25g/ml in filter residue obtained by step c
For mass concentration be 5% NaOH solution and mass fraction be 3% H2O2The mixed bleach liquid of isometric mixing composition, 80 DEG C
Water bath processing 90min is filtered, and washing obtains Chinese medicine slag crude fibre to neutral, dewatered drying to constant weight；
E, quality microcrystalline cellulose processed: is added with solid-to-liquid ratio 1:16g/ml in Chinese medicine slag crude fibre obtained by step d
Concentration is 1% hydrochloric acid solution, and 100 DEG C of water bath processing 85min filter, wash to neutral, dewatered drying to constant weight, crystallite is made
Cellulose.
The yield of microcrystalline cellulose made from the present embodiment is 34.13%, purity 98.41%, whiteness 90.16, the degree of polymerization
It is 260.77.
Comparative example 1
Comparative example 1 is identical as the preparation method of the microcrystalline cellulose of embodiment 1, the difference is that step b and step c
Processing sequence is different, and comparative example 1 first carries out HCl treatment, carries out alkali process later, i.e. preparation step is a, c, b, d and e.It is made
Crude fibre and microcrystalline cellulose yield, purity and whiteness comparison such as table 1.
Table 1
Comparative example 2
Comparative example 2 is identical as the preparation method of the microcrystalline cellulose of embodiment 2, the difference is that step b and step c
Processing sequence is different, and comparative example 2 first carries out sulfuric acid treatment, carries out alkali process later, i.e. preparation step is a, c, b, d and e.It is made
Crude fibre and microcrystalline cellulose yield, purity and whiteness comparison such as table 2.
Table 2
Comparative example 3
Comparative example 3 is identical as the preparation method of the microcrystalline cellulose of embodiment 4, the difference is that step b and step c
Processing sequence is different, and comparative example 3 first carries out nitric acid treatment, carries out alkali process later, i.e. preparation step is a, c, b, d and e.It is made
Crude fibre and microcrystalline cellulose yield, purity and whiteness comparison such as table 3.
Table 3
By table 1, table 2 and table 3 it is found that first using alkali process in the microcrystalline cellulose preparation method of embodiment 1,2 and 4,
Later using acid processing, in the microcrystalline cellulose preparation method of comparative example 1,2 and 3 first using acid processing after use alkali process phase
The purity and whiteness of the crude fibre and microcrystalline cellulose that are obtained than, embodiment 1,2 and 4 be significantly better than corresponding comparative example 1,
The crude fibre and microcrystalline cellulose obtained in 2 and 3, in terms of yield, the crude fibre and crystallite that embodiment 2 and 4 obtains are fine
Tie up what plain yield was obtained also superior to the crude fibre and microcrystalline cellulose obtained in corresponding comparative example 2 and 3, embodiment 1
The yield of crude fibre and microcrystalline cellulose and the yield of crude fibre and microcrystalline cellulose that comparative example 1 obtains are essentially identical.
Comparative experiments shows for acid processing is using nitric acid or sulfuric acid, carries out the thick fibre that acid processing obtains after first carrying out alkali process
Dimension element, microcrystalline cellulose extract yield, be above in purity and whiteness carried out after first carrying out sour processing alkali process as a result,
For hydrochloric acid, soda acid sequencing influences less the yield of its crude fibre, microcrystalline cellulose, but first carries out alkali process
The system that the crude fibre of HCl treatment, the purity of microcrystalline cellulose and whiteness are apparently higher than alkali process after first HCl treatment is carried out afterwards
Preparation Method.
In the method for the invention, due to Chinese medicine slag powder diameter very little, if using alkali process after first acid, in alkali process
Afterwards, it because of the swollen reason of alkali soluble, when treatment fluid centrifugal treating, needs to be centrifuged repeatedly, waste time, also, cannot adequately make
Filter residue is in neutrality, and is washed remaining alkali and needed to consume a large amount of water resource, if not washing clean on the contrary, remaining alkali can also be right
Acid hydrolysis step in microcrystalline cellulose preparation process has a adverse impact.Using acid processing after first alkali in the present invention, it is added
Inorganic acid can neutralize residual alkali in solution, avoid and cleaned using a large amount of water, economized on resources.Applicant sends out in an experiment
Existing, the chemical reaction of cellulose is mainly the reaction of three activity hydroxies on its molecule, due to its multilayered structure, great amount of hydroxy group
It is closed in crystal region, chemical reagent is difficult to penetrate into.The advantageous lye of alkali process and lignin, hemicellulose etc. are carried out first
Component reacts, because alkali can eliminate the ester bond of lignin-carbohydrate complexes, selective dissolution and removing Chinese medicine
In hemicellulose and lignin, sufficiently expose the filament structure of cellulose, improve the degradability of cellulose.Another party
Face makes the cellulose of amorphous region that peeling reaction occur, and to cellulose crystallite due to the cellulolytic amorphous region of alkali energy
The swelling action in area, crystal region enclosed construction are opened, and change original closed Chinese medicine wood fibre structure.At alkali
After reason, although the hemicellulose in traditional Chinese medicinal material samples cannot be removed completely, hemicellulose is easier quilt for comparing cellulose
Mineral acid hydrolysis becomes monosaccharide, so first carry out alkali process is adjusted with acid PH again, the hemicellulose not eliminated can be removed dry
Only, without generating big destruction to cellulosic structure, the purity of crude fibre product is improved.In addition, in the system of microcrystalline cellulose
During standby, according to the processing method of alkali after first acid, acid can have larger impact to the color of fiber, this is because coloring matter
It is even closer in conjunction with fiber fine structure after oxidation, affect the color of Chinese medicine slag cellulose.Coarse-fibred color burn must
Subsequent bleaching effect is so influenced, and will affect alkali to the removal effect of hemicellulose and lignin, reduces microcrystalline cellulose
Purity, and the substance after this pigment oxidation is closer in conjunction with fiber fine structure, to microcrystalline cellulose below
The inhibition that acid generates the hydrolysis of cellulose in preparation process is also bigger.Therefore, in the present invention using first alkali
The process of acid processing prepares microcrystalline cellulose after reason, has been obviously improved the purity and whiteness of microcrystalline cellulose, and save
Great lot of water resources.
Comparative example 4
Comparative example 4 is identical as the preparation method of the microcrystalline cellulose of embodiment 4, the difference is that used in step d
Bleaching liquid is the liquor natrii hypochloritis that single bleaching agent available chlorine content is 5%, 80 DEG C of water bath processing 120min.
Comparative example 5
Comparative example 5 is identical as the preparation method of the microcrystalline cellulose of embodiment 4, the difference is that used in step d
Bleaching liquid is the sodium sulfite solution that single bleaching agent mass concentration is 3%, 80 DEG C of water bath processing 120min.
Crude fibre made from embodiment 4, comparative example 4 and comparative example 5 and microcrystalline cellulose comparison such as table 4.
Table 4
It is compared by table 4 it is found that the mixed bleach mixed in embodiment 4 using sodium sulfite and liquor natrii hypochloritis
Agent, the whiteness of crude fibre and microcrystalline cellulose obtained are significantly better than comparative example 4 and comparative example 5 using single bleaching agent,
And the yield and purity of the final microcrystalline cellulose obtained of embodiment 4 are also significantly better than comparative example 4 and comparative example 5.Embodiment 4
The time of middle mixed bleach agent processing is 60min, and the time of single bleaching agent processing is 120min in comparative example 4 and 5.This hair
Bright middle use can significantly improve microcrystalline cellulose obtained by the mixed bleach agent that sodium sulfite and sodium hypochlorite mixing form
Yield, purity and whiteness, and shorten bleaching time, hence it is evident that better than using single bleaching agent sodium hypochlorite or sulfurous acid
Sodium.
Comparative example 6
Comparative example 6 is identical as the preparation method of the microcrystalline cellulose of embodiment 6, the difference is that used in step d
Bleaching liquid is the H that single bleaching agent mass fraction is 4%2O2, 80 DEG C of water bath processing 120min.
Crude fibre made from embodiment 6 and comparative example 6 and microcrystalline cellulose comparison such as table 5.
Table 5
It is compared by table 5 it is found that the mixed bleach mixed in embodiment 6 using sodium hydroxide solution and hydrogen peroxide
Agent, the whiteness that crude fibre and microcrystalline cellulose is made are significantly better than the single bleaching agent hydrogen peroxide used in comparative example 6, make
The purity and yield for obtaining microcrystalline cellulose are also significantly better than the single bleaching agent hydrogen peroxide used in comparative example 6, and embodiment 6
The middle time for using bleaching agent to handle is 90min, and the bleaching time used in comparative example 6 is 120min.It is used in the present invention
The mixed bleach agent of sodium hydroxide and hydrogen peroxide composition can be obviously improved the yield of microcrystalline cellulose obtained, purity and white
Degree, and shorten bleaching time, hence it is evident that better than using single bleaching agent hydrogen peroxide.
The microcrystalline cellulose sample quality index that embodiment 4 is prepared is analyzed according to national standard, as shown in table 6,
The Chinese medicine slag microcrystalline cellulose of preparation meets national standard.
6 Chinese medicine slag of table prepares the quality analysis of food additives MCC
Claims (7)
1. a kind of method that Chinese medicine slag prepares microcrystalline cellulose, comprising the following steps:
A, Chinese medicine slag and deionized water are mixed with solid-to-liquid ratio 1:15-1:30g/mL, slightly boiled 100-120min, centrifugation must filter
Slag；
B, alkali process: filter residue obtained by step a is molten with solid-to-liquid ratio 1:10-1:15g/ml addition 0.02-0.08g/ml sodium hydroxide
Liquid, 50-80 DEG C of water bath processing 60-120min are centrifuged and wash and be precipitated to neutrality, collect filter residue；
C, acid processing: filter residue obtained by step b is added into distilled water with solid-to-liquid ratio 1:2-1:10g/ml, is 1%-5%'s with mass concentration
Hydrochloric acid, nitric acid, sulfuric acid or phosphoric acid tune pH value to 1-2,50-80 DEG C of constant temperature water bath handle 60-90 min, are centrifuged to obtain filter residue, wash
To neutrality, dewatered drying；
D, Chinese medicine slag crude fibre extracts: bleaching liquid is added with solid-to-liquid ratio 1:20-1:50g/ml in filter residue obtained by step c, it is described
The liquor natrii hypochloritis that bleaching liquid is the sodium sulfite solution that mass concentration is 1%-4% and available chlorine content is 3%-5% is isometric
The mixed bleach liquid of composition is mixed, 50-80 DEG C of water bath processing 60-90 min is filtered, washing to neutral, dewatered drying to constant weight,
Obtain Chinese medicine slag crude fibre；
E, matter microcrystalline cellulose processed: is added with solid-to-liquid ratio 1:10-1:20g/ml in Chinese medicine slag crude fibre obtained by step d
Amount concentration is 1%-6% hydrochloric acid solution, and 50-90 DEG C of water bath processing 65-115min is filtered, washed to neutral, dewatered drying to perseverance
Microcrystalline cellulose is made in weight.
2. the method that Chinese medicine slag as described in claim 1 prepares microcrystalline cellulose, wherein in the step d, the bleaching liquid
For mass concentration be 3% sodium sulfite solution and available chlorine content be 5% liquor natrii hypochloritis mix the mixed of composition in equal volume
Close bleaching liquid.
3. the method that Chinese medicine slag as described in claim 1 prepares microcrystalline cellulose, wherein in the step e, by step d institute
Chinese medicine slag crude fibre obtained with solid-to-liquid ratio 1:12-1:16g/ml be added mass concentration be 3%-5% hydrochloric acid solution, 60-80 DEG C
Water bath processing 65-85min filters, washs to neutral, dewatered drying to constant weight, microcrystalline cellulose is made.
4. the method that Chinese medicine slag as claimed in claim 3 prepares microcrystalline cellulose, wherein in the step e, by step d institute
Chinese medicine slag crude fibre obtained with solid-to-liquid ratio 1:14g/ml be added mass concentration be 4% hydrochloric acid solution, 70 DEG C of water bath processings
65min filters, washs to neutral, dewatered drying to constant weight, microcrystalline cellulose is made.
5. the method that Chinese medicine slag as claimed in claim 4 prepares microcrystalline cellulose, wherein dense using quality in the step c
Degree is the nitric acid of 1%-5%.
6. the method that Chinese medicine slag as described in claim 1 prepares microcrystalline cellulose, wherein in the step a, the Chinese medicine slag
Cellulose mass fraction is 15% or more.
7. the method that Chinese medicine slag as described in claim 1 prepares microcrystalline cellulose, wherein in the step a, the Chinese medicine slag
For the Chinese medicine slag generated after Radix Ophiopogonis, Schisandra chinensis, Rehmannia glutinosa, wine-prepared fructus corni, cortex moutan, Chinese yam, Poria cocos, the processing of rhizoma alismatis Chinese materia medica preparation.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710316191.6A CN106916231B (en) | 2017-05-08 | 2017-05-08 | A kind of method that Chinese medicine slag prepares microcrystalline cellulose |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710316191.6A CN106916231B (en) | 2017-05-08 | 2017-05-08 | A kind of method that Chinese medicine slag prepares microcrystalline cellulose |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106916231A CN106916231A (en) | 2017-07-04 |
| CN106916231B true CN106916231B (en) | 2019-07-16 |
Family
ID=59567891
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710316191.6A Active CN106916231B (en) | 2017-05-08 | 2017-05-08 | A kind of method that Chinese medicine slag prepares microcrystalline cellulose |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106916231B (en) |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107652070A (en) * | 2017-11-06 | 2018-02-02 | 张培栋 | Ecological sponge fertilizer is produced with the Chinese medicine slag treatment of wastes with processes of wastes against one another |
| CN108086029B (en) * | 2017-12-05 | 2021-04-09 | 成都中医药大学 | Magnolia officinalis leaf cellulose and preparation method and application thereof |
| CN108410923B (en) * | 2018-02-07 | 2021-07-23 | 兰州理工大学 | Method for preparing microcrystalline cellulose from sorghum straws |
| CN109627348B (en) * | 2018-12-28 | 2021-03-30 | 武汉理工大学 | Method for extracting microcrystalline cellulose from taxus media branch residues |
| CN110731360B (en) * | 2019-10-10 | 2023-07-04 | 广西科技师范学院 | Preparation method and application of food-grade microcrystalline cellulose |
| CN112934205A (en) * | 2021-02-24 | 2021-06-11 | 上海交通大学 | Preparation method and application of porous hydrogel adsorbent based on astragalus waste residues |
| 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 |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| BG19462A1 (en) * | 1973-08-02 | 1975-06-25 | ||
| CN102002875B (en) * | 2010-10-23 | 2012-01-18 | 吉林大学 | Method for preparing microcrystalline cellulose by using carrot pomace |
| CN103965365B (en) * | 2014-05-12 | 2016-03-02 | 甘肃农业大学 | A kind of preparation method of apple residue Microcrystalline Cellulose |
| CN104963227B (en) * | 2015-05-27 | 2017-04-12 | 深圳先进技术研究院 | Wheat bran microcrystalline cellulose and preparation method thereof |
-
2017
- 2017-05-08 CN CN201710316191.6A patent/CN106916231B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN106916231A (en) | 2017-07-04 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106916231B (en) | A kind of method that Chinese medicine slag prepares microcrystalline cellulose | |
| Wang et al. | Selective removal of lignin with sodium chlorite to improve the quality and antioxidant activity of xylo-oligosaccharides from lignocellulosic biomass | |
| CN1231144C (en) | Method for extracting edible bran fiber from wheat bran | |
| CN105838755B (en) | A kind of biological method extracting natural pectin from plant residue containing pectin | |
| CN103614435A (en) | Method for preparing xylo-oligosaccharide from bagasse | |
| CN110230228A (en) | The method of stalk coproduction cellulosic material, furfural and lignin | |
| CN105986497A (en) | Process for extracting cellulose from natural wormwood | |
| CN101649569B (en) | Process for preparing low-pollution wheatgrass microcrystalline cellulose | |
| CN107303578A (en) | It is a kind of to comprehensively utilize the method that straw prevents and treats industrial pollution | |
| CN109988060A (en) | A kind of extracting method of cannabidiol | |
| CN105249481B (en) | It is a kind of extracted by mulberry leaf after the residue method of producing high swelling property dietary fiber | |
| CN102225970B (en) | Extraction method of polysaccharide from potentilla discolor | |
| CN111472186B (en) | Method for preparing high-quality crop straw dissolving pulp through hydrothermal pretreatment | |
| CN104523765A (en) | Preparation method of poria cocos formula granule | |
| CN106832051A (en) | A kind of preparation method of Chinese fiber crops pectin and the new Chinese fiber crops jelly powder prepared according to the method | |
| CN106496337B (en) | The preparation method of microcrystalline cellulose | |
| CN101649570B (en) | Process for preparing wheatgrass cellulose with low pollution | |
| CN103442816A (en) | Pre-treatment method for plant biomass hydrolysis reaction raw materials and plant biomass saccharification method | |
| CN102925516A (en) | Xylo-oligosaccharide preparation method | |
| CN105239435A (en) | Treatment method of wood fiber raw material | |
| CN105076921A (en) | Method for producing microcrystalline cellulose by utilizing leftovers of bamboo shoots | |
| CN109602783A (en) | A kind of method of enzyme assisted extraction folium cortex eucommiae active constituent | |
| CN108017724A (en) | A kind of preparation method of plant-derived chitosan | |
| CN1243487C (en) | Sea-tangle edible fiber and its making method | |
| CN1166319C (en) | Productive technology for extracting diet fiber from-sargassum |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20201026 Address after: No.428, Qingyang Road, Zhangye road street, Chengguan District, Lanzhou City, Gansu Province Patentee after: Lanzhou Mingde Pharmaceutical Co., Ltd Address before: 730050 Qilihe, Gansu Province Lan Ping Ping Road, No. 287, No. Patentee before: LANZHOU University OF TECHNOLOGY |