CN103265711A - Method for preparing colloidal microcrystalline cellulose (MCC) - Google Patents
Method for preparing colloidal microcrystalline cellulose (MCC) Download PDFInfo
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- CN103265711A CN103265711A CN2013102141739A CN201310214173A CN103265711A CN 103265711 A CN103265711 A CN 103265711A CN 2013102141739 A CN2013102141739 A CN 2013102141739A CN 201310214173 A CN201310214173 A CN 201310214173A CN 103265711 A CN103265711 A CN 103265711A
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- microcrystalline cellulose
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Abstract
The invention discloses a method for preparing colloidal microcrystalline cellulose (MCC). Common food-grade MCC (with particle diameter 30 to 40mum) and sodium carboxymethyl cellulose (CMC) undergo dispersion, shear (the particle diameter is reduced through shear, and the MCC with the particle diameter less than 2mum is named as colloidal MCC) and spray drying to form a fine particle product. The obtained colloidal MCC product has good dispersion performance and suspension performance, and the aqueous solution of the product has the three-dimensional network structure suspension mechanism, has super thermal stability and acid resistance and can be used as an excellent suspension stabilizer in the industries of medicine, food and the like.
Description
Technical field
The preparation method of colloidal state grade microcrystalline cellulose of the present invention (MCC), its three-dimensional net structure has fabulous thermostability and acid resistance, a kind of good suspension stablizer that belongs to medicine and field of food uses, particularly the preparation method of a kind of colloidal state grade microcrystalline cellulose (MCC).
Background technology
Microcrystalline Cellulose (Microcrystalline cellulose is called for short MCC) is the certain limit molecular weight ultrafine powder product that the natural cellulose hydrolysis produces.Functions such as MCC has viscosity adjustment, promotes into glue, stable suspersion (particle diameter less than 2 μ m time just suspend good), alternative fats, agglomeration resistance are the extremely strong green additives of biocompatibility, have extensive use in industries such as medicine, food, makeup.The size of its molecular weight or fineness has determined it to use effect and marketable value.Particle diameter is called colloidal mcc less than the MCC of 2 μ m, and it is the high-end product in the MCC series product, and its production difficulty is big, with high content of technology, and marketable value is huge simultaneously.The MCC product generally method production, a large amount of contaminated wastewater two large problems of corresponding production technique ubiquity product fineness finite sum such as separates altogether by natural cellulose acidolysis, enzymolysis or sour enzyme.Because the natural cellulose crystallinity is very strong, the acid enzymolysis, or sour enzymolysis is difficult to realize effective reduction of Mierocrystalline cellulose particle diameter in conjunction with the production method of mechanical disintegration, cause the median size of present homemade MCC to be generally more than 20～30 μ m, be difficult to promote its economy and using value.The acid enzymolysis process needs a large amount of water to make solvent, certainly leads to a large amount of waste water, serious environment pollution, and it is very big to administer pressure.Therefore developing the environmental protection technology that the small particle size colloidal mcc is produced, is the inexorable trend of MCC development.
Summary of the invention
The objective of the invention is to overcome the deficiency of prior art, a kind of environmental protection technology is provided, the preparation method of colloidal state grade microcrystalline cellulose, make and adopt colloidal state grade microcrystalline cellulose product cut size that this preparation method obtains less than 2 μ m, dispersing property and suspension property are good, its aqueous solution has three-dimensional net structure suspension mechanism, and fabulous thermostability and acid resistance are arranged, and can be used as industry good suspension stablizers such as medicine, food and uses.
For solving the problems of the technologies described above, the technical solution used in the present invention is as follows:
A kind of preparation method of colloidal state grade microcrystalline cellulose, this preparation method is to be 100 raw material with bread and cheese grade microcrystalline cellulose (particle diameter 30～40 μ m) parts by weight earlier, with parts by weight be that 800～1400 soft water is added to high-shear emulsion machine, start shears, adding parts by weight slowly are 8～15 food grade Xylo-Mucine product, and emulsification times is 25～40 minutes at normal temperatures; After emulsification finishes; Material is transported to high pressure homogenizer (standard mechanical through spiral pump, outsourcing is arranged) shear, control pressure 15～30MPa for the first time, material after high pressure homogenizer is sheared flows to next high-shear emulsion machine, material is transported to high pressure homogenizer through spiral pump and shears, control pressure 50～80MPa for the second time, material after high pressure homogenizer is sheared flows to next high-shear emulsion machine, being transported to high pressure homogenizer through spiral pump shears, control pressure 100～150MPa for the third time, material after high pressure homogenizer is sheared flows to next high-shear emulsion machine, material is transported to spray-drier through spiral pump, spray-dried back becomes tiny granular material, namely obtains colloidal state grade microcrystalline cellulose (colloidal state level MCC, particle diameter is less than 2 μ m);
In the technique scheme, preparation method of the present invention uses bread and cheese grade microcrystalline cellulose (particle diameter 30～40 μ m) as raw material.
High-shear emulsion machine and high pressure homogenizer that preparation method of the present invention uses all are standard mechanicals, purchase on market.This preparation method is simple, and is easy to operate, can effectively reduce total production cost.The colloidal state grade microcrystalline cellulose that the present invention obtains (colloidal state level MCC, particle diameter is less than 2 μ m) product, dispersing property and suspension property are good, its aqueous solution has three-dimensional net structure suspension mechanism, and fabulous thermostability and acid resistance are arranged, can be used as industry good suspension stablizers such as medicine, food and use.
Embodiment
Embodiment 1: be 100 raw material with bread and cheese grade microcrystalline cellulose (particle diameter 30～40 μ m) parts by weight earlier, with parts by weight be that 900 soft water is added to high-shear emulsion machine, start shears, adding parts by weight slowly are 9 food grade Xylo-Mucine product, and emulsification times is 30 minutes at normal temperatures; After emulsification finishes; Material is transported to high pressure homogenizer (standard mechanical through spiral pump, outsourcing is arranged) shear, control pressure 20MPa for the first time, material after high pressure homogenizer is sheared flows to next high-shear emulsion machine, material is transported to high pressure homogenizer through spiral pump and shears, control pressure 50MPa for the second time, material after high pressure homogenizer is sheared flows to next high-shear emulsion machine, being transported to high pressure homogenizer through spiral pump shears, control pressure 100MPa for the third time, material after high pressure homogenizer is sheared flows to next high-shear emulsion machine, material is transported to spray-drier through spiral pump, spray-dried back becomes tiny granular material, namely obtains colloidal state grade microcrystalline cellulose (colloidal state level MCC, particle diameter is less than 2 μ m).
The product physical and chemical index that above-described embodiment 1 is made is by the determination of test method in the Chinese Pharmacopoeia, and is all qualified, recorded by particle size analyzer: product cut size 1.2 μ m, and get product 2g and be placed in the 1000ml distilled water, become very muddy suspension.
Embodiment 2: be 100 raw material with bread and cheese grade microcrystalline cellulose (particle diameter 30～40 μ m) parts by weight earlier, with parts by weight be that 1100 soft water is added to high-shear emulsion machine, start shears, adding parts by weight slowly are 11 food grade Xylo-Mucine product, and emulsification times is 35 minutes at normal temperatures; After emulsification finishes; Material is transported to high pressure homogenizer (standard mechanical through spiral pump, outsourcing is arranged) shear, control pressure 25MPa for the first time, material after high pressure homogenizer is sheared flows to next high-shear emulsion machine, material is transported to high pressure homogenizer through spiral pump and shears, control pressure 60MPa for the second time, material after high pressure homogenizer is sheared flows to next high-shear emulsion machine, being transported to high pressure homogenizer through spiral pump shears, control pressure 120MPa for the third time, material after high pressure homogenizer is sheared flows to next high-shear emulsion machine, material is transported to spray-drier through spiral pump, spray-dried back becomes tiny granular material, namely obtains colloidal state grade microcrystalline cellulose (colloidal state level MCC, particle diameter is less than 2 μ m).
The product physical and chemical index that above-described embodiment 2 is made is by the determination of test method in the Chinese Pharmacopoeia, and is all qualified, recorded by particle size analyzer: product cut size 1.1 μ m, and get product 2g and be placed in the 1000ml distilled water, become very muddy suspension.
Embodiment 3: be 100 raw material with bread and cheese grade microcrystalline cellulose (particle diameter 30～40 μ m) parts by weight earlier, with parts by weight be that 1250 soft water is added to high-shear emulsion machine, start shears, adding parts by weight slowly are 12 food grade Xylo-Mucine product, and emulsification times is 40 minutes at normal temperatures; After emulsification finishes; Material is transported to high pressure homogenizer (standard mechanical through spiral pump, outsourcing is arranged) shear, control pressure 25MPa for the first time, material after high pressure homogenizer is sheared flows to next high-shear emulsion machine, material is transported to high pressure homogenizer through spiral pump and shears, control pressure 70MPa for the second time, material after high pressure homogenizer is sheared flows to next high-shear emulsion machine, being transported to high pressure homogenizer through spiral pump shears, control pressure 140MPa for the third time, material after high pressure homogenizer is sheared flows to next high-shear emulsion machine, material is transported to spray-drier through spiral pump, spray-dried back becomes tiny granular material, namely obtains colloidal state grade microcrystalline cellulose (colloidal state level MCC, particle diameter is less than 2 μ m).
The product physical and chemical index that above-described embodiment 3 is made is by the determination of test method in the Chinese Pharmacopoeia, and is all qualified, recorded by particle size analyzer: product cut size 1.0 μ m, and get product 2g and be placed in the 1000ml distilled water, become very muddy suspension.
To sum up state, colloidal state grade microcrystalline cellulose (the colloidal state level MCC that obtains according to the present invention, particle diameter is less than 2 μ m) product, dispersing property and suspension property are good, its aqueous solution has three-dimensional net structure suspension mechanism, and fabulous thermostability and acid resistance are arranged, can be used as industry good suspension stablizers such as medicine, food and use.
Claims (6)
1. the preparation method of a colloidal state grade microcrystalline cellulose (MCC), bread and cheese grade microcrystalline cellulose (particle diameter 30～40 μ m), process and Xylo-Mucine (CMC) disperse together, shear (by shearing its particle diameter of reduction, particle diameter claims colloidal mcc less than the MCC of 2 μ m), spraying drying and make the product of fine particle, it is characterized in that:
Using at above-mentioned raw materials is the bread and cheese grade microcrystalline cellulose;
In above-mentioned dispersion step, employed is high-shear emulsion machine (standard mechanical, outsourcing is arranged), during beginning, is 100 raw material with bread and cheese grade microcrystalline cellulose (particle diameter 30～40 μ m) parts by weight earlier, with parts by weight be that 800～1400 soft water is added to high-shear emulsion machine, start shears, adding parts by weight slowly are 8～15 food grade Xylo-Mucine product, and emulsification times is 25～40 minutes at normal temperatures; After emulsification finishes; Material is transported to high pressure homogenizer (standard mechanical through spiral pump, outsourcing is arranged) shear, control pressure 15～30MPa for the first time, material after high pressure homogenizer is sheared flows to next high-shear emulsion machine, material is transported to high pressure homogenizer through spiral pump and shears, control pressure 50～80MPa for the second time, material after high pressure homogenizer is sheared flows to next high-shear emulsion machine, being transported to high pressure homogenizer through spiral pump shears, control pressure 100～150MPa for the third time, material after high pressure homogenizer is sheared flows to next high-shear emulsion machine, material is transported to spray-drier through spiral pump, spray-dried back becomes tiny granular material, namely obtains colloidal state grade microcrystalline cellulose (colloidal state level MCC).
2. colloidal state grade microcrystalline cellulose preparation method according to claim 1 is characterized in that, in above-mentioned dispersion step, use be high-shear emulsion machine (standard mechanical has outsourcing).
3. colloidal state grade microcrystalline cellulose preparation method according to claim 1 is characterized in that, in above-mentioned cutting operation, use be high pressure homogenizer (standard mechanical has outsourcing).
4. colloidal state grade microcrystalline cellulose preparation method according to claim 1 is characterized in that, above-mentioned dispersion step adds parts by weight and be 8～15 food grade Xylo-Mucine product and bread and cheese grade microcrystalline cellulose dispersion and emulsion together.
5. colloidal state grade microcrystalline cellulose preparation method according to claim 1 is characterized in that above-mentioned cutting operation, material is through three sub-high pressure homogeneous, its homogenization pressure, control pressure 15～30MPa for the first time, for the second time control pressure 50～80MPa, control pressure 100～150MPa for the third time.
6. colloidal state grade microcrystalline cellulose preparation method according to claim 1 is characterized in that, the material homogeneous finishes to be transported to spray-drier, and spray-dried back becomes tiny granular material, namely obtains colloidal state grade microcrystalline cellulose (colloidal state level MCC).
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| CN2013102141739A CN103265711A (en) | 2013-06-03 | 2013-06-03 | Method for preparing colloidal microcrystalline cellulose (MCC) |
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| CN2013102141739A CN103265711A (en) | 2013-06-03 | 2013-06-03 | Method for preparing colloidal microcrystalline cellulose (MCC) |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105597101A (en) * | 2015-09-28 | 2016-05-25 | 广东国源国药制药有限公司 | Innovative pharmaceutic adjuvant colloidal microcrystalline cellulose and preparation method thereof |
| CN111333875A (en) * | 2020-04-13 | 2020-06-26 | 牡丹江霖润药用辅料有限责任公司 | Superfine high-performance microcrystalline cellulose product and preparation method thereof |
| CN111802448A (en) * | 2020-07-16 | 2020-10-23 | 江西中医药大学 | Compound plant essential oil sterilization preservative and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1222527A (en) * | 1998-12-30 | 1999-07-14 | 中国科学院广州化学研究所 | Preparation of microcrystal cellulose colloid |
| WO2013052114A1 (en) * | 2011-10-05 | 2013-04-11 | Fmc Corporation | Stabilizer composition of microcrystalline cellulose and carboxymethylcellulose, method for making, and uses |
-
2013
- 2013-06-03 CN CN2013102141739A patent/CN103265711A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1222527A (en) * | 1998-12-30 | 1999-07-14 | 中国科学院广州化学研究所 | Preparation of microcrystal cellulose colloid |
| WO2013052114A1 (en) * | 2011-10-05 | 2013-04-11 | Fmc Corporation | Stabilizer composition of microcrystalline cellulose and carboxymethylcellulose, method for making, and uses |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105597101A (en) * | 2015-09-28 | 2016-05-25 | 广东国源国药制药有限公司 | Innovative pharmaceutic adjuvant colloidal microcrystalline cellulose and preparation method thereof |
| CN111333875A (en) * | 2020-04-13 | 2020-06-26 | 牡丹江霖润药用辅料有限责任公司 | Superfine high-performance microcrystalline cellulose product and preparation method thereof |
| CN111333875B (en) * | 2020-04-13 | 2023-02-07 | 牡丹江霖润药用辅料有限责任公司 | Superfine high-performance microcrystalline cellulose product and preparation method thereof |
| CN111802448A (en) * | 2020-07-16 | 2020-10-23 | 江西中医药大学 | Compound plant essential oil sterilization preservative and preparation method thereof |
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Application publication date: 20130828 |