CN104557507A - Method for preparing magnesium stearate - Google Patents
Method for preparing magnesium stearate Download PDFInfo
- Publication number
- CN104557507A CN104557507A CN201310525505.5A CN201310525505A CN104557507A CN 104557507 A CN104557507 A CN 104557507A CN 201310525505 A CN201310525505 A CN 201310525505A CN 104557507 A CN104557507 A CN 104557507A
- Authority
- CN
- China
- Prior art keywords
- magnesium stearate
- saponification reaction
- metathesis
- replacement
- tablet hardness
- 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.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/41—Preparation of salts of carboxylic acids
- C07C51/412—Preparation of salts of carboxylic acids by conversion of the acids, their salts, esters or anhydrides with the same carboxylic acid part
Abstract
The invention discloses a method for preparing magnesium stearate which neither holds up drug dissolution nor reduces tablet hardness. The method comprises the processes of saponification, replacement reaction, washing and drying, hot-melt extrusion, grinding and sieving and the like. 1865 stearic acid, caustic soda flacks and magnesium sulphate are used as main raw materials, and the obtained magnesium stearate can be used for remarkably avoiding adverse phenomena of holding up drug dissolution and reducing tablet hardness due to the over-lubrication effect, has the specific volume lower than 1.5g/ml and the angle of repose of 30 degrees, and is capable of effectively improving the tablet hardness by about 30% and fully improving drug dissolution when used in a tablet at the same proportion as ordinary magnesium stearate.
Description
Technical field
The present invention relates to a kind of preparation method of Magnesium Stearate, particularly relate to the stripping of a kind of not blocking medicine and do not reduce the preparation method of Magnesium Stearate of tablet hardness, belong to organic chemical industry field.
Background technology
Magnesium Stearate is that white is easily without the fine powder of grittiness; Micro-have special smell; There is soapy feeling with skin contact, be mainly used as lubricant, antisticking agent, glidant.The granulation of special appropriate oil, extract medicament, the particle made has good mobility and compressibility.Glidant etc. is used as in direct compression.It is widely used in makeup, food and pharmaceutical preparation.
Magnesium Stearate is when the preparation of solid preparation, and the bulk drug especially large for viscosity, material fluidity is poor, the excellent oilness of Magnesium Stearate and resistance to bond serve most important and irreplaceable effect in the preparation of tablet.But Magnesium Stearate is hydrophobicity, usually there will be because crossing the blocking medicine stripping that lubricating effect causes and the bad phenomenon reducing tablet hardness.It is when mixing with tablet and powder, and the variation coefficient of mixing is increased, and tablet crushing strength reduces, thus the hardness of tablet is reduced and the stripping from solid dosage of energy blocking medicine.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of Magnesium Stearate, Magnesium Stearate prepared by described method, when the preparation for solid preparation, can avoid the bad phenomenon producing blocking medicine stripping because crossing lubricating effect and reduce tablet hardness.
The present invention is achieved by the following technical solutions: a kind of preparation method of Magnesium Stearate comprises the following steps:
1) saponification reaction: drop into tap water 800 ~ 1000kg and open heating, treat that temperature-stable rises to 50 DEG C, according to dosage than input sheet alkali 12 ~ 16kg, be heated with stirring to 80 ~ 95 DEG C, add 1865 type stearic acid 80 ~ 100kg, limit edged stirs, saponification reaction time 30 ~ 50min
2) replacement(metathesis)reaction: saponification reaction terminates slowly to add magnesium sulfate 35 ~ 60kg afterwards, is now cooled to 70 ~ 85 DEG C of replacement(metathesis)reaction time 25 ~ 45min;
3) washing is dry: purified water washing material, to neutral, adopts expansion drying to material moisture 10 ~ 15%;
4) hot-melt extruded: adopt twin screw extruder to carry out hot-melt extruded operation to material, making material when reaching its molten distance 110 ~ 128 DEG C, crystal formation occurring and changes, forming white clear granular crystals;
5) crystalline thing crushed and screened and obtain not blocking medicine stripping and do not reduce the Magnesium Stearate of tablet hardness.
Technique effect of the present invention is: stearic model used is 1865 types, when effectively can reach hot-melt extruded crystal formation change needed for the melting range temperature that reaches; Adopt torching mark, make material when reaching its melting range 110 ~ 128 DEG C, generation crystal formation changes, form white clear granular crystals, Magnesium Stearate obtained after crushing and screening can significantly be avoided because crossing the blocking medicine stripping that lubricating effect produces and the bad phenomenon reducing tablet hardness, meanwhile, the Magnesium Stearate prepared by the present invention possesses again quite excellent mobility, resistance to bond and helps the advantages such as fluidity compared with common Magnesium Stearate.The Magnesium Stearate bulking value that the present invention obtains is lower than 1.5g/ml, and 30 °, slope of repose, when using in tablets in proportion with common Magnesium Stearate, can effectively improve tablet hardness and reach about 30%; And substantially improve drug-eluting.
Embodiment
For convenience of explanation, the present invention is illustrated in detail below in conjunction with embodiment.
Embodiment 1
1. saponification reaction: drop into tap water 800kg and open heating, treat that temperature-stable rises to 50 DEG C, according to dosage than input sheet alkali 13kg, be heated with stirring to 85 DEG C, add 1865 type stearic acid 90kg, limit edged stirs, saponification reaction time 30min;
2. replacement(metathesis)reaction: saponification reaction terminates slowly to add magnesium sulfate 50kg afterwards, is now cooled to 80 DEG C of replacement(metathesis)reaction time 40min;
3. washing is dry: purified water washing material, to neutral, adopts expansion drying to material moisture 15%;
4. hot-melt extruded: adopt twin screw extruder to carry out hot-melt extruded operation to material, when reaching 118 DEG C, there is crystal formation and changing, forming white clear granular crystals in material;
5., after crystalline thing crushes and screens, obtained bulking value 1.4g/ml, slope of repose are the modified form Magnesium Stearate 85kg of 30 °.
Embodiment 2
1. saponification reaction: drop into tap water 900kg and open heating, treat that temperature-stable rises to 50 DEG C, according to dosage than input sheet alkali 14kg, be heated with stirring to 89 DEG C, add 1865 type stearic acid 85kg, limit edged stirs, saponification reaction time 35min;
2. replacement(metathesis)reaction: saponification reaction terminates slowly to add magnesium sulfate 45kg afterwards, is now cooled to 75 DEG C of replacement(metathesis)reaction time 42min;
3. washing is dry: purified water washing material, to neutral, adopts expansion drying to material moisture 14%;
4. hot-melt extruded: adopt twin screw extruder to carry out hot-melt extruded operation to material, when reaching 116 DEG C, there is crystal formation and changing, forming white clear granular crystals in material;
5., after crystalline thing crushes and screens, obtained bulking value 1.4g/ml, slope of repose are the modified form Magnesium Stearate 80.1kg of 31 °.
Embodiment 3
1. saponification reaction: drop into tap water 900kg and open heating, treat that temperature-stable rises to 50 DEG C, according to dosage than input sheet alkali 15kg, be heated with stirring to 92 DEG C, add 1865 type stearic acid 95kg, limit edged stirs, saponification reaction time 40min;
2. replacement(metathesis)reaction: saponification reaction terminates slowly to add magnesium sulfate 48kg afterwards, is now cooled to 80 DEG C of replacement(metathesis)reaction time 46min;
3. washing is dry: purified water washing material, to neutral, adopts expansion drying to material moisture 13%;
4. hot-melt extruded: adopt twin screw extruder to carry out hot-melt extruded operation to material, when reaching 120 DEG C, there is crystal formation and changing, forming white clear granular crystals in material;
5., after crystalline thing crushes and screens, obtained bulking value 1.5g/ml, slope of repose are the modified form Magnesium Stearate 87kg of 30 °.
Embodiment 4
1. saponification reaction: drop into tap water 1000kg and open heating, treat that temperature-stable rises to 50 DEG C, according to dosage than input sheet alkali 16kg, be heated with stirring to 95 DEG C, add 1865 type stearic acid 100kg, limit edged stirs, saponification reaction time 50min;
2. replacement(metathesis)reaction: saponification reaction terminates slowly to add magnesium sulfate 60kg afterwards, is now cooled to 85 DEG C of replacement(metathesis)reaction time 25min;
3. washing is dry: purified water washing material, to neutral, adopts expansion drying to material moisture 15%;
4. hot-melt extruded: adopt twin screw extruder to carry out hot-melt extruded operation to material, when reaching 128 DEG C, there is crystal formation and changing, forming white clear granular crystals in material;
5., after crystalline thing crushes and screens, obtained bulking value 1.5g/ml, slope of repose are the modified form Magnesium Stearate 95kg of 31 °.
Embodiment 5
1. saponification reaction: drop into tap water 900kg and open heating, treat that temperature-stable rises to 50 DEG C, according to dosage than input sheet alkali 12kg, be heated with stirring to 80 DEG C, add 1865 type stearic acid 80kg, limit edged stirs, saponification reaction time 40min;
2. replacement(metathesis)reaction: saponification reaction terminates slowly to add magnesium sulfate 35kg afterwards, is now cooled to 70 DEG C of replacement(metathesis)reaction time 45min;
3. washing is dry: purified water washing material, to neutral, adopts expansion drying to material moisture 13%;
4. hot-melt extruded: adopt twin screw extruder to carry out hot-melt extruded operation to material, when reaching 110 DEG C, there is crystal formation and changing, forming white clear granular crystals in material;
5., after crystalline thing crushes and screens, obtained bulking value 1.4g/ml, slope of repose are the modified form Magnesium Stearate 68.1kg of 30 °.
Claims (1)
1. a preparation method for Magnesium Stearate, is characterized in that comprising the following steps:
1) saponification reaction: drop into tap water 800 ~ 1000kg and open heating, treat that temperature-stable rises to 50 DEG C, according to dosage than input sheet alkali 12 ~ 16kg, be heated with stirring to 80 ~ 95 DEG C, add 1865 type stearic acid 80 ~ 100kg, limit edged stirs, saponification reaction time 30 ~ 50min
2) replacement(metathesis)reaction: saponification reaction terminates slowly to add magnesium sulfate 35 ~ 60kg afterwards, is now cooled to 70 ~ 85 DEG C of replacement(metathesis)reaction time 25 ~ 45min;
3) washing is dry: purified water washing material, to neutral, adopts expansion drying to material moisture 10 ~ 15%;
4) hot-melt extruded: adopt twin screw extruder to carry out hot-melt extruded operation to material, making material when reaching its molten distance 110 ~ 128 DEG C, crystal formation occurring and changes, forming white clear granular crystals;
5) crystalline thing crushed and screened and obtain not blocking medicine stripping and do not reduce the Magnesium Stearate of tablet hardness.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310525505.5A CN104557507B (en) | 2013-10-31 | 2013-10-31 | A kind of preparation method of Magnesium Stearate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310525505.5A CN104557507B (en) | 2013-10-31 | 2013-10-31 | A kind of preparation method of Magnesium Stearate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104557507A true CN104557507A (en) | 2015-04-29 |
| CN104557507B CN104557507B (en) | 2016-04-13 |
Family
ID=53074690
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310525505.5A Active CN104557507B (en) | 2013-10-31 | 2013-10-31 | A kind of preparation method of Magnesium Stearate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104557507B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104892399A (en) * | 2015-05-07 | 2015-09-09 | 溧阳市云凯化工有限公司 | Lithium stearate production process |
| CN109528956A (en) * | 2018-12-27 | 2019-03-29 | 郑州大学第附属医院 | It is a kind of to reduce Steroid-resistant nephrotic syndrome patient to the drug of Hormone refractory |
| CN111003783A (en) * | 2019-12-30 | 2020-04-14 | 南通新邦化工科技有限公司 | Method for reducing PH value of wastewater in stearate production |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102372620A (en) * | 2010-08-17 | 2012-03-14 | 安徽山河药用辅料股份有限公司 | Preparation method of magnesium stearate with improved specific volume and whiteness |
-
2013
- 2013-10-31 CN CN201310525505.5A patent/CN104557507B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102372620A (en) * | 2010-08-17 | 2012-03-14 | 安徽山河药用辅料股份有限公司 | Preparation method of magnesium stearate with improved specific volume and whiteness |
Non-Patent Citations (1)
| Title |
|---|
| EVA ROBLEGG ET AL.: "Development of sustained-release lipophilic calcium stearate pellets via hot melt extrusion", 《EUROPEAN JOURNAL OF PHARMACEUTICS AND BIOPHARMACEUTICS》, 31 December 2011 (2011-12-31), pages 1 - 11 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104892399A (en) * | 2015-05-07 | 2015-09-09 | 溧阳市云凯化工有限公司 | Lithium stearate production process |
| CN109528956A (en) * | 2018-12-27 | 2019-03-29 | 郑州大学第附属医院 | It is a kind of to reduce Steroid-resistant nephrotic syndrome patient to the drug of Hormone refractory |
| CN111003783A (en) * | 2019-12-30 | 2020-04-14 | 南通新邦化工科技有限公司 | Method for reducing PH value of wastewater in stearate production |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104557507B (en) | 2016-04-13 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Chattoraj et al. | Crystal and particle engineering strategies for improving powder compression and flow properties to enable continuous tablet manufacturing by direct compression | |
| CN104557507B (en) | A kind of preparation method of Magnesium Stearate | |
| CN103819271B (en) | A kind of manufacture method of novel particle Repone K fertilizer | |
| KR101515683B1 (en) | Natural lubricants for direct compression and method for preparation natural tablet using the same | |
| CN103146916B (en) | A kind of method of granulating of high titanium slag, golden red stone flour | |
| NO166034B (en) | DIRECT COMPRESSABLE, GRANULAR MANNITOL AND A PROCEDURE FOR MANUFACTURING THEREOF. | |
| DE102013004597A1 (en) | Process for press granulation of non-ductile salts | |
| CN101270206A (en) | Biodegradation plastics with high-content of starch for producing tableware and method of producing the same | |
| RU2010107185A (en) | DEXTROSA FOR DIRECT PRESS | |
| CN103820583B (en) | A kind of preparation method of granular compressible sugar | |
| CA2656181A1 (en) | Compressed preparation of compositions comprising olmesartan medoxomil | |
| CN102716092B (en) | Formula of aureomycin hydrochloride premix granule and granulating process | |
| CN105616407A (en) | Clopidogrel hydrogen sulfate solid preparation and preparation method thereof | |
| HRP20120583T1 (en) | Flupentixol compositions | |
| CA2648667A1 (en) | Sustained-release tablet production process | |
| PH12020551285A1 (en) | Granular composition, production method for granular composition, and dissolution property improvement method for granular composition | |
| JP6338413B2 (en) | Slag granulator and method for producing the same | |
| CN102048736A (en) | Dasatinib pharmaceutical composition and preparation method thereof | |
| KR101520121B1 (en) | Process for producing a free-flowing and storage-stable solid comprising essentially alpha-alanine-n,n-diacetic acid and/or one or more derivatives of alpha-alanine-n,n-diacetic acid | |
| CN102077955A (en) | Soluble konjac dietary fiber tablets and preparation method thereof | |
| MX2021013343A (en) | Mixture of steam-cracked biomass and lignin for granule production. | |
| JP5778921B2 (en) | Method for producing lime granular material | |
| CN102204910B (en) | Pharmaceutical composition of moxifloxacin hydrochloride, and preparation method thereof | |
| CN104840972A (en) | Tablet preparation method capable of overcoming hang punching of tablet press | |
| JP2008187959A (en) | Method for producing solid coffee |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |