CN101747175B - Medicinal-grade magnesium stearate and refining process thereof - Google Patents
Medicinal-grade magnesium stearate and refining process thereof Download PDFInfo
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- CN101747175B CN101747175B CN 200910265330 CN200910265330A CN101747175B CN 101747175 B CN101747175 B CN 101747175B CN 200910265330 CN200910265330 CN 200910265330 CN 200910265330 A CN200910265330 A CN 200910265330A CN 101747175 B CN101747175 B CN 101747175B
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Abstract
The invention provides a medicinal-grade magnesium stearate and a refining process thereof. The process comprises the following steps: (a) adding a food-grade magnesium stearate in a dissolving tank and then adding absolute ethyl alcohol, stirring for 15 to 30 minutes at the speed of 100 to 150 rpm under the temperature of 50 to 70 DEG C, wherein the mixing proportion of the magnesium stearates and the absolute ethyl alcohol is 1 to 10 (g/ml); (b) adding 10 to 20 g/ml sepiolite absorbents modified by iron to the obtained solution for oscillation and absorption for 2 to 3 h and then filtering; (c) distilling the filtrate at reduced pressure under the temperature of 60 to 70 DEG C to recover ethyl alcohol, thereby collecting a product; (d) adding the product in the dissolving tank and adding purified water, stirring for 15 to 30 minutes at the speed of 100 to 150 rpm under the temperature of 70 to 90 DEG C, wherein the mixing proportion of the magnesium stearates and the purified water is 1 to 8 (g/ml); (e) filtering, drying, sieving, testing and split charging to obtain the product.
Description
Technical field
The present invention relates to field of pharmaceutical excipients, especially relate to a kind of medicinal-grade magnesium stearate and process for purification thereof.
Background technology
Magnesium Stearate, molecular formula are Mg (C
17H
35COO)
2Be widely used in makeup, food and pharmaceutical preparation industry, be mainly used in the lubricant releasing agent of tablet, also can be used as the batching of makeup and coordinate with calcium soap, zinc soap for the stablizer of polyvinyl chloride and the siccative of paint, produced Social benefit and economic benefit preferably.Magnesium Stearate it has been generally acknowledged that oral nontoxic as the pharmaceutical excipient of widespread use.In the capsule and tablet manufacturing of medicine, mainly as lubricant and vehicle, working concentration is generally 0.25%-5.0% (w/w) for it.Yet, a large amount of can cause diarrhoea or mucosa irritation after oral.At present the Magnesium Stearate major part is by chemical industry, food enterprise production at home, though there is enterprise that medicinal standard has an approval number of the drug seldom.
In Chinese Pharmacopoeia, for the Magnesium Stearate that is used for medicinal use, strict regulation is arranged, for example heavy metal content should not surpass 20ppm.Because industrial Magnesium Stearate can not the fulfilling medicinal standard, therefore the heavy metal content in Magnesium Stearate and sulphate content are had higher requirement.Traditional Magnesium Stearate mainly synthesizes by double decomposition, the synthetic Magnesium Stearate purity of the method is low, tankage is large, production efficiency is low, energy consumption and the water consumption high, the shortcoming that heavy metal content and sulphate content are high is not suitable for medicinal use.
Therefore, market has demand to the medicinal-grade magnesium stearate of the low-heavy metal content that can satisfy the pharmaceutical industries demand.
Summary of the invention
In order to solve above-mentioned prior art problem, the invention provides a kind of medicinal-grade magnesium stearate that can satisfy the low-heavy metal content of pharmaceutical industries demand.
Magnesium Stearate content of the present invention is greater than 99.8%, and heavy metal content satisfies Chinese Pharmacopoeia and the Sanitation Ministry medicine standard to the requirement of heavy metal content in medicinal-grade magnesium stearate less than 10ppm.
The present invention also provides a kind of method for preparing the medicinal-grade magnesium stearate of low-heavy metal content and vitriol, chloride content, and the method comprises the following steps:
(a) the food grade Magnesium Stearate is joined in dissolving vessel, add dehydrated alcohol, stirring velocity with 100-150rpm at the temperature of 50-70 ℃ stirs 15-30 minute fully to dissolve, and wherein the blending ratio of Magnesium Stearate and dehydrated alcohol is 1: 10 (g/ml);
(b) add the meerschaum adsorbent vibration absorption 2-3h of 10-20g/L iron modification in the solution that obtains in step (a), filter;
(c) ethanol is reclaimed in filtrate underpressure distillation at 60-70 ℃ of temperature, collects product;
(d) product with gained joins in dissolving vessel, add purified water, stirring velocity with 100-150rpm at the temperature of 70-90 ℃ stirs 15-30 minute fully to wash, and wherein the blending ratio of Magnesium Stearate and purified water is 1: 8 (g/ml);
(e) filter, isolate solid substance, discard filtrate;
(f) with the material that separates in the baking oven of 70-90 ℃ dry 4-6 hour;
(g) crushing material with drying sieves, and the check packing is to obtain product.
In the specific embodiment of the present invention, in step (b), add in the described food grade Magnesium Stearate and account for the meerschaum adsorbent that its mass ratio is the iron modification of 1.5-5%, perhaps add the amount of iron modified meerschaum sorbent material to be preferably 15-18g/L, normal temperature vibration adsorption time is 2 hours.
Preferably, the meerschaum adsorbent of iron modification is that sepiolite fine powder and ferric chloride Solution reaction make, and solid-to-liquid ratio is 1: 5.
In the specific embodiment of the present invention, the temperature in step (d) is preferably 80-90 ℃, and churning time is preferably 20-30 minute.
In the specific embodiment of the present invention, the drying temperature in step (f) is preferred 70-80 ℃, is preferably 5-6 hour time of drying.
The Magnesium Stearate of low-heavy metal content of the present invention can satisfy the service requirements of pharmaceutical industries.The preparation technology of the Magnesium Stearate of low-heavy metal content of the present invention is simple, and is with low cost, and the product quality level that adopts the method to make is high, and can satisfy pharmaceutical industries to the demand of low-heavy metal content.The Magnesium Stearate content of the medicinal-grade magnesium stearate of employing present method preparation is greater than 99.8%, and heavy metal content is less than 10ppm, and heavy metal content is lower.
Description of drawings
Accompanying drawing consists of the part of this specification sheets, is used for further understanding the present invention.Accompanying drawing shows preferred embodiment, and is used for illustrating embodiments of the present invention together with specification sheets.
Fig. 1 is medicinal-grade magnesium stearate preparation method's of the present invention process flow sheet.
Embodiment
Hereinafter with reference to accompanying drawing, the technical process according to the preparation method of Magnesium Stearate of the present invention is specifically described, those skilled in the art should understand, following specific descriptions are for the ease of understanding the present invention, not being used for limiting protection scope of the present invention.
Be noted that the description and the following detailed description are all exemplary, are intended for the requested to provide further explanation of the invention.Unless otherwise, all technology used herein and scientific terminology have the identical meanings of usually understanding with the general technical staff of the technical field of the invention.
The present invention has mainly utilized the modified meerschaum sorbent material that the food grade Magnesium Stearate is processed, thereby greatly reduces the heavy metal content in the food grade Magnesium Stearate, obtains heavy metal content less than the medicinal-grade magnesium stearate of 10ppm.
Sepiolite (Sepiolite) is a kind of moisture magnesia silicate, and molecular formula is: Si
12Mg
8O
30(OH)
4(OH
2)
48H
2O is magnesium silicate a kind of fibre shape, that have chain structure, and its silicon-oxy tetrahedron is continuous, but in adjacent ribbons, the sensing of tetrahedron top is opposite, and each band is all staggered with a sipes that is parallel to fibre axis.This special structure makes it have larger specific surface area, data show, specific surface area can reach 800-900m
2/ g, wherein internal surface area is 500m
2/ g, outer surface area are 400m
2/ g.So large specific surface area and cell texture, make it have stronger adsorptive power.China's sepiolite reserves are abundant, and taste is higher, can satisfy the source demand of sorbent material of the present invention.
Studies show that, when sepiolite uses as sorbent material, carry out the adsorptive power of the modified meerschaum after activation treatment much larger than the natural sea afrodite.Particularly, the present inventor's research is learnt, iron trichloride (FeCl
3) the modifying function best results of solution, reason is as follows:
1, sepiolite is carried out sour modification: FeCl
3Belong to strong acid weak base salt, water-soluble rear Fe
3+Be hydrolyzed, make solution aobvious acid, the Cl in solution
-Form strong acid HCl, the H of HCl in water
+Can replace the Mg in the sepiolite skeleton
2+, the part micropore expands to central hole structure, has further increased the specific surface area of sepiolite, strengthens its adsorptive power.
2, Fe
3+Form Fe (OH) in solution
3Colloid is filtered and removes.
To sum up, the Mg between the silicon-oxy tetrahedron layer of sepiolite
2+Enter solution under being dissociated and remove Mg in modifying process
2+The space that stays can be partly by H
+Replace or the room.During as sorbent material, heavy metal ion just can be adsorbed or and H when modified meerschaum
+Exchange interaction occurs.Test shows, the sepiolite after the iron modification can reach more than 95% the metal ion clearance in solution.
Can find out, the preparation of modified meerschaum sorbent material is extremely important in embodiments of the present invention.At first preparation method and the flow process of modified meerschaum sorbent material are described therefore.The preparation of modified meerschaum sorbent material
(1) sepiolite is purified
Sepiolite original soil mining water is dissolved, the foreign material such as silt are removed in sedimentation, and with gauze, the suspending sundries foam on liquid level is removed, get upper strata suspension suction filtration, after the gained filter cake is placed in 105 ℃ of dry 24h of baking oven, grind to form the particle of 100 mesh sieves, then put into 105 ℃ of oven drying 12h, namely got the sepiolite fine powder.
(2) preparation of iron modified meerschaum sorbent material
Get the beaker that 3 parts of sepiolite fine powder 10g are placed in respectively 100mL, adding successively massfraction is 2.5%, 5.0%, 10% FeCl
3Solution 50mL, solid-to-liquid ratio is 1: 5, stirring reaction 30min places precipitation 24h, during stir 7-8 time.Discard supernatant liquid, lower sediment is transferred in funnel, filter, wash with water until do not contain Fe in water outlet
3+, Mg
2+Till.Take out, be placed in more than 150 ℃ of baking ovens cure 8h, after smashing, dry, pulverized 100 mesh sieves to pieces with ceramic alms bowl, namely make 2.5%, 5.0% and 10% iron modified meerschaum sorbent material, this iron modified meerschaum sorbent material is placed in the sealing bag of moisture eliminator standby.
The preparation of the high-purity forms of magnesium stearate of pharmaceutical grade low-heavy metal content
Fig. 1 is medicinal-grade magnesium stearate preparation method's of the present invention process flow sheet.Referring to Fig. 1, step is:
(a) the food grade Magnesium Stearate is joined in dissolving vessel, add dehydrated alcohol, stirring velocity with 100-150rpm at the temperature of 50-70 ℃ stirs 15-30 minute fully to dissolve, and wherein the blending ratio of Magnesium Stearate and dehydrated alcohol is 1: 10 (g/ml);
(b) add the meerschaum adsorbent vibration absorption 2-3h of 10-20g/L iron modification in the solution that obtains in step (a), filter;
(c) ethanol is reclaimed in filtrate underpressure distillation at 60-70 ℃ of temperature, collects product;
(d) product with gained joins in dissolving vessel, add purified water, stirring velocity with 100-150rpm at the temperature of 70-90 ℃ stirs 15-30 minute fully to wash, and wherein the blending ratio of Magnesium Stearate and purified water is 1: 8 (g/ml);
(e) filter, isolate solid substance, discard filtrate;
(f) with the material that separates in the baking oven of 70-90 ℃ dry 4-6 hour;
(g) crushing material with drying sieves, and the check packing is to obtain product.The Magnesium Stearate content of the medicinal-grade magnesium stearate of employing the method preparation is greater than 99.8%, and heavy metal content satisfies pharmaceutical industries to the requirement of the medicinal-grade magnesium stearate of heavy metal content less than 10ppm.
In the specific embodiment of the present invention, in step (b), add the amount of iron modified meerschaum sorbent material to be preferably the 1.5-5% of Magnesium Stearate mass ratio, be perhaps 15-18g/L, normal temperature vibration adsorption time is 2 hours.
In the specific embodiment of the present invention, the temperature in step (d) is preferably 80-90 ℃, and churning time is preferably 20-30 minute.
In the specific embodiment of the present invention, the drying temperature in step (f) is preferred 70-80 ℃, is preferably 5-6 hour time of drying.
The Magnesium Stearate of low-heavy metal content of the present invention can satisfy the service requirements of pharmaceutical industries.The preparation technology of the Magnesium Stearate of low-heavy metal content of the present invention is simple, and is with low cost.In addition, utilize the meerschaum adsorbent processing of iron modification to make cost low, processing speed is fast, and is easy to control, and Treatment technique for processing is relatively simple, and sorbent material is renewable.The product quality level that adopts the method to make is high, and can satisfy pharmaceutical industries to the demand of low-heavy metal content and sulphate content.The Magnesium Stearate content of the medicinal-grade magnesium stearate of employing present method preparation is greater than 99.8%, and heavy metal content is less than 10ppm, and preferred heavy metal content is less than 8ppm.
Hereinafter, further illustrate the present invention in connection with some embodiment.
The preparation method of embodiment 1 Magnesium Stearate
100g food grade Magnesium Stearate is joined in dissolving vessel, then add the 1000ml dehydrated alcohol in dissolving vessel, stirred 20 minutes with the stirring velocity of 120rpm, and be heated to 50 ℃ fully to dissolve; The iron modified meerschaum sorbent material that the solution that obtains is added 10g/L, vibration absorption 2h filters; Ethanol is reclaimed in filtrate underpressure distillation at 60 ℃ of temperature, collects product; The product of gained is joined in dissolving vessel, add purified water, the stirring velocity with 120rpm at the temperature of 75 ℃ stirs 20 minutes fully to wash, and wherein the blending ratio of Magnesium Stearate and purified water is 1: 8 (g/ml); Filter, isolate solid substance, discard filtrate; With the material that separates in the baking oven of 80 ℃ dry 4 hours; The crushing material of drying is sieved, and the check packing is to obtain product.Adopting the Magnesium Stearate content of the medicinal-grade magnesium stearate of the method preparation is 99.8%, and heavy metal content satisfies pharmaceutical industries to the requirement of the medicinal-grade magnesium stearate of heavy metal content less than 10ppm.
Accordingly, can obtain having the medicinal-grade magnesium stearate product of following characteristics: products obtained therefrom is that the light fine powder without grittiness of white, heavy metal content are less than 10ppm.
The contriver adopts the same step operation of embodiment 1, the operational condition parameter is optimized, find to adopt following listed condition substantially can implement the present invention, the Magnesium Stearate that adopts preferred condition to make has and the essentially identical effect of the product of embodiment 1.
Embodiment 2
200g food grade Magnesium Stearate is joined in dissolving vessel, then add the 2000ml dehydrated alcohol in dissolving vessel, stirred 30 minutes with the stirring velocity of 130rpm, and be heated to 60 ℃ fully to dissolve; The iron modified meerschaum sorbent material that the solution that obtains is added 20g/L, vibration absorption 3h filters; Ethanol is reclaimed in filtrate underpressure distillation at 70 ℃ of temperature, collects product; The product of gained is joined in dissolving vessel, add purified water, the stirring velocity with 150rpm at the temperature of 75 ℃ stirs 30 minutes fully to wash, and wherein the blending ratio of Magnesium Stearate and purified water is 1: 8 (g/ml); Filter, isolate solid substance, discard filtrate; With the material that separates in the baking oven of 85 ℃ dry 5 hours; The crushing material of drying is sieved, and the check packing is to obtain product.Adopting the Magnesium Stearate content of the medicinal-grade magnesium stearate of the method preparation is 99.87%, and heavy metal content is 5.1ppm, satisfies pharmaceutical industries to the requirement of the medicinal-grade magnesium stearate of heavy metal content.
Embodiment 3
150g food grade Magnesium Stearate is joined in dissolving vessel, then add the 1500ml dehydrated alcohol in dissolving vessel, stirred 30 minutes with the stirring velocity of 130rpm, and be heated to 55 ℃ fully to dissolve; The iron modified meerschaum sorbent material that the solution that obtains is added 15g/L, vibration absorption 2.5h filters; Ethanol is reclaimed in filtrate underpressure distillation at 65 ℃ of temperature, collects product; The product of gained is joined in dissolving vessel, add purified water, the stirring velocity with 130rpm at the temperature of 70 ℃ stirs 20 minutes fully to wash, and wherein the blending ratio of Magnesium Stearate and purified water is 1: 8 (g/ml); Filter, isolate solid substance, discard filtrate; With the material that separates in the baking oven of 70 ℃ dry 4.5 hours; The crushing material of drying is sieved, and the check packing is to obtain product.Adopting the Magnesium Stearate content of the medicinal-grade magnesium stearate of the method preparation is 99.81%, and heavy metal content is 4.0ppm, satisfies pharmaceutical industries to the requirement of the medicinal-grade magnesium stearate of heavy metal content.
Embodiment 4
120g food grade Magnesium Stearate is joined in dissolving vessel, then add the 1200ml dehydrated alcohol in dissolving vessel, stirred 25 minutes with the stirring velocity of 120rpm, and be heated to 65 ℃ fully to dissolve; The iron modified meerschaum sorbent material that the solution that obtains is added 18g/L, vibration absorption 2.8h filters; Ethanol is reclaimed in filtrate underpressure distillation at 65 ℃ of temperature, collects product; The product of gained is joined in dissolving vessel, add purified water, the stirring velocity with 100rpm at the temperature of 75 ℃ stirs 15 minutes fully to wash, and wherein the blending ratio of Magnesium Stearate and purified water is 1: 8 (g/ml); Filter, isolate solid substance, discard filtrate; With the material that separates in the baking oven of 90 ℃ dry 5.5 hours; The crushing material of drying is sieved, and the check packing is to obtain product.Adopting the Magnesium Stearate content of the medicinal-grade magnesium stearate of the method preparation is 99.85%, and heavy metal content is 2.4ppm, satisfies pharmaceutical industries to the requirement of the medicinal-grade magnesium stearate of heavy metal content.
Embodiment 5
50g food grade Magnesium Stearate is joined in dissolving vessel, then add the 500ml dehydrated alcohol in dissolving vessel, stirred 15 minutes with the stirring velocity of 100rpm, and be heated to 65 ℃ fully to dissolve; It is the iron modified meerschaum sorbent material of 1.5% (quality is 4.32g) that the solution that obtains is added mass ratio, and vibration absorption 2h filters; Ethanol is reclaimed in filtrate underpressure distillation at 60 ℃ of temperature, collects product; The product of gained is joined in dissolving vessel, add purified water, the stirring velocity with 110rpm at the temperature of 85 ℃ stirs 20 minutes fully to wash, and wherein the blending ratio of Magnesium Stearate and purified water is 1: 8 (g/ml); Filter, isolate solid substance, discard filtrate; With the material that separates in the baking oven of 75 ℃ dry 5 hours; The crushing material of drying is sieved, and the check packing is to obtain product.Adopting the Magnesium Stearate content of the medicinal-grade magnesium stearate of the method preparation is 99.90%, and heavy metal content is 2.7ppm, satisfies pharmaceutical industries to the requirement of the medicinal-grade magnesium stearate of heavy metal content.
Embodiment 6
80g food grade Magnesium Stearate is joined in dissolving vessel, then add the 800ml dehydrated alcohol in dissolving vessel, stirred 15 minutes with the stirring velocity of 120rpm, and be heated to 60 ℃ fully to dissolve; It is the iron modified meerschaum sorbent material of 3% (quality is 12.04g) that the solution that obtains is added mass ratio, and vibration absorption 2.2h filters; Ethanol is reclaimed in filtrate underpressure distillation at 60 ℃ of temperature, collects product; The product of gained is joined in dissolving vessel, add purified water, the stirring velocity with 120rpm at the temperature of 90 ℃ stirs 20 minutes fully to wash, and wherein the blending ratio of Magnesium Stearate and purified water is 1: 8 (g/ml); Filter, isolate solid substance, discard filtrate; With the material that separates in the baking oven of 88 ℃ dry 4 hours; The crushing material of drying is sieved, and the check packing is to obtain product.Adopting the Magnesium Stearate content of the medicinal-grade magnesium stearate of the method preparation is 99.84%, and heavy metal content is 3.4ppm, satisfies pharmaceutical industries to the requirement of the medicinal-grade magnesium stearate of heavy metal content.
Embodiment 7
160g food grade Magnesium Stearate is joined in dissolving vessel, then add the 1600ml dehydrated alcohol in dissolving vessel, stirred 20 minutes with the stirring velocity of 150rpm, and be heated to 70 ℃ fully to dissolve; It is the iron modified meerschaum sorbent material of 5% (quality is 42.7g) that the solution that obtains is added mass ratio, and vibration absorption 2.2h filters; Ethanol is reclaimed in filtrate underpressure distillation at 60 ℃ of temperature, collects product; The product of gained is joined in dissolving vessel, add purified water, the stirring velocity with 120rpm at the temperature of 80 ℃ stirs 20 minutes fully to wash, and wherein the blending ratio of Magnesium Stearate and purified water is 1: 8 (g/ml); Filter, isolate solid substance, discard filtrate; With the material that separates in the baking oven of 75 ℃ dry 6 hours; The crushing material of drying is sieved, and the check packing is to obtain product.Adopting the Magnesium Stearate content of the medicinal-grade magnesium stearate of the method preparation is 99.89%, and heavy metal content is 6.9ppm, satisfies pharmaceutical industries to the requirement of the medicinal-grade magnesium stearate of heavy metal content.
Comparative example 1
Utilize common process to prepare Magnesium Stearate, do not use iron modified meerschaum sorbent material to carry out the removing heavy metals ion.100g food grade Magnesium Stearate is joined in dissolving vessel, then add the 1000ml purified water in dissolving vessel, the stirring velocity with 120rpm in 20 minutes stirs, and is heated to 80 ℃ fully to wash; Filter, isolate solid substance, discard filtrate; With the material that separates in the baking oven of 80 ℃ dry 4 hours; The crushing material of drying is sieved, and the check packing is to obtain product.Adopting the Magnesium Stearate content of the medicinal-grade magnesium stearate of the method preparation is 99.0%, and heavy metal content is 25ppm.
The inspection after construction of food grade Magnesium Stearate and the Magnesium Stearate by method of the present invention preparation the results are shown in following table 1.
The inspection after construction result of the Magnesium Stearate of table 1 preparation
By the inspection after construction result of table 1 as can be known, muriate, vitriol, molysite and the heavy metal content of the Magnesium Stearate product of producing by method of the present invention are all lower, and heavy metal content can satisfy the service requirements of pharmaceutical industries less than 10ppm.
The assay that the heavy metal content of the Magnesium Stearate of embodiment 1-7 and comparative example 1 preparation is tested is shown in following table 2.
The heavy metal assay of the Magnesium Stearate of table 2 embodiment 1-7 and comparative example 1 preparation
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 | Embodiment 7 | Comparative example 1 | |
| Heavy metal content (ppm) | 3.6 | 5.1 | 4.0 | 2.4 | 2.7 | 3.4 | 6.9 | 25 |
As can be known from the results of Table 2, compare with the comparative example 1 that does not use iron modified meerschaum sorbent material to carry out heavy-metal ion removal, the heavy metal content of the Magnesium Stearate that the embodiment of the present invention 1-7 that uses iron modified meerschaum sorbent material to carry out removal of heavy metal ions makes is all less than 8ppm, degree of purification is high, can satisfy pharmaceutical industries to the requirement of the medicinal-grade magnesium stearate of heavy metal content.
In addition, method of the present invention raw material used is the Magnesium Stearate of food grade, and production process only relates to washing, filtration, drying, pulverize and sieve and make finished product, occur without chemical reaction, and mild condition, can not change the Magnesium Stearate structure.Therefore exempt to do the structural identification test.
Although described and illustrated the present invention by specific embodiment, should be appreciated that for a person skilled in the art, in the situation that do not deviate from the spirit and scope of the present invention, can carry out various modifications and be equal to replacement the present invention.Therefore, the invention is not restricted to the specific embodiment described in this article.More properly, protection scope of the present invention is limited by the accompanying claims.
Claims (7)
1. method for preparing medicinal-grade magnesium stearate wherein, said method comprising the steps of:
(a) the food grade Magnesium Stearate is joined in dissolving vessel, add dehydrated alcohol, stirring velocity with 100-150rpm at the temperature of 50-70 ℃ stirs 15-30 minute fully to dissolve, and wherein the blending ratio of Magnesium Stearate and dehydrated alcohol is 1: 10g/ml;
(b) add the meerschaum adsorbent vibration absorption 2-3h of 10-20g/L iron modification in the solution that obtains in step (a), filter;
(c) ethanol is reclaimed in filtrate underpressure distillation at 60-70 ℃ of temperature, collect product;
(d) product with gained joins in dissolving vessel, adds purified water, and the stirring velocity with 100-150rpm at the temperature of 70-90 ℃ stirs 15-30 minute fully to wash, and wherein the blending ratio of Magnesium Stearate and purified water is 1: 8g/ml;
(e) filter, isolate solid substance, discard filtrate;
(f) with the material that separates in the baking oven of 70-90 ℃ dry 4-6 hour;
(g) crushing material with drying sieves, and the check packing obtains product.
2. method according to claim 1, wherein, the stirring velocity in step (a) is 100-120rpm.
3. method according to claim 1, wherein, add the amount of iron modified meerschaum sorbent material to be preferably 15-18g/L in step (b).
4. method according to claim 1, is characterized in that, is that sepiolite fine powder and ferric chloride Solution reaction make at the meerschaum adsorbent of the described iron modification of step (b), and solid-to-liquid ratio is 1: 5.
5. method according to claim 1, wherein, the temperature in step (d) is preferably 80-90 ℃, and churning time is preferably 20-30 minute.
6. method according to claim 1, wherein, the drying temperature in step (f) is 70-80 ℃, be 5-6 hour time of drying.
7. method according to claim 1 wherein, in step (b), adds in the described food grade Magnesium Stearate to account for the meerschaum adsorbent that its mass ratio is the described iron modification of 1.5-5%.
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Non-Patent Citations (3)
| Title |
|---|
| 吴茂英等.硬脂酸镁合成新工艺.《化工科技》.2000,(第06期), * |
| 国家药典委员会编.硬脂酸镁.《中国药典》.化学工业出版社,2000版第二部,2000,第833页. * |
| 秦玉楠.药用硬脂酸镁制备工艺及其改进.《中国现代应用药学》.1991,(第03期), * |
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