CN101704719B - Method for preparing medical-grade propylene glycol - Google Patents
Method for preparing medical-grade propylene glycol Download PDFInfo
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- CN101704719B CN101704719B CN 200910249992 CN200910249992A CN101704719B CN 101704719 B CN101704719 B CN 101704719B CN 200910249992 CN200910249992 CN 200910249992 CN 200910249992 A CN200910249992 A CN 200910249992A CN 101704719 B CN101704719 B CN 101704719B
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Abstract
The invention provides a method for preparing medical-grade propylene glycol. The method uses industrial-grade propylene glycol as a raw material, and comprises the following steps: (a) adding zeolite-chitosan spherical granules into the industrial-grade propylene glycol with the mass ratio of 1-2:100, oscillating the mixture for 1 to 3 minutes every 2 to 5 minutes, co-adsorbing the mixture for 15 to 40 minutes, and filtering the mixture; (b) adding 0.5 to 1 percent of medical active carbon with the mass ratio with the industrial-grade propylene glycol into the filtered solution, heating the solution to between 75 and 85 DEG C, preserving the heat and standing the solution for 20 to 40 minutes; and (c) filtering the solution, heating the filtered solution to between 90 and 100 DEG C, performing evaporation and dehydration, and stopping dehydration till the solution is not turbid to obtain the medical-grade propylene glycol. The method for preparing the medical-grade propylene glycol has the advantages of simple preparation process and low cost; and the medical-grade propylene glycol prepared by the method has high quality level, and can meet the requirements of the medicament, food and cosmetic industries on propylene glycol.
Description
Technical field
The present invention relates to a kind of method for preparing medical-grade propylene glycol, particularly, the present invention relates to a kind of method for preparing medical-grade propylene glycol take the technical grade propylene glycol as raw material.
Background technology
Medical-grade propylene glycol is the thick liquid of achromaticity and clarification; Odorless, it is little sweet to distinguish the flavor of; Have draw moist; Can be miscible arbitrarily with water, ethanol or trichloromethane; Stable under the normal temperature, at high temperature easily generate propionic aldehyde, lactic acid, acetone, acetic acid.The Application Areas of medical-grade propylene glycol is wider, and it can be applicable in the fields such as medicine, food, makeup.In field of medicaments, medical-grade propylene glycol can be used as solvent, extraction solvent and the sanitas of injection and non-injection pharmaceutical preparation, and it can dissolve various materials such as reflunomide, phenol, sulfa drugs, barbiturate(s), vitamin A and D, most of alkaloid and many narcotics; Also can be used as fungistat, the effect of its mould fungus inhibition is similar to glycerine; Be commonly used in addition the softening agent of aqueous film coating's material.In foods and cosmetics industry, medical-grade propylene glycol can be used as the carrier of emulsifying agent, the solvent of spices, because its non-volatility helps the fragrance that keeps stable, thereby effect is better than ethanol.The quality control standards (QCS) of medical-grade propylene glycol is: muriate≤0.007%, vitriol≤0.006%, moisture≤0.2%, residue on ignition≤0.007%, heavy metal≤5ppm.
The technical grade propylene glycol is mainly used to produce coating and unsaturated polyester resin, also is the raw material of softening agent, tensio-active agent, emulsifying agent and emulsion splitter.At present, the production method of technical grade propylene glycol mainly contains five kinds: propylene oxide direct hydration method, the indirect hydration method of propylene oxide, propylene Direct Catalytic Oxidation method, bioid engineering method, methylcarbonate propylene glycol co-production method etc.
The technical grade propylene glycol is compared medical-grade propylene glycol, foreign matter content, especially heavy metal, sulfide content are too high, to human body certain toxicity may be arranged, therefore technical grade propylene glycol and be not suitable for medicine, food, cosmetic field, need to carry out to it processing such as removal of impurities purification, to obtain medical-grade propylene glycol.
Summary of the invention
The present invention aims to provide a kind of method for preparing medical-grade propylene glycol in order to address the above problem, and particularly, the present invention aims to provide a kind of method for preparing medical-grade propylene glycol take the technical grade propylene glycol as raw material.
According to the present invention, a kind of method for preparing medical-grade propylene glycol is provided, the method mainly comprises following step take the technical grade propylene glycol as raw material:
(a) adding in the technical grade propylene glycol with its mass ratio is the zeolite-chitosan sphere particle of 1-2%, every vibration in 2-5 minute 1-3 minute, co-adsorption 15-40 minute, filters.
(b) mass ratio that adds in the filtrate with the technical grade propylene glycol is the medicinal carbon of 0.5%-1%, is warming up to 75-85 ℃, and insulation was left standstill 20-40 minute;
(c) mentioned solution is filtered, filtrate is heated to 90-100 ℃ of dehydration by evaporation, until stop dehydration during without muddiness, obtain medical-grade propylene glycol.
In a kind of embodiment of the present invention, in step (a), the mass ratio of the zeolite of adding-chitosan sphere particle and technical grade propylene glycol is 1.55%.
In a kind of embodiment of the present invention, in step (a), every vibration in 2 minutes 1 minute, co-adsorption 20 minutes.
In a kind of embodiment of the present invention, in step (b), after insulation is left standstill 20-40 minute, solution was stirred 60-120 minute under 20 ℃.
In a kind of embodiment of the present invention, in step (b), the consumption of medicinal carbon is, with the mass ratio of described technical grade propylene glycol be 0.5%.
In a kind of embodiment of the present invention, in step (b), be warming up to 80 ℃, insulation was left standstill about 30 minutes.
In a kind of embodiment of the present invention, in step (c), described filtrate is heated to 100 ℃ carries out dehydration by evaporation.
The preparation technology of medical-grade propylene glycol of the present invention is simple, required with low cost; Adopt the product quality level of the medical-grade propylene glycol that the method makes high, can satisfy medicine, food, cosmetic industry to the demand of propylene glycol.
Description of drawings
Fig. 1 shows according to the present invention the schema for the preparation of the method for medical-grade propylene glycol.
Embodiment
It is raw material that the present invention adopts the technical grade propylene glycol, through some objectionable impurities in Physical Processing removal and the minimizing industrial raw material, the final medical-grade propylene glycol that obtains to be used for food, medicine, cosmetic field.Technical grade propylene glycol heavy metal content is too high, does not meet the medical grade standard, uses method of the present invention and can obtain all standard compliant products of outward appearance, proterties, foreign matter content.
The method for preparing medical-grade propylene glycol of the present invention mainly may further comprise the steps:
(a) adding in the technical grade propylene glycol with its mass ratio is the zeolite-chitosan sphere particle of 1-2%, every vibration in 2-5 minute 1-3 minute, co-adsorption 15-40 minute, filters.
(b) mass ratio that adds in the filtrate with the technical grade propylene glycol is the medicinal carbon of 0.5%-1%, is warming up to 75-85 ℃, and insulation was left standstill 20-40 minute;
(c) mentioned solution is filtered, filtrate is heated to 90-100 ℃ of dehydration by evaporation, until stop dehydration during without muddiness, obtain medical-grade propylene glycol.
In above-mentioned steps (a), preferably add mass ratio with the technical grade propylene glycol in the technical grade propylene glycol and be 1.55% zeolite-chitosan sphere particle, and every vibration in 2 minutes 1 minute, co-adsorption 20 minutes, filter.
In above-mentioned steps (b), in the technical grade propylene glycol, adding medicinal carbon and after 75-85 ℃ of insulation left standstill 20-40 minute, preferably solution being descended cold stirrings 60-120 minute at 20 ℃, make the charcoal absorption effect complete.The inventor is surprised to find that, in the presence of gac, with propylene glycol cold stirring 60-120 minute under the temperature about 20 ℃, played good effect.
In the method for the present invention for the preparation of medical-grade propylene glycol, the yield that the consumption of medicinal carbon, the propylene glycol that should obtain to purify meet medical standard and acquisition medical-grade propylene glycol is unlikely excessively low as purpose.In the present invention, the consumption of medicinal carbon is chosen as, with the mass ratio of used technical grade propylene glycol be 0.5-1%, be preferably 0.5%.
In sum, characteristics of the present invention are, adopt respectively zeolite-chitosan sphere particle, gac as sorbent material the technical grade propylene glycol to be carried out double adsorption-edulcoration, can significantly improve the refining effect of technical grade propylene glycol; And the consumption of gac carried out preferably, so that can remove preferably impurity, can avoid again the loss of too much propylene glycol; The present invention has increased the step of 20 ℃ of cold stirrings in the process of adsorbing with gac in addition, can make the absorption of gac more thorough.
Hereinafter enumerate exemplary embodiment of the present invention and comparative example, more clearly to describe the present invention, do not limit the scope of the invention but should not be understood as.
The preparation of zeolite-chitosan sphere particle
Be that the hydrochloric acid of 80 purpose natural zeolites and 1mol/L mixes according to weight ratio and soaked 24 hours at 1: 10 with granularity.Remove by filter the impurity such as organism, with distilled water natural zeolite is washed till neutrality again, dry for standby.Get chitosan 5g, in the acetic acid solution of adding 4%, fully stirring is dissolved chitosan fully.Add the 120g zeolite of above-mentioned dry for standby and fully stirring, the furnishing pasty state makes it abundant infiltration.Use extruding granulator to make the zeolite of particle diameter 1.0mm-chitosan sphere particle, dry after 100 ℃ of lower oven dry 2 hours, to be used for that the technical grade propylene glycol is adsorbed purification.
Embodiment 1 (1.55% zeolite-chitosan sphere particle, 0.5% gac)
1000g technical grade propylene glycol is added in the flask of 1500mL, the zeolite of adding 15.5g-chitosan sphere particle every vibration in 2 minutes 1 minute, adsorbed 20 minutes, filtered.Add 5g (0.5%) gac in filtrate, 80 ℃ are incubated 30 minutes; Then use Büchner funnel (400 order filter cloth) to filter; At last filtrate is heated to 100 ℃ of dehydration by evaporation 30 minutes, obtains product 978.5g.
Embodiment 2 (1.55% zeolite-chitosan sphere particle, 1% gac)
1000g technical grade propylene glycol is added in the flask of 1500mL, the zeolite of adding 15.5g-chitosan sphere particle every vibration in 2 minutes 1 minute, adsorbed 20 minutes, filtered.Add 10g (1%) gac in filtrate, 80 ℃ are incubated 30 minutes; Then use Büchner funnel (400 order filter cloth) to filter; At last filtrate is heated to 100 ℃ of dehydration by evaporation 30 minutes, obtains product 951.0g.
Embodiment 3 (1.55% zeolite-chitosan sphere particle, 0.5% gac, cold stirring)
1000g technical grade propylene glycol is added in the flask of 1500mL, the zeolite of adding 15.5g-chitosan sphere particle every vibration in 2 minutes 1 minute, adsorbed 20 minutes, filtered.Add 5g (0.5%) gac in filtrate, 80 ℃ were incubated 30 minutes, 20 ℃ of lower cold stirrings 100 minutes; Then use Büchner funnel (400 order filter cloth) to filter; At last filtrate is heated to 100 ℃ of dehydration by evaporation 30 minutes, obtains product 968.8g.
Comparative example (does not use zeolite-chitosan sphere particle; Concentration of activated carbon is 0.2%)
1000g technical grade propylene glycol is added in the flask of 1500mL, be warming up to 80 ℃, add 2g (0.2%) gac, 80 ℃ are incubated 30 minutes; Then use Büchner funnel (400 order filter cloth) to filter; At last filtrate is heated to 100 ℃ of dehydration by evaporation 30 minutes, obtains product 982.6g.
Product to embodiment 1-3 and comparative example is tested, the method for inspection as detailed below, assay is referring to table 1.
The method of inspection of medical-grade propylene glycol and inspecting standard
Acidity: get product 10.0ml, after adding the cold water 50ml dissolving of newly boiling, add 3 of bromothymol blue indicating liquids, it is aobvious blue to be titrated to solution with sodium hydroxide titrating solution (0.01mol/L), consume volume and be not more than 0.50ml and namely meet the medical-grade propylene glycol standard;
Muriate: get product 1.0ml, according to the method for inspection of two appendix VIIIA of Chinese Pharmacopoeia nineteen ninety-five version, the contrast liquor ratio made from standard sodium chloride solution 7.0ml must not denseer (0.007%), for meeting the medical-grade propylene glycol standard;
Vitriol: get product 5.0ml, according to the method for inspection of two appendix VIIIB of Chinese Pharmacopoeia nineteen ninety-five version, the contrast liquor ratio made from standard potassium sulfate solution 3.0ml must not denseer (0.006%), for meeting the medical-grade propylene glycol standard;
Oxidizing substance: get product 5.0ml, put in the iodine flask, add potassiumiodide test solution 1.5ml and dilute sulphuric acid 2ml, close plug, in the dark placed 15 minutes, and added starch indicating liquid 2ml, as aobvious blue, be titrated to blue the disappearance with Sulfothiorine titrating solution (0.005mol/L), the consumption volume is no more than 0.2ml and namely meets pharmaceutical grade propylene glycol standard;
Moisture: it is an amount of to get product, and (two appendix VIII of Chinese Pharmacopoeia nineteen ninety-five version M first method A) measures according to aquametry, and moisture must not surpass 0.2%, for meeting the medical-grade propylene glycol standard;
Residue on ignition: get product 50g, be heated to burning, namely stopped heating makes spontaneous firing to doing, and in 700～800 ℃ of ignition to constant weight, leaves over residue and must not surpass 3.5mg for meeting the medical-grade propylene glycol standard;
Heavy metal: get product 4.0ml, add water 19ml and acetate buffer (pH3.5) 2ml, mixing according to the check of two appendix VIII of Chinese Pharmacopoeia nineteen ninety-five version H first method, contains heavy metal and must not surpass 5/1000000ths (5ppm) for meeting the medical-grade propylene glycol standard.
The calculating of yield: yield=final product quality/1000 * 100%
The assay of the product of table 1 couple embodiment 1-3, comparative example
| Project | The medical grade standard | Comparative example | Embodiment 1 | Embodiment 2 | Embodiment 3 |
| Proterties | Colourless, clarification thick liquid | Colourless, clarification thick liquid | Colourless, clarification thick liquid | Colourless, clarification thick liquid | Colourless, clarification thick liquid |
| Acidity | Should meet inspecting standard | Meet inspecting standard | Meet inspecting standard | Meet inspecting standard | Meet inspecting standard |
| Muriate | ≤0.007％ | 0.007％ | 0.004％ | 0.003％ | 0.003％ |
| Vitriol | ≤0.006％ | 0.007％ | 0.003％ | 0.002％ | 0.002％ |
| Oxidizing substance | Should meet inspecting standard | Meet inspecting standard | Meet inspecting standard | Meet inspecting standard | Meet inspecting standard |
| Moisture | ≤0.2％ | 0.1％ | 0.1％ | 0.1％ | 0.1％ |
| Residue on ignition | ≤3.5mg | 3.3mg | 3.0mg | 2.5mg | 2.3mg |
| Heavy metal | ≤5ppm | 15ppm | 3ppm | 2ppm | 1.5ppm |
| Yield | - | 98.26％ | 97.85％ | 95.10％ | 96.88％ |
Interpretation of result
As shown in Table 1, although comparative example can obtain the product (982.6g) of maximum, yield is the highest, because heavy metal content exceeds standard, and does not meet the standard of medical-grade propylene glycol; Embodiment 1-3 all can obtain standard compliant medical-grade propylene glycol.Use zeolite-chitosan sphere particle and concentration are 0.5% gac (embodiment 1), can be guaranteeing that product meets under the prerequisite of medical grade standard, so that yield is the highest but by contrast; And to use zeolite-chitosan sphere particle and concentration be 0.5% gac and carry out cold stirring (embodiment 3) at 20 ℃, can obtain the less medical-grade propylene glycol of foreign matter content with higher yield.
In sum, the method according to this invention can be take the technical grade propylene glycol as raw material, through the steps such as zeolite-chitosan sphere particle and charcoal absorption removal of impurities, filtration, thermal dehydration, the final propylene glycol that obtains to meet the medical grade standard.
Claims (7)
1. method for preparing medical-grade propylene glycol, described method may further comprise the steps take the technical grade propylene glycol as raw material:
(a) adding in the technical grade propylene glycol with the mass ratio of described technical grade propylene glycol is the zeolite-chitosan sphere particle of 1-2%, every vibration in 2-5 minute 1-3 minute, co-adsorption 15-40 minute, filters;
(b) mass ratio that adds in the filtrate with described technical grade propylene glycol is the medicinal carbon of 0.5%-1%, is warming up to 75-85 ℃, and insulation was left standstill 20-40 minute;
(c) adding of step (b) being processed has the filtrate of medicinal carbon to filter, the filtrate that obtains is heated to 90-100 ℃ of dehydration by evaporation, until stop dehydration during without muddiness, obtains medical-grade propylene glycol.
2. method according to claim 1 is characterized in that, in step (a), adding in the described technical grade propylene glycol with its mass ratio is 1.55% described zeolite-chitosan sphere particle.
3. method according to claim 1 is characterized in that, in step (a), every vibration in 2 minutes 1 minute, co-adsorption 20 minutes.
4. method according to claim 1 is characterized in that, in step (b), after insulation is left standstill 20-40 minute, adding is had the filtrate of medicinal carbon 20 ℃ of lower stirrings 60-120 minute.
5. method according to claim 1 is characterized in that, in step (b), the consumption of described medicinal carbon is, with the mass ratio of described technical grade propylene glycol be 0.5%.
6. method according to claim 1 is characterized in that, in step (b), is warming up to 80 ℃, and insulation was left standstill 30 minutes.
7. method according to claim 1 is characterized in that, in step (c), described filtrate is heated to 100 ℃ carries out dehydration by evaporation.
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| CN 200910249992 CN101704719B (en) | 2009-12-08 | 2009-12-08 | Method for preparing medical-grade propylene glycol |
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| CN105924331B (en) * | 2016-04-28 | 2017-09-22 | 湖南尔康制药股份有限公司 | A kind of process for purification of propane diols |
| CN109608309A (en) * | 2019-01-23 | 2019-04-12 | 湖北葛店人福药用辅料有限责任公司 | A kind of refining methd of glycerol |
| CN115974651B (en) * | 2023-01-04 | 2024-04-09 | 山东德普新材料科技有限公司 | Method for preparing medical propylene glycol from propylene glycol prepared by transesterification method |
| CN116462573A (en) * | 2023-04-26 | 2023-07-21 | 德元堂(上海)健康科技发展有限公司 | Preparation method of pharmaceutical propylene glycol |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5076896A (en) * | 1988-06-13 | 1991-12-31 | Henkel Kommanditgesellschaft Auf Aktien | Process for the separation of propylene glycol from fatty alcohols |
| CN1318521A (en) * | 2001-04-24 | 2001-10-24 | 赵金星 | Preparation of water purifying agent |
| KR20010094573A (en) * | 2000-03-31 | 2001-11-01 | 김동석 | Manufacturing method of crab shell - biosorbent for the removal of heavy metal ion from aquous solution |
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- 2009-12-08 CN CN 200910249992 patent/CN101704719B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5076896A (en) * | 1988-06-13 | 1991-12-31 | Henkel Kommanditgesellschaft Auf Aktien | Process for the separation of propylene glycol from fatty alcohols |
| KR20010094573A (en) * | 2000-03-31 | 2001-11-01 | 김동석 | Manufacturing method of crab shell - biosorbent for the removal of heavy metal ion from aquous solution |
| CN1318521A (en) * | 2001-04-24 | 2001-10-24 | 赵金星 | Preparation of water purifying agent |
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