CN109608309A - A kind of refining methd of glycerol - Google Patents
A kind of refining methd of glycerol Download PDFInfo
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- CN109608309A CN109608309A CN201910064161.XA CN201910064161A CN109608309A CN 109608309 A CN109608309 A CN 109608309A CN 201910064161 A CN201910064161 A CN 201910064161A CN 109608309 A CN109608309 A CN 109608309A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
- B01J20/041—Oxides or hydroxides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28016—Particle form
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28078—Pore diameter
- B01J20/28083—Pore diameter being in the range 2-50 nm, i.e. mesopores
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
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- Chemical Kinetics & Catalysis (AREA)
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- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
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Abstract
The invention discloses a kind of refining methds of glycerol.A kind of refining methd of glycerol disclosed by the invention comprising following steps: the technical grade glycerol by water content lower than 0.5% carries out S1, and S2 step or S2, S1 step can obtain refined glycerine；Wherein, glycerol content is not less than 95% in the technical grade glycerol, and the percentage is mass percent；The S1 is to be adsorbed by calcium oxide-chitin fiber mesoporous nano particle ball adsorbent, is filtered；The S2 is to be decolourized by decolorising agent, is filtered.The refining methd is easy to operate, and adsorbent is simple and easy to get, does not generate impurity substantially, environmentally protective, reduces production cost, meets the needs of industrialized production.Through primary purification, glycerol purity is up to 99.5% or more, metal, inorganic salts, and organic impurities etc. is all satisfied pharmaceutical grade requirement.
Description
Technical field
The present invention relates to a kind of refining methds of glycerol.
Background technique
Glycerol is also referred to as glycerine, is a kind of widely used chemicals, in coating, papermaking, weaving, food, medicine, cigarette
The industrial circles such as grass, cosmetics are widely used, and are mainly used as excipient, moisturizer, smooth agent, sweetener, thickener, antifreeze
Agent, emulsifier etc. can be divided into pharmaceutical grade and technical grade according to the purity of glycerol height.The traditional source of technical grade glycerol is main
Be grease hydrolysis by-product, amylofermentation and produce diesel oil by-product, the crude product glycerol being synthetically prepared by filtering, concentration,
The purification of the processes such as chemical addition agent, distillation obtains technical grade glycerol.However, pharmaceutical grade qualities of glycerin norm controlling is stringent, chlorine
The concentration requirement of the permissions such as compound, sulfate, molysite, readily carbonizable substance is very low, therefore industry glycerol has to pass through further purification
Just it can be used for medicinal.The refining methd of traditional pharmaceutical grade glycerol includes two methods, rectification method and ion-exchange.But it is smart
The medicine company grade glycerol for evaporating method preparation easily forms glyceraldehyde, generates strange taste；Vapo(u)rizing temperature is high, is easy to produce polymer and energy damage
Consume high disadvantage.The glycerol quality of ion-exchange production is high, but the processing cost of resin is high, and waste water yield is big, salt
Substance corrodes the disadvantages of production pipeline.
Summary of the invention
The technical problem to be solved by the present invention is in order to overcome in the prior art rectification method purification of glycerol be also easy to produce polymerization
Object, energy loss are high；Ion exchange methods glycerol is costly, waste water yield is big, corrosive equipment defect, and provides
A kind of refining methd of glycerol.The refining methd is easy to operate, and adsorbent is simple and easy to get, does not generate impurity substantially, environmentally protective,
High financial profit, the glycerol product being refining to obtain can reach medicinal grade standard.
The present invention mainly solves above-mentioned technical problem by the following technical programs.
The present invention provides a kind of refining methds of glycerol comprising following steps:
Technical grade glycerol by water content lower than 0.5% carries out S1, and S2 step or S2, S1 step can obtain refined glycerine；
Wherein, glycerol content is not less than 95% in the technical grade glycerol, and the percentage is mass percent；
The S1 is to be adsorbed by calcium oxide-chitin fiber mesoporous nano particle ball adsorbent, is filtered；
The S2 is to be decolourized by decolorising agent, is filtered.
The technical grade glycerol source is this field usual sources, preferably vegetable oil hydrolysising by-product, animal oil
One of hydrolysising by-product and production biological diesel oil byproduct are a variety of.Plant described in the vegetable oil hydrolysising by-product
Object oil is preferably one of rapeseed oil, soybean oil, peanut oil, corn oil, cottonseed oil, palm oil and olive oil or a variety of.Institute
Animal oil described in the animal oil hydrolysising by-product stated is preferably one of fish oil, lard, butter and sheep oil or a variety of.
In a specific embodiment of the invention, in the refining methd of the glycerol, in S1 the and S2 step
Preceding can also further comprise that the technical grade glycerol by water content more than or equal to 0.5% is dehydrated to obtain the water content and is lower than
0.5% technical grade glycerol.
The temperature of the dehydration is that this field is conventional, preferably 90~100 DEG C.The dewatering time is this field
It is conventional, preferably 1~2 hour.
In S1, the calcium oxide-chitin fiber mesoporous nano particle ball adsorbent and the technical grade glycerol
Mass ratio is that this field is conventional, preferably 0.01~0.05.The temperature of the absorption is that this field is conventional, preferably 30
~50 DEG C.The time of the absorption is that this field is conventional, preferably 10~60 minutes.The temperature of the filtering is ability
Domain is conventional, and preferably 30~50 DEG C.Filter used in the filtering is that this field is conventional, preferably bag type filtering
Device.The filter cloth mesh number of the bag filter is preferably 200 mesh~400 mesh.
The calcium oxide-chitin fiber mesoporous nano particle ball adsorbent can be by such adsorbent of this field routine
Preparation method is prepared, for example, chitin fiber is added in dilute calcium hydroxide aqueous solution, is sufficiently stirred, and it is extra to remove
Free acid, the chitin fiber after filtering to alkalize.By chitin fiber after the food-grade calcium hydroxide of 1kg and 5kg alkalization
It is added in 5kg distilled water, is sufficiently stirred to form paste.Calcium hydroxide-chitin fiber particle is formed using Spheroidgranulator
Ball.Particle ball is dried into 5h at 150 DEG C, removes moisture, forms calcium oxide-chitin fiber mesoporous nano particle ball.
The calcium oxide-chitin fiber mesoporous nano particle spherolite diameter can be 1.9~2.1mm.
In S2, the decolorising agent is that this field is conventional, preferably active carbon and/or atlapulgite.The activity
Charcoal is preferably medicinal carbon.The atlapulgite is preferably medical active carclazyte.The decolorising agent and described
The mass ratio of technical grade glycerol is that this field is conventional, preferably 0.05%~0.25%.The temperature of the decoloration is ability
Domain is conventional, and preferably 50~70 DEG C.The time of the decoloration is that this field is conventional, preferably 1~4 hour.Described
The temperature of filtering is that this field is conventional, preferably 50~70 DEG C.Filter used in the filtering is that this field is conventional, compared with
It is filtered goodly for plate filter.The filter cloth mesh number of the plate filter is preferably 400 mesh~800 mesh.
In a preferred embodiment of the present invention, in S2, the filtering can carry out in the presence of filter aid.It is described
Filter aid be that this field is conventional, preferably diatomite and/or gypsum.The diatomite is preferably medicinal diatomite.
The gypsum is preferably gypsum of pharmaceutic.The mass ratio of the filter aid and the technical grade glycerol is that this field is normal
Rule, preferably 0.05%~0.25%.
In a preferred embodiment of the present invention, in S2, when the filtering carries out in the presence of filter aid, S2
It can be filtered to be decolourized by the compound adsorbent of decolorising agent and filter aid.The compound suction of the decolorising agent and filter aid
Attached dose is that this field is conventional with the mass ratio of the technical grade glycerol, preferably 0.1%~0.5%.The compound suction
Decolorising agent and filter aid in attached dose is same as above.
The compound adsorbent of the decolorising agent and filter aid can be by the preparation method system of such adsorbent routine of this field
It is standby to obtain, such as the gypsum of pharmaceutic or medicinal diatomite of the medicinal carbon of 1kg or medical active carclazyte and 1kg are subjected to physics
Mixing, the dry activation 2h at 120 DEG C.Obtain the compound adsorbent of decolorising agent and filter aid.
The present invention also provides calcium oxide-chitin fiber mesoporous nano particle ball adsorbent as adsorbent in glycerol essence
Application in system.
Readily carbonizable substance in technical grade glycerol；Diethylene glycol (DEG), ethylene glycol and other impurities；Residue on ignition；Content of beary metal ammonium
The indexs such as salt meet 2015 editions the 4th regulations to pharmaceutical grade glycerol of Chinese Pharmacopoeia.
Without prejudice to the field on the basis of common sense, above-mentioned each optimum condition, can any combination to get the present invention it is each preferably
Example.
The reagents and materials used in the present invention are commercially available.
The positive effect of the present invention is that: operation of the present invention is simple, and adsorbent is simple and easy to get, does not generate substantially miscellaneous
Matter, it is environmentally protective, production cost is reduced, the needs of industrialized production are met.Through primary purification, glycerol purity is reachable
99.5% or more, metal, inorganic salts, organic impurities etc. be all satisfied pharmaceutical grade requirement.
Specific embodiment
The present invention is further illustrated below by the mode of embodiment, but does not therefore limit the present invention to the reality
It applies among a range.In the following examples, the experimental methods for specific conditions are not specified, according to conventional methods and conditions, or according to quotient
The selection of product specification.
Embodiment 1
The preparation of calcium oxide-chitin fiber mesoporous nano particle ball adsorbent: dilute hydroxide is added in chitin fiber
It in calcium aqueous solution, is sufficiently stirred, removes extra free acid, the chitin fiber after filtering to alkalize.By the food-grade hydrogen of 1kg
Chitin fiber is added in 5kg distilled water after calcium oxide and 5kg alkalization, is sufficiently stirred to form paste.Use marumerizer
Machine forms 2mm calcium hydroxide-chitin fiber particle ball.Particle ball is dried into 5h at 150 DEG C, removes moisture, is formed
Calcium oxide-chitin fiber mesoporous nano particle ball.
Embodiment 2
The preparation of the compound adsorbent of decolorising agent and filter aid: by the medicinal carbon of 1kg or medical active carclazyte and 1kg
Gypsum of pharmaceutic or medicinal diatomite carry out physical mixed, the dry activation 2h at 120 DEG C.Decolorising agent and filter aid it is compound
Adsorbent.
Embodiment 3
The technical grade glycerol of 3000kg water content 4~5% is added in 5000L reaction kettle, is heated to 90 DEG C, keeps the temperature 2h.
50 DEG C are cooled to, calcium oxide-chitin fiber mesoporous nano particle ball adsorbent that 30kg is made by embodiment 1 is added, absorption
50min is filtered with 200 mesh bag filters.3kg active carbon as made from embodiment 2/composite diatomite is added into filtrate to inhale
2h is adsorbed at attached dose, 60 DEG C, is filtered using 400 mesh plate filters, obtains pharmaceutical grade glycerol.
Embodiment 4
The technical grade glycerol of 3000kg water content 4~5% is added in 5000L reaction kettle, is heated to 100 DEG C, keeps the temperature 1h.
35 DEG C are cooled to, calcium oxide-chitin fiber mesoporous nano particle ball adsorbent that 60kg is made by embodiment 1 is added, absorption
40min is filtered with 400 mesh bag filters.6kg atlapulgite/composite diatomite as made from embodiment 2 is added into filtrate
Adsorbent adsorbs 3h at 50 DEG C, is filtered using 800 mesh plate filters, obtains pharmaceutical grade glycerol.
Embodiment 5
The technical grade glycerol of 3000kg water content 4~5% is added in 5000L reaction kettle, is heated to 95 DEG C, heat preservation
1.5h.30 DEG C are cooled to, calcium oxide-chitin fiber mesoporous nano particle ball adsorbent that 90kg is made by embodiment 1 is added,
20min is adsorbed, is filtered with 200 mesh bag filters.It is multiple that 3kg atlapulgite/gypsum as made from embodiment 2 is added into filtrate
Adsorbent is closed, adsorbs 1h at 70 DEG C, is filtered using 800 mesh plate filters, obtains pharmaceutical grade glycerol.
Embodiment 6
The technical grade glycerol of 3000kg water content 4~5% is added in 5000L reaction kettle, is heated to 90 DEG C, keeps the temperature 2h.
40 DEG C are cooled to, calcium oxide-chitin fiber mesoporous nano particle ball adsorbent that 120kg is made by embodiment 1 is added, absorption
20min is filtered with 200 mesh bag filters.9kg active carbon as made from embodiment 2/gypsum composite adsorption is added into filtrate
Agent adsorbs 4h at 60 DEG C, is filtered using 400 mesh plate filters, obtains pharmaceutical grade glycerol.
Embodiment 7
The technical grade glycerol of 3000kg water content 4~5% is added in 5000L reaction kettle, is heated to 100 DEG C, keeps the temperature 2h.
45 DEG C are cooled to, calcium oxide-chitin fiber mesoporous nano particle ball adsorbent that 150kg is made by embodiment 1 is added, absorption
10min is filtered with 200 mesh bag filters.12kg active carbon/composite diatomite as made from embodiment 2 is added into filtrate
Adsorbent adsorbs 1h at 60 DEG C, is filtered using 800 mesh plate filters, obtains pharmaceutical grade glycerol.
Embodiment 8
The technical grade glycerol of 3000kg water content 4~5% is added in 5000L reaction kettle, is heated to 90 DEG C, keeps the temperature 1h.
40 DEG C are cooled to, calcium oxide-chitin fiber mesoporous nano particle ball adsorbent that 60kg is made by embodiment 1 is added, absorption
30min is filtered with 200 mesh bag filters.15kg compound suction of active carbon/gypsum as made from embodiment 2 is added into filtrate
1h is adsorbed at attached dose, 50 DEG C, is filtered using 800 mesh plate filters, obtains pharmaceutical grade glycerol.
Comparative example 1
The technical grade glycerol of 3000kg water content 4~5% is added in 5000L reaction kettle, is warming up to 50 DEG C, 30kg is added
Calcium oxide-chitin fiber mesoporous nano particle ball adsorbent adsorbs 50min, is filtered with 200 mesh bag filters.To filtrate
Middle addition 3kg active carbon/composite absorption agent of diatomite adsorbs 2h at 60 DEG C, is filtered using 400 mesh plate filters.Finally will
Filtered glycerol is heated to 90 DEG C, keeps the temperature 2h, obtains pharmaceutical grade glycerol.
Effect example 1
By chloride, sulfate, aldehyde and reducing substances, fatty acid in the glycerol of 2015 editions the 4th records of Chinese Pharmacopoeia
The pharmaceutical grade being prepared with the detection method measurement embodiment 1-6 of lipid, the detection method of molysite and glycerol content is sweet
Oil, measurement result is as shown in table 1,
The pharmaceutical grade glycerol physical and chemical parameter that 1 embodiment 1-6 of table is prepared
Connect table
| Fatty acid and lipid | Molysite | Moisture | Content (anhydride meter) | |
| Technical grade glycerol | Consume titrating solution > 4.0ml | 0.001% | 4.8% | 95%-96.5% |
| Embodiment 1 | Consume titrating solution 1.2ml | < 0.0002% | 0.1% | 99.5% |
| Embodiment 2 | Consume titrating solution 1.0ml | < 0.0002% | 0.1% | 99.6% |
| Embodiment 3 | Consume titrating solution 1.1ml | < 0.0002% | 0.1% | 99.5% |
| Embodiment 4 | Consume titrating solution 1.2ml | < 0.0002% | 0.1% | 99.7% |
| Embodiment 5 | Consume titrating solution 1.0ml | < 0.0002% | 0.1% | 99.5% |
| Embodiment 6 | Consume titrating solution 1.1ml | < 0.0002% | 0.1% | 99.6% |
| Comparative example 1 | Consume titrating solution 2.8ml | < 0.0002% | 0.4% | 97.2% |
It is provided in Chinese Pharmacopoeia 2015 editions the 4th, chloride must not exceed 0.0015% in glycerol；Sulfate must not surpass
Cross 0.002%；Fatty acid and the sodium hydroxide titration liquid of lipid consumption must not exceed 4.0ml；Molysite must not exceed 0.0002%.
Claims (10)
1. a kind of refining methd of glycerol, which is characterized in that itself the following steps are included:
Technical grade glycerol by water content lower than 0.5% carries out S1, and S2 step or S2, S1 step can obtain refined glycerine；Its
In, glycerol content is not less than 95% in the technical grade glycerol, and the percentage is mass percent；
The S1 is to be adsorbed by calcium oxide-chitin fiber mesoporous nano particle ball adsorbent, is filtered；
The S2 is to be decolourized by decolorising agent, is filtered.
2. the refining methd of glycerol as described in claim 1, which is characterized in that wherein, in S2, the filtering is in filter aid
In the presence of carry out.
3. the refining methd of glycerol as claimed in claim 2, which is characterized in that wherein, S2 is to pass through decolorising agent and filter aid
Compound adsorbent decolourize, filter.
4. the refining methd of glycerol as claimed in any one of claims 1 to 3, which is characterized in that wherein,
The technical grade glycerol be vegetable oil hydrolysising by-product, animal oil hydrolysising by-product and production biological diesel oil byproduct in
It is one or more；Vegetable oil described in the vegetable oil hydrolysising by-product be preferably rapeseed oil, soybean oil, peanut oil,
One of corn oil, cottonseed oil, palm oil and olive oil are a variety of；Animal described in the animal oil hydrolysising by-product
Oil is preferably one of fish oil, lard, butter and sheep oil or a variety of；
And/or the calcium oxide-chitin fiber mesoporous nano particle ball adsorbent and technical grade glycerol quality
Than being 0.01~0.05；
And/or in S1, the temperature of the absorption is 30~50 DEG C；
And/or in S1, the time of the absorption is 10~60 minutes；
And/or in S1, the temperature of the filtering is 30~50 DEG C；
And/or in S1, filter used in the filtering is bag filter；The filter cloth mesh number of the bag filter
Preferably 200 mesh~400 mesh；
And/or in S2, the decolorising agent is active carbon and/or atlapulgite；The active carbon is preferably medical active
Charcoal；The atlapulgite is preferably medical active carclazyte；
And/or in S2, the temperature of the decoloration is 50~70 DEG C；
And/or in S2, the time of the decoloration is 1~4 hour；
And/or in S2, the temperature of the filtering is 50~70 DEG C；
And/or in S2, filter used in the filtering is plate filter filtering；The filter cloth of the plate filter
Mesh number is preferably 400 mesh~800 mesh.
5. the refining methd of glycerol as claimed in claim 1 or 2, which is characterized in that wherein,
In S2, the mass ratio of the decolorising agent and the technical grade glycerol is 0.05%~0.25%.
6. the refining methd of glycerol as claimed in claim 2, which is characterized in that wherein,
The filter aid is diatomite and/or gypsum；The diatomite is preferably medicinal diatomite；The gypsum compared with
It goodly is gypsum of pharmaceutic；
And/or the mass ratio of the filter aid and the technical grade glycerol is 0.05%~0.25%.
7. the refining methd of glycerol as claimed in claim 3, which is characterized in that wherein,
The filter aid is diatomite and/or gypsum；The diatomite is preferably medicinal diatomite；The gypsum compared with
It goodly is gypsum of pharmaceutic；
And/or the compound adsorbent of the decolorising agent and filter aid is 0.1% with the mass ratio of the technical grade glycerol
~0.5%.
8. the refining methd of glycerol as described in any one of claims 1 to 7, which is characterized in that in S1 the and S2 step
Before still further comprise and be dehydrated water content more than or equal to 0.5% technical grade glycerol, obtain the water content and be lower than
0.5% technical grade glycerol.
9. the refining methd of glycerol as claimed in claim 8, which is characterized in that wherein,
The temperature of the dehydration is 90~100 DEG C；
And/or the time of the dehydration is 1~2 hour.
10. a kind of calcium oxide-application of the chitin fiber mesoporous nano particle ball adsorbent as adsorbent in purification of glycerin.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110372809A (en) * | 2019-07-09 | 2019-10-25 | 浙江海洋大学 | One one-step preparation method of shrimp shell of modified chitin fiber and its application |
| WO2024081659A1 (en) * | 2022-10-13 | 2024-04-18 | Archer Daniels Midland Company | Purification of glycerin as excipient in parenteral pharmaceutical applications |
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