CN108047190A - Utilize the method for D-ALPHA-Hydroxypropionic acid production D- lactides - Google Patents
Utilize the method for D-ALPHA-Hydroxypropionic acid production D- lactides Download PDFInfo
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- C07D319/00—Heterocyclic compounds containing six-membered rings having two oxygen atoms as the only ring hetero atoms
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Abstract
The present invention discloses a kind of method using D production of lactic acid D lactides, includes the following steps：(1) raw material prepares：The D lactic acid solutions of 35 60wt%, the optical purity of D lactic acid are greater than or equal to 99.5%；(2) oligomerization is dehydrated, obtains D lactic acid oligomers；(3) depolymerization of D lactic acid oligomers prepares D lactides.The method that the present invention utilizes D production of lactic acid D lactides, can obtain the relatively narrow lactic acid oligomer of molecular weight distribution, and very high as the yield of D lactides made from raw material and optical purity using it.
Description
Technical field
The present invention relates to lactic acid deep process technology FIELD OF THE INVENTIONThes.More particularly, to a kind of D- third is produced using D-ALPHA-Hydroxypropionic acid
The method of lactide.
Background technology
Polylactic acid is a kind of function admirable, has biocompatibility and the polymer of biodegradability, is mainly used for
Degradable package material and medicine microsphere carrier, antiadhesion barrier, biological duct, orthopaedics fixture, bone surgery device, people
In terms of the medical materials such as work bone.
By monomer lactic acid prepare polylactic acid during, be that lactic acid oligomer is generated by monomer lactic acid first, then again by
Lactic acid oligomer direct polycondensation prepares polylactic acid or prepares lactide and then lactide ring-opening polymerisation generation by lactic acid oligomer
Polylactic acid.Wherein, the higher polylactic acid of molecular weight can be prepared using lactide ring-opening polymerisation, thus as current first choice.
Lact-acid oligomer acts not only as preparing the original of polylactic acid, is also used as medicine intermediate, Chinese patent text
It offers CN1498237A and discloses a kind of preparation method of lactic acid oligomer, be raw material using lactide, can selectively make
Standby chain and cyclic lactic acid oligosaccharide mixture.The disadvantages of this method is：(1) it is raw material that must use lactide, but in industry
The most cheap by raw material of lactic acid monomer in metaplasia production, it is higher directly to prepare the cost of lactide by lactic acid monomer, can only make
By the use of the by-product lactide in melt polycondensation as raw material；(2) the tetrahydrofuran equal solvent used is toxic, is not suitable for industrializing
Using.
The content of the invention
It is an object of the present invention to provide a kind of utilization D-ALPHA-Hydroxypropionic acid monomer generation D-ALPHA-Hydroxypropionic acid oligomer and prepare D- third
The method of lactide.
In order to achieve the above objectives, the present invention uses following technical proposals：
A kind of method using D-ALPHA-Hydroxypropionic acid production D- lactides includes the following steps：
(1) raw material prepares：The D-ALPHA-Hydroxypropionic acid solution of 40-60wt%, the optical purity of D-ALPHA-Hydroxypropionic acid are greater than or equal to 99.5%；
(2) oligomerization is dehydrated, obtains D-ALPHA-Hydroxypropionic acid oligomer；
(3) depolymerization of D-ALPHA-Hydroxypropionic acid oligomer prepares D- lactides.
In step (2), acetone is added in into D-ALPHA-Hydroxypropionic acid solution for the above-mentioned method using D-ALPHA-Hydroxypropionic acid production D- lactides
The volume ratio of acetoacetic ester, ethyl pyruvate and D-ALPHA-Hydroxypropionic acid solution is 0.5-1:1；Simultaneously into mixed solution add in cobalt oxide and
Two-acthiol-J vanadyl is as catalyst, stirring；The usage amount of cobalt oxide is the 0.02%- of D-ALPHA-Hydroxypropionic acid quality
0.04%, two-acthiol-J vanadyl usage amount is the 0.04%-0.08% of D-ALPHA-Hydroxypropionic acid quality；Reaction time is 3h-6h,
Reaction temperature is 5-30 DEG C.
The above-mentioned method using D-ALPHA-Hydroxypropionic acid production D- lactides, in step (2)：
During initial reaction：The addition mass ratio of cobalt oxide and two-acthiol-J vanadyl is 1:1.5, cobalt oxide exists
Addition during initial reaction is the 1/2 of the total addition of cobalt oxide；Reaction temperature goes over two points from initial reaction to the reaction time
One of be always maintained at 5 DEG C -10 DEG C；
When reaction time goes over half：Remaining two-acthiol-J vanadyl is all added in reaction kettle；
Past reaction temperature autoreaction time half to the past in reaction time 3/4ths is always maintained at 15 DEG C -20 DEG C；
When past in reaction time 3/4ths：Remaining cobalt oxide is all added in reaction kettle；Reaction temperature autoreaction
Past time 3/4ths terminates to be always maintained at 25-30 DEG C to reaction.
The above-mentioned method using D-ALPHA-Hydroxypropionic acid production D- lactides, in step (2), the system of two-acthiol-J vanadyl
Preparation Method is：Acthiol-J and vanadic sulfate are mixed, react 3-5h, obtain purple at room temperature in boric acid solution
Solid；The amount of acthiol-J and vanadic sulfate substance ratio 5:1, concentration of the acthiol-J in boric acid solution is
0.1-5mol/L。
The above-mentioned method using D-ALPHA-Hydroxypropionic acid production D- lactides, in step (2), after reaction, filtering stands and divides
Layer isolates organic phase, washes organic phase；Organic phase vacuum distillation after washing is removed into solvent, obtains white solid.
The above-mentioned method using D-ALPHA-Hydroxypropionic acid production D- lactides, in step (3), the D-ALPHA-Hydroxypropionic acid that will be obtained in step (2)
Oligomer input lactide prepares kettle, is warming up to 145-160 DEG C, melts D-ALPHA-Hydroxypropionic acid oligomer；Synthesis D- lactides are used
Catalyst be the mixture of nickel oxide and glycine hydroxy acid molybdenum, nickel oxide usage amount is D-ALPHA-Hydroxypropionic acid oligomerization amount of substance
0.01%-0.03%, glycine hydroxy acid molybdenum usage amount are the 0.03%-0.09%, reaction time 3- of D- lactic acid oligomer quality
5h, reaction pressure 0.01 × 105Pa-0.1 ×105Pa；
During initial reaction：The addition mass ratio of nickel oxide and glycine hydroxy acid molybdenum is 1:2, nickel oxide is in initial reaction
When addition be the total addition of nickel oxide 1/3；
When past in reaction time 1/3rd：Remaining nickel oxide is all added in lactide and prepares kettle；
When past in reaction time 2/3rds：Remaining glycine hydroxy acid molybdenum is all added in lactide and prepares kettle.
The above-mentioned method using D-ALPHA-Hydroxypropionic acid production D- lactides, in step (3), the preparation method of glycine hydroxy acid molybdenum
For：Sodium molybdate and glycine hydroxy acid are mixed at room temperature in methanol solution, react 2-3h, it is glycine to obtain solid
Hydroxy acid molybdenum；The amount of glycine hydroxy acid and sodium molybdate substance ratio 4:1, concentration of the sodium molybdate in methanol solution is 0.1-2mol/L.
It is above-mentioned using D-ALPHA-Hydroxypropionic acid production D- lactides method, in step (3), lactide prepare kettle top by every
Hot channel and condensation collecting tank fluid communication, the D- lactides of generation are in condensation collecting tank crystallisation by cooling.
Beneficial effects of the present invention are as follows：
(1) using D-ALPHA-Hydroxypropionic acid monomer cheap and easy to get in actual industrial production as raw material, it has been worth molecular weight distribution relatively narrow
D-ALPHA-Hydroxypropionic acid oligomer, reaction condition is mild and easily controllable, D-ALPHA-Hydroxypropionic acid oligomer high income, suitable for industrialized production.
(2) lactide is prepared by raw material of D-ALPHA-Hydroxypropionic acid oligomer, the yield and purity of lactide are all very high, and improve
Reaction pressure, it is energy saving in the industrial production.
Specific embodiment
In order to illustrate more clearly of the present invention, with reference to preferred embodiment, the present invention is described further.Ability
Field technique personnel should be appreciated that following specifically described content is illustrative and be not restrictive, this should not be limited with this
The protection domain of invention.
Embodiment 1
A kind of method using D-ALPHA-Hydroxypropionic acid production D- lactides includes the following steps：
(1) raw material prepares：The D-ALPHA-Hydroxypropionic acid solution of the 40wt% of applicant's production, the optical purity of D-ALPHA-Hydroxypropionic acid are more than or wait
In 99.5%；
(2) oligomerization is dehydrated, obtains D-ALPHA-Hydroxypropionic acid oligomer；
Mixed solution is obtained after ethyl pyruvate stirring is added in into D-ALPHA-Hydroxypropionic acid solution, ethyl pyruvate and D- lactic acid are molten
The volume ratio of liquid is 1:1；
Cobalt oxide and two-acthiol-J vanadyl are added in into mixed solution in accordance with the following steps simultaneously as catalysis
Agent：
During initial reaction (0h)：The addition mass ratio of cobalt oxide and two-acthiol-J vanadyl is 1:1.5, oxidation
Addition of the cobalt in initial reaction is the 1/2 of the total addition of cobalt oxide；Reaction temperature is gone over from initial reaction to the reaction time
Half is always maintained at 5 DEG C；Stirring；
Reaction time goes over when half (2h)：Remaining two-acthiol-J vanadyl is all added in reaction
Kettle；Past reaction temperature autoreaction time half to the past in reaction time 3/4ths is always maintained at 15 DEG C；Stirring；
When past in reaction time 3/4ths (3h)：Remaining cobalt oxide is all added in reaction kettle；Reaction temperature is certainly
Past in reaction time 3/4ths terminates to be always maintained at 25 DEG C to reaction；Stirring.
The usage amount of cobalt oxide is the 0.02% of D-ALPHA-Hydroxypropionic acid quality, and two-acthiol-J vanadyl usage amount is D-ALPHA-Hydroxypropionic acid
The 0.04% of quality；The preparation method of two-acthiol-J vanadyl is：Acthiol-J and vanadic sulfate are molten in boric acid
Liquid is mixed at room temperature, reacts 3-5h, obtains violet solid；The amount of acthiol-J and vanadic sulfate substance ratio 5:
1, concentration of the acthiol-J in boric acid solution is 2mol/L.
After reaction, filter, stratification, isolate organic phase, wash organic phase；Organic after washing is subtracted each other
Solvent is distilled off in pressure, obtains white solid, and fast atom bombardment mass spectroscopy is carried out to gained white solid and nuclear-magnetism detects, white is solid
Body is the D-ALPHA-Hydroxypropionic acid oligomer of 6-19 aggressiveness, and the yield of D-ALPHA-Hydroxypropionic acid oligomer is 95%.
(3) depolymerization of D-ALPHA-Hydroxypropionic acid oligomer prepares D- lactides；
The D-ALPHA-Hydroxypropionic acid oligomer obtained in step (2) input lactide is prepared into kettle, lactide prepare kettle top by every
Hot channel and condensation collecting tank fluid communication；Lactide prepares kettle and is warming up to 145 DEG C, melts D-ALPHA-Hydroxypropionic acid oligomer；
The mixture that nickel oxide and glycine hydroxy acid molybdenum are added in kettle is prepared as catalysis to lactide in accordance with the following steps
(nickel oxide usage amount is the 0.01% of D-ALPHA-Hydroxypropionic acid oligomerization amount of substance, and glycine hydroxy acid molybdenum usage amount is D-ALPHA-Hydroxypropionic acid oligomerization substance for agent
The 0.03% of amount, reaction time 3h, reaction pressure 0.01 × 105Pa)：
During initial reaction (0h)：The addition mass ratio of nickel oxide and glycine hydroxy acid molybdenum is 1:2, nickel oxide is initial
Addition during reaction is the 1/3 of the total addition of nickel oxide；
When past in reaction time 1/3rd (1h)：Remaining nickel oxide is all added in lactide and prepares kettle；
When past in reaction time 2/3rds (2h)：Remaining glycine hydroxy acid molybdenum is all added in lactide to prepare
Kettle.
The preparation method of glycine hydroxy acid molybdenum is：In methanol solution, mixing at room temperature is stirred for sodium molybdate and glycine hydroxy acid
It mixes, reacts 3h, it is glycine hydroxy acid molybdenum to obtain solid；The amount of glycine hydroxy acid and sodium molybdate substance ratio 4:1, sodium molybdate exists
Concentration in methanol solution is 2mol/L.
The D- lactides of generation are 97.1% in condensation collecting tank crystallisation by cooling, D- lactides yield, and optical purity is
99.9%.
Embodiment 2
A kind of method using D-ALPHA-Hydroxypropionic acid production D- lactides includes the following steps：
(1) raw material prepares：The D-ALPHA-Hydroxypropionic acid solution of the 60wt% of applicant's production, the optical purity of D-ALPHA-Hydroxypropionic acid are more than or wait
In 99.5%；
(2) oligomerization is dehydrated, obtains D-ALPHA-Hydroxypropionic acid oligomer；
Mixed solution is obtained after ethyl pyruvate stirring is added in into D-ALPHA-Hydroxypropionic acid solution, ethyl pyruvate and D- lactic acid are molten
The volume ratio of liquid is 1:1；Cobalt oxide and two-acthiol-J vanadyl are added in into mixed solution as catalyst；Cobalt oxide
Usage amount be D-ALPHA-Hydroxypropionic acid quality 0.04%, two-acthiol-J vanadyl usage amount be D-ALPHA-Hydroxypropionic acid quality 0.08%,
3h is stirred to react at room temperature；The preparation method of two-acthiol-J vanadyl is：Acthiol-J and vanadic sulfate are in boron
Acid solution is mixed at room temperature, reacts 3-5h, obtains violet solid；The amount of acthiol-J and vanadic sulfate substance
Than 5:1, concentration of the acthiol-J in boric acid solution is 0.5mol/L.
After reaction, filter, stratification, isolate organic phase, wash organic phase；Organic after washing is subtracted each other
Solvent is distilled off in pressure, obtains white solid, and fast atom bombardment mass spectroscopy is carried out to gained white solid and nuclear-magnetism detects, white is solid
Body is except the D-ALPHA-Hydroxypropionic acid oligomer containing 6-19 aggressiveness, the D-ALPHA-Hydroxypropionic acid oligomer also containing 30-50 aggressiveness；D-ALPHA-Hydroxypropionic acid oligomer
Yield be 82%.
(3) depolymerization of D-ALPHA-Hydroxypropionic acid oligomer prepares D- lactides；
The D-ALPHA-Hydroxypropionic acid oligomer obtained in step (2) input lactide is prepared into kettle, lactide prepare kettle top by every
Hot channel and condensation collecting tank fluid communication；Lactide prepares kettle and is warming up to 150 DEG C, melts D-ALPHA-Hydroxypropionic acid oligomer；It is handed over to third
Prepared by ester adds in the mixture of nickel oxide and glycine hydroxy acid molybdenum as catalyst in kettle：
During initial reaction (0h)：The addition mass ratio of nickel oxide and glycine hydroxy acid molybdenum is 1:2, nickel oxide is initial
Addition during reaction is the 1/3 of the total addition of nickel oxide；
When past in reaction time 1/3rd (1h)：Remaining glycine hydroxy acid molybdenum is all added in lactide to prepare
Kettle；
When past in reaction time 3/4ths (2h)：Remaining nickel oxide is all added in lactide and prepares kettle.
Nickel oxide usage amount is the 0.03% of D-ALPHA-Hydroxypropionic acid oligomerization amount of substance, and glycine hydroxy acid molybdenum usage amount is few for D- lactic acid
The 0.09% of polymers quality, reaction time 3h, reaction pressure 0.1 × 105Pa；The preparation method of glycine hydroxy acid molybdenum is：Molybdic acid
Sodium and glycine hydroxy acid are mixed at room temperature in methanol solution, react 3h, it is glycine hydroxy acid molybdenum to obtain solid；It is sweet
The amount of propylhomoserin hydroxy acid and sodium molybdate substance ratio 4:1, concentration of the sodium molybdate in methanol solution is 1mol/L.
The D- lactides of generation are 86.5% in condensation collecting tank crystallisation by cooling, D- lactides yield, and optical purity is
99.9%.
Embodiment 3
A kind of method using D-ALPHA-Hydroxypropionic acid production D- lactides includes the following steps：
(1) raw material prepares：The D-ALPHA-Hydroxypropionic acid solution of the 50wt% of applicant's production, the optical purity of D-ALPHA-Hydroxypropionic acid are more than or wait
In 99.5%；
(2) oligomerization is dehydrated, obtains D-ALPHA-Hydroxypropionic acid oligomer；
Mixed solution is obtained after ethyl pyruvate stirring is added in into D-ALPHA-Hydroxypropionic acid solution, ethyl pyruvate and D- lactic acid are molten
The volume ratio of liquid is 1:1；
Cobalt oxide and two-acthiol-J vanadyl are added in into mixed solution in accordance with the following steps simultaneously as catalysis
Agent：
During initial reaction (0h)：The addition mass ratio of cobalt oxide and two-acthiol-J vanadyl is 1:1.5, oxidation
Addition of the cobalt in initial reaction is the 1/2 of the total addition of cobalt oxide；Reaction temperature is gone over from initial reaction to the reaction time
Half is always maintained at 10 DEG C；Stirring；
Reaction time goes over when half (3h)：Remaining cobalt oxide is all added in reaction kettle；Reaction temperature is certainly
Past in reaction time half to the past in reaction time 3/4ths is always maintained at 15 DEG C；Stirring；
When past in reaction time 3/4ths (4.5h)：Remaining two-acthiol-J vanadyl is all added in anti-
Answer kettle；Past reaction temperature autoreaction time 3/4ths terminates to be always maintained at 30 DEG C to reaction；Stirring.
The usage amount of cobalt oxide is the 0.03% of D-ALPHA-Hydroxypropionic acid quality, and two-acthiol-J vanadyl usage amount is D-ALPHA-Hydroxypropionic acid
The 0.06% of quality；The preparation method of two-acthiol-J vanadyl is：Acthiol-J and vanadic sulfate are molten in boric acid
Liquid is mixed at room temperature, reacts 3-5h, obtains violet solid；The amount of acthiol-J and vanadic sulfate substance ratio 5:
1, concentration of the acthiol-J in boric acid solution is 1mol/L.
After reaction, filter, stratification, isolate organic phase, wash organic phase；Organic after washing is subtracted each other
Solvent is distilled off in pressure, obtains white solid, and fast atom bombardment mass spectroscopy is carried out to gained white solid and nuclear-magnetism detects, white is solid
Body is the D-ALPHA-Hydroxypropionic acid oligomer of 6-40 aggressiveness, and the yield of D-ALPHA-Hydroxypropionic acid oligomer is 90%.
(3) depolymerization of D-ALPHA-Hydroxypropionic acid oligomer prepares D- lactides；
The D-ALPHA-Hydroxypropionic acid oligomer obtained in step (2) input lactide is prepared into kettle, lactide prepare kettle top by every
Hot channel and condensation collecting tank fluid communication；Lactide prepares kettle and is warming up to 160 DEG C, melts D-ALPHA-Hydroxypropionic acid oligomer；It is handed over to third
Prepared by ester adds in the mixture of nickel oxide and glycine hydroxy acid molybdenum as catalyst in kettle；Nickel oxide usage amount is few for D-ALPHA-Hydroxypropionic acid
The 0.02% of polymers quality, glycine hydroxy acid molybdenum usage amount are 0.06%, reaction time 5h of D-ALPHA-Hydroxypropionic acid oligomerization amount of substance, instead
Answer pressure 0.05 × 105Pa；The preparation method of glycine hydroxy acid molybdenum is：Sodium molybdate and glycine hydroxy acid are in methanol solution, room
Temperature is lower to be mixed, and reacts 3h, it is glycine hydroxy acid molybdenum to obtain solid；The amount of glycine hydroxy acid and sodium molybdate substance ratio 4:
1, concentration of the sodium molybdate in methanol solution is 1mol/L.
The D- lactides of generation are 73.1% in condensation collecting tank crystallisation by cooling, D- lactides yield, and optical purity is
99.9%.
Obviously, the above embodiment of the present invention is only intended to clearly illustrate example of the present invention, and is not pair
The restriction of embodiments of the present invention for those of ordinary skill in the art, may be used also on the basis of the above description
To make other variations or changes in different ways, all embodiments can not be exhaustive here, it is every to belong to this hair
The obvious changes or variations that bright technical solution is extended out is still in the row of protection scope of the present invention.
Claims (8)
1. utilize the method for D-ALPHA-Hydroxypropionic acid production D- lactides, which is characterized in that include the following steps：
(1) raw material prepares：The D-ALPHA-Hydroxypropionic acid solution of 35-60wt%, the optical purity of D-ALPHA-Hydroxypropionic acid are greater than or equal to 99.5%；
(2) oligomerization is dehydrated, obtains D-ALPHA-Hydroxypropionic acid oligomer；
(3) depolymerization of D-ALPHA-Hydroxypropionic acid oligomer prepares D- lactides.
2. the method according to claim 1 using D-ALPHA-Hydroxypropionic acid production D- lactides, which is characterized in that in step (2),
Add in ethyl pyruvate into D-ALPHA-Hydroxypropionic acid solution, the volume ratio of ethyl pyruvate and D-ALPHA-Hydroxypropionic acid solution is 0.5-1:1；Simultaneously to mixed
It closes and cobalt oxide and two-acthiol-J vanadyl is added in solution as catalyst, stirring；The usage amount of cobalt oxide is D-ALPHA-Hydroxypropionic acid
The 0.02%-0.04% of quality, two-acthiol-J vanadyl usage amount are the 0.04%-0.08% of D-ALPHA-Hydroxypropionic acid quality；Reaction
Time is 3h-6h, and reaction temperature is 5-30 DEG C.
3. the method according to claim 2 using D-ALPHA-Hydroxypropionic acid production D- lactides, which is characterized in that in step (2)：
During initial reaction：The addition mass ratio of cobalt oxide and two-acthiol-J vanadyl is 1:1.5, cobalt oxide is initial
Addition during reaction is the 1/2 of the total addition of cobalt oxide；Reaction temperature goes over half from initial reaction to the reaction time
It is always maintained at 5 DEG C -10 DEG C；
When reaction time goes over half：Remaining two-acthiol-J vanadyl is all added in reaction kettle；Reaction temperature
Degree autoreaction time past half to the past in reaction time 3/4ths is always maintained at 15 DEG C -20 DEG C；
When past in reaction time 3/4ths：Remaining cobalt oxide is all added in reaction kettle；The reaction temperature autoreaction time
Past 3/4ths terminates to be always maintained at 25-30 DEG C to reaction.
4. the method according to claim 3 using D-ALPHA-Hydroxypropionic acid production D- lactides, which is characterized in that in step (2),
The preparation method of two-acthiol-J vanadyl is：Acthiol-J and vanadic sulfate are mixed at room temperature in boric acid solution
Stirring reacts 3-5h, obtains violet solid；The amount of acthiol-J and vanadic sulfate substance ratio 5:1, acthiol-J exists
Concentration in boric acid solution is 0.1-5mol/L.
5. the method according to claim 4 using D-ALPHA-Hydroxypropionic acid production D- lactides, which is characterized in that in step (2),
After reaction, filter, stratification, isolate organic phase, wash organic phase；Organic phase after washing is evaporated under reduced pressure and is removed
Solvent obtains white solid.
6. the method according to claim 1 using D-ALPHA-Hydroxypropionic acid production D- lactides, which is characterized in that in step (3),
The D-ALPHA-Hydroxypropionic acid oligomer obtained in step (2) input lactide is prepared into kettle, 145-160 DEG C is warming up to, makes D-ALPHA-Hydroxypropionic acid oligomer
Fusing；Synthesize catalyst used in D- lactides is for nickel oxide and the mixture of glycine hydroxy acid molybdenum, nickel oxide usage amount
The 0.01%-0.03% of D-ALPHA-Hydroxypropionic acid oligomerization amount of substance, glycine hydroxy acid molybdenum usage amount are the 0.03%- of D-ALPHA-Hydroxypropionic acid oligomerization amount of substance
0.09%, reaction time 3-5h, reaction pressure 0.01 × 105Pa-0.1×105Pa；
During initial reaction：The addition mass ratio of nickel oxide and glycine hydroxy acid molybdenum is 1:2, nickel oxide adding in initial reaction
Enter 1/3 that amount is the total addition of nickel oxide；
When past in reaction time 1/3rd：Remaining nickel oxide is all added in lactide and prepares kettle；
When past in reaction time 2/3rds：Remaining glycine hydroxy acid molybdenum is all added in lactide and prepares kettle.
7. the method according to claim 6 using D-ALPHA-Hydroxypropionic acid production D- lactides, which is characterized in that in step (3),
The preparation method of glycine hydroxy acid molybdenum is：Sodium molybdate and glycine hydroxy acid are mixed at room temperature in methanol solution, react 2-
3h, it is glycine hydroxy acid molybdenum to obtain solid；The amount of glycine hydroxy acid and sodium molybdate substance ratio 4:1, sodium molybdate is in methanol solution
In concentration be 0.1-2mol/L.
8. the method according to claim 7 using D-ALPHA-Hydroxypropionic acid production D- lactides, which is characterized in that in step (3),
Lactide prepares kettle top by heat-insulating pipeline and condensation collecting tank fluid communication, and the D- lactides of generation are cold in condensation collecting tank
But crystallize.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101649042A (en) * | 2009-07-08 | 2010-02-17 | 安徽丰原发酵技术工程研究有限公司 | Preparation method of high molecular poly lactic acid |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101649042A (en) * | 2009-07-08 | 2010-02-17 | 安徽丰原发酵技术工程研究有限公司 | Preparation method of high molecular poly lactic acid |
Non-Patent Citations (1)
| Title |
|---|
| FARKAS E等: "Oxygen versus nitrogen co-ordination in complexes of MoⅥ and hydroxamate derivatives of a-amino acids：equilibrium，structural and theoretical studies", 《J．CHEM．SOC．》 * |
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