CN103897070B - A kind of take ionic liquid as the preparation method of the hydroxyethylamyle 130/0.4 of reaction medium - Google Patents
A kind of take ionic liquid as the preparation method of the hydroxyethylamyle 130/0.4 of reaction medium Download PDFInfo
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Abstract
The invention belongs to amylopectin chemical derivative technical field, being specifically related to a kind of take ionic liquid as the preparation method of the hydroxyethylamyle 130/0.4 of reaction medium, comprises the following steps: amylopectin is joined ionic liquid and heating and dissolves by a; B adds salt acid degradation; C adds etherifying agent hydroxyethylation; D adds alcohol compound precipitation; E obtains product after decolouring, ultrafiltration, drying.The present invention adopts ionic liquid to substitute water as reaction medium, the hydrolysis of starch and etherification reaction is carried out in homogeneous system, when overcoming using water as inhomogeneous reaction medium, reactant consumption amount is large, the shortcomings such as by product is many, and product substitution value is difficult to control, product performance homogeneity difference.In addition, ionic liquid as green reaction medium have tasteless, pollution-free, nonflammable, easily and product separation, easily reclaim, can the premium properties such as iterative cycles use, make that synthesis technique is safer, environmental protection.
Description
Technical field
The invention belongs to amylopectin chemical derivative technical field, being specifically related to a kind of take ionic liquid as the preparation method of the hydroxyethylamyle 130/0.4 of reaction medium.
Background technology
Hydroxyethylamyle is the one of current most popular artificial plasm's surrogate, and it is the polymer composite formed through hydroxyethylation by the glucose ring of amylopectin.Its chemical structure is similar with glycogen to the polysaccharide in body, side effect is less than other plasma substitute product, due to the existence of hydroxyethyl groups, slow down the degradation speed of body endo-amylase to hydroxyethylamyle on the one hand, make it have certain antishock curative effect, thus extend it in the endovascular residence time, maintain its capacity enlargement effect.Because hydroxyethyl starch solution often comprises descending variable grain, relative molecular mass generally represents with mean number, and replacement degree refers to the ratio being accounted for total glucose molecule by the glucose molecule that hydroxyethyl replaces; Replacement mode then main manifestations is the ratio of the hydroxyethyl groups number on Shang YuC6 position, glucose C2 position.The dilatation intensity of hydroxyethyl starch solution and holding time, be decided by their concentration and relative molecular mass, and mol replaces degree and the mode of replacement.In general, average molecular mass is larger, and replace degree higher, C2/C6 ratio is larger, then longer in the endovascular residence time, dilatation intensity is higher.The hydroxyethylamyle of the low replacement level of middle-molecular-weihydroxyethyl due to body substantially without anaphylaxis and kidney function damage, do not affect by blood group coupling, and obvious untoward reaction be there is no to other aspects of blood, Clinical practice Be very effective, become most popular artificial plasm's surrogate.
The development experience of hydroxyethylamyle three generations: first-generation hydroxyethylamyle is a kind of hydroxyethylamyle (as hydroxyethylamyle 20/0.8, hydroxyethylamyle 40/0.8) of high replacement level high molecular.S-generation Hetastarch 200/0.5 is released as the hydroxyethylamyle of the low replacement level of middle-molecular-weihydroxyethyl.Third generation hydroxyethylamyle 130/0.4 also belongs to the product of the low replacement level of middle-molecular-weihydroxyethyl, and it reduce further molecular weight and replaces level on the basis of Hetastarch 200/0.5, obtains the hydroxyethylamyle product that performance is more superior.
In the bibliographical information of current preparation medium molecular weight hydroxyethyl starch 130/0.4, all take water as reaction medium, and during using water as reaction medium, the degraded of amylopectin and etherificate are heterogeneous reaction system, and reactant consumption amount is large, and by product ethylene glycol is many, product substitution value is difficult to control, cause product performance homogeneity poor, meanwhile, also can produce a large amount of waste water.Therefore, the homogeneous reaction medium of the callable amylopectin of development of new, improves hydroxyethylamyle quality product, has become domestic and international hydroxyethylamyle manufacturing enterprise urgent need to solve the problem.
Summary of the invention
The present invention is directed to deficiency of the prior art, thering is provided a kind of take ionic liquid as the preparation method of the hydroxyethylamyle 130/0.4 of reaction medium, the present invention adopts ionic liquid to substitute water as reaction medium, the hydrolysis of starch and etherification reaction are carried out in homogeneous system, when overcoming using water as inhomogeneous reaction medium, reactant consumption amount is large, and by product is many, the shortcomings such as product substitution value is difficult to control, product performance homogeneity difference.In addition, ionic liquid as green reaction medium have tasteless, pollution-free, nonflammable, easily and product separation, easily reclaim, can the premium properties such as iterative cycles use, make that synthesis technique is safer, environmental protection.
The present invention is achieved by the following technical solutions:
Take ionic liquid as a preparation method for the hydroxyethylamyle 130/0.4 of reaction medium, comprise the following steps:
A, amylopectin joined ionic liquid and heating and stir, make it be uniformly dissolved, form homogeneous reaction system;
B, add hydrochloric acid to the reaction system of step a, the kinematic viscosity to reaction solution is 12 ~ 20mm
2stop heating after/s, cool rapidly, add NaOH in process of cooling and be neutralized to reaction solution for neutral; In every milliliter of ionic liquid, the weight of amylopectin is the concentration of 0.05 ~ 0.15g, HCl is 0.1 ~ 0.5mol/L;
C, in the reacted reaction solution of step b, add sodium hydroxide, and drip etherifying agent and carry out etherification reaction, obtain reaction solution; Described etherifying agent is chloroethanol; The add-on of etherifying agent is: the mol ratio of amylopectin and etherifying agent is 1:0.3 ~ 0.7, and the concentration of sodium hydroxide is 0.5 ~ 1.5mol/L;
Add alcohol compound in d, the reaction solution that obtains in step c, its add-on be 5 times to the dehydrated alcohol of reaction solution volume, make it precipitation;
E, the throw out of steps d is obtained hydroxyethylamyle 130/0.4 product after decolouring, ultrafiltration, drying;
Described ionic liquid is that any one or a few in chlorination-1-allyl group-3-methylimidazole salt, 1-ethyl-3-methylimidazole acetic acid positive ion, 1-butyl-3-methylimidazolium chloride, 1-hydroxyethyl-3-methyl imidazolium tetrafluoroborate, 1-hydroxyethyl-3-Methylimidazole dodecane sulfonate, 1-hydroxyethyl-3-Methylimidazole villaumite, 1-hydroxyethyl-3-methylimidazolium hydrogen sulphate salt or 1-hydroxyethyl-3-methylimidazolium nitrate is composite.
In described step a, type of heating is steam-heated cal(l)andria, and the temperature being heated to reaction solution is 80 ~ 90 DEG C, and the best is 80 DEG C.
In described step b, temperature of reaction is 80 ~ 90 DEG C, and the best is 85 DEG C.
In described step c, temperature of reaction is 15 ~ 30 DEG C, and the best is 20 DEG C, and the reaction times is 4 ~ 6 hours, and the best is 4.5 hours.
Preferably, in described steps d, described alcohol compound is the mixture of any one or the two in dehydrated alcohol or methyl alcohol.
Preferably, described a kind of take ionic liquid as the preparation method of the hydroxyethylamyle 130/0.4 of reaction medium, comprise following concrete steps:
A, side chain W-Gum 100g is joined in 1000mL ionic liquid, under agitation reaction solution is heated to 85 DEG C, makes it be uniformly dissolved, form homogeneous reaction system.
B, in the reaction system of step a, add the hydrochloric acid that concentration is 0.3mol/L, under agitation in 85 DEG C of reactions, when the kinematic viscosity of reaction solution is 17mm
2stop heating after/s, be cooled to rapidly 30 DEG C, add NaOH in process of cooling and be neutralized to reaction solution for neutral.
C, in the reacted reaction solution of step b, add NaOH, the concentration of NaOH is 1.2mol/L, and drips chloroethanol, insulation reaction 4 hours at 20 DEG C, and the mol ratio of side chain W-Gum and chloroethanol is 1:0.55.
D, in the reacted reaction solution of step c, add dehydrated alcohol, the volume 5 of dehydrated alcohol, doubly to reaction solution, makes it precipitation.
E, precipitated products steps d obtained obtain white powder hydroxyethylamyle 130/0.4 after decolouring, ultrafiltration, drying.
The outstanding effect that the present invention compared with prior art has is:
The present invention adopts ionic liquid to substitute water as reaction medium, the hydrolysis of starch and etherification reaction are carried out in homogeneous system, and when overcoming using water as inhomogeneous reaction medium, reactant consumption amount is large, the shortcomings such as by product ethylene glycol content is high, product performance homogeneity difference.Adopt this Technology, effectively can reduce the residual of by product ethylene glycol in hydroxyethylamyle product, in finished product hydroxyethylamyle, ethylene glycol content is lower than 0.004%, meets the requirement of European Pharmacopoeia 7.0 editions.In addition, due to ionic liquid as green reaction medium have tasteless, pollution-free, nonflammable, easily and product separation, easily reclaim, can the advantage such as iterative cycles use, make that the synthesis technique of hydroxyethylamyle is safer, environmental protection, also there is wide market outlook and economic benefit.
Embodiment
Below in conjunction with embodiment, the present invention is further illustrated.
Embodiment 1
Take ionic liquid as a preparation method for the hydroxyethylamyle 130/0.4 of reaction medium, comprise the steps:
A, side chain W-Gum 100g is joined in 1000mL ionic liquid, under agitation reaction solution is heated to 85 DEG C, makes it be uniformly dissolved, form homogeneous reaction system.
B, in the reaction system of step a, add the hydrochloric acid that concentration is 0.3mol/L, under agitation in 85 DEG C of reactions, when the kinematic viscosity of reaction solution is 17mm
2stop heating after/s, be cooled to rapidly 30 DEG C, add NaOH in process of cooling and be neutralized to reaction solution for neutral.
C, in the reacted reaction solution of step b, add NaOH, the concentration of NaOH is 1.2mol/L, and drips chloroethanol, insulation reaction 4 hours at 20 DEG C, and the mol ratio of side chain W-Gum and chloroethanol is 1:0.55.
D, in the reacted reaction solution of step c, add dehydrated alcohol, the volume 5 of dehydrated alcohol, doubly to reaction solution, makes it precipitation.
E, precipitated products steps d obtained obtain white powder hydroxyethylamyle 130/0.4 after decolouring, ultrafiltration, drying.
Embodiment 2
Take ionic liquid as a preparation method for the hydroxyethylamyle 130/0.4 of reaction medium, comprise the steps:
A, side chain W-Gum 50g is joined in 1000mL ionic liquid, under agitation reaction solution is heated to 80 DEG C, makes it be uniformly dissolved, form homogeneous reaction system.
B, in the reaction system of step a, add the hydrochloric acid that concentration is 0.1mol/L, under agitation in 80 DEG C of reactions, when the kinematic viscosity of reaction solution is 16mm
2stop heating after/s, be cooled to rapidly 30 DEG C, add NaOH in process of cooling and be neutralized to reaction solution for neutral.
C, in the reacted reaction solution of step b, add NaOH, the concentration of NaOH is 1.3mol/L, and drips chloroethanol, insulation reaction 5 hours at 30 DEG C, and the mol ratio of side chain W-Gum and chloroethanol is 1:0.6.
D, in the reacted reaction solution of step c, add the methyl alcohol of 5 times of volumes, make it precipitation.
E, precipitated products steps d obtained obtain white powder hydroxyethylamyle 130/0.4 after decolouring, ultrafiltration, drying.
Embodiment 3
Take ionic liquid as a preparation method for the hydroxyethylamyle 130/0.4 of reaction medium, comprise the steps:
A, side chain W-Gum 70g is joined in 1000mL ionic liquid, under agitation reaction solution is heated to 90 DEG C, makes it be uniformly dissolved, form homogeneous reaction system.
B, in the reaction system of step a, add the hydrochloric acid that concentration is 0.15mol/L, under agitation in 90 DEG C of reactions, when the kinematic viscosity of reaction solution is 20mm
2stop heating after/s, be cooled to rapidly 30 DEG C, add NaOH in process of cooling and be neutralized to reaction solution for neutral.
C, in the reacted reaction solution of step b, add NaOH, the concentration of NaOH is 1.4mol/L, and drips chloroethanol, insulation reaction 6 hours at 15 DEG C, and the mol ratio of side chain W-Gum and chloroethanol is 1:0.65.
D, in the reacted reaction solution of step c, add the methyl alcohol of 5 times of volumes, make it precipitation.
E, precipitated products steps d obtained obtain white powder hydroxyethylamyle 130/0.4 after decolouring, ultrafiltration, drying.
Embodiment 4
Take ionic liquid as a preparation method for the hydroxyethylamyle 130/0.4 of reaction medium, comprise the steps:
A, side chain W-Gum 130g is joined in 1000mL ionic liquid, under agitation reaction solution is heated to 85 DEG C, makes it be uniformly dissolved, form homogeneous reaction system.
B, in the reaction system of step a, add the hydrochloric acid that concentration is 0.45mol/L, under agitation in 85 DEG C of reactions, when the kinematic viscosity of reaction solution is 19mm
2stop heating after/s, be cooled to rapidly 30 DEG C, add NaOH in process of cooling and be neutralized to reaction solution for neutral.
C, in the reacted reaction solution of step b, add NaOH, the concentration of NaOH is 1.5mol/L, and drips chloroethanol, insulation reaction 6 hours at 20 DEG C, and the mol ratio of side chain W-Gum and chloroethanol is 1:0.7.
D, in the reacted reaction solution of step c, add the dehydrated alcohol of 5 times of volumes, make it precipitation.
E, precipitated products steps d obtained obtain white powder hydroxyethylamyle 130/0.4 after decolouring, ultrafiltration, drying.
Embodiment 5
Take ionic liquid as a preparation method for the hydroxyethylamyle 130/0.4 of reaction medium, comprise the steps:
A, side chain W-Gum 150g is joined in 1000mL ionic liquid, under agitation reaction solution is heated to 90 DEG C, makes it be uniformly dissolved, form homogeneous reaction system.
B, in the reaction system of step a, add the hydrochloric acid that concentration is 0.5mol/L, under agitation in 90 DEG C of reactions, when the kinematic viscosity of reaction solution is 18mm
2stop heating after/s, be cooled to rapidly 30 DEG C, add NaOH in process of cooling and be neutralized to reaction solution for neutral.
C, in the reacted reaction solution of step b, add NaOH, the concentration of NaOH is 1.4mol/L, and drips chloroethanol, insulation reaction 5 hours at 20 DEG C, and the mol ratio of side chain W-Gum and chloroethanol is 1:0.65.
D, in the reacted reaction solution of step c, add the dehydrated alcohol of 5 times of volumes, make it precipitation.
E, precipitated products steps d obtained obtain white powder hydroxyethylamyle 130/0.4 after decolouring, ultrafiltration, drying.
Embodiment 6
Take ionic liquid as a preparation method for the hydroxyethylamyle 130/0.4 of reaction medium, comprise the steps:
A, side chain W-Gum 120g is joined in 1000mL ionic liquid, under agitation reaction solution is heated to 90 DEG C, makes it be uniformly dissolved, form homogeneous reaction system.
B, in the reaction system of step a, add the hydrochloric acid that concentration is 0.4mol/L, under agitation in 90 DEG C of reactions, when the kinematic viscosity of reaction solution is 15mm
2stop heating after/s, be cooled to rapidly 30 DEG C, add NaOH in process of cooling and be neutralized to reaction solution for neutral.
C, in the reacted reaction solution of step b, add NaOH, the concentration of NaOH is 1.5mol/L, and drips chloroethanol, insulation reaction 6 hours at 20 DEG C, and the mol ratio of side chain W-Gum and chloroethanol is 1:0.7.
D, in the reacted reaction solution of step c, add the methyl alcohol of 5 times of volumes, make it precipitation.
E, precipitated products steps d obtained obtain white powder hydroxyethylamyle 130/0.4 after decolouring, ultrafiltration, drying.
Embodiment 7
Take ionic liquid as a preparation method for the hydroxyethylamyle 130/0.4 of reaction medium, comprise the steps:
A, side chain W-Gum 110g is joined in 1000mL ionic liquid, under agitation reaction solution is heated to 85 DEG C, makes it be uniformly dissolved, form homogeneous reaction system.
B, in the reaction system of step a, add the hydrochloric acid that concentration is 0.25mol/L, under agitation in 85 DEG C of reactions, when the kinematic viscosity of reaction solution is 13mm
2stop heating after/s, be cooled to rapidly 30 DEG C, add NaOH in process of cooling and be neutralized to reaction solution for neutral.
C, in the reacted reaction solution of step b, add NaOH, the concentration of NaOH is 0.5mol/L, and drips chloroethanol, insulation reaction 4 hours at 30 DEG C, and the mol ratio of side chain W-Gum and chloroethanol is 1:0.3.
D, in the reacted reaction solution of step c, add the dehydrated alcohol of 5 times of volumes and the mixture of methyl alcohol, make it precipitation, the volume ratio of described dehydrated alcohol and methyl alcohol is 1:1.
E, precipitated products steps d obtained obtain white powder hydroxyethylamyle 130/0.4 after decolouring, ultrafiltration, drying.
Embodiment 8
Take ionic liquid as a preparation method for the hydroxyethylamyle 130/0.4 of reaction medium, comprise the steps:
A, side chain W-Gum 90g is joined in 1000mL ionic liquid, under agitation reaction solution is heated to 80 DEG C, makes it be uniformly dissolved, form homogeneous reaction system.
B, in the reaction system of step a, add the hydrochloric acid that concentration is 0.2mol/L, under agitation in 80 DEG C of reactions, when the kinematic viscosity of reaction solution is 14mm
2stop heating after/s, be cooled to rapidly 30 DEG C, add NaOH in process of cooling and be neutralized to reaction solution for neutral.
C, in the reacted reaction solution of step b, add NaOH, the concentration of NaOH is 0.6mol/L, and drips chloroethanol, insulation reaction 5 hours at 20 DEG C, and the mol ratio of side chain W-Gum and chloroethanol is 1:0.4.
D, in the reacted reaction solution of step c, add the dehydrated alcohol of 5 times of volumes and the mixture of methyl alcohol, make it precipitation, the volume ratio of described dehydrated alcohol and methyl alcohol is 1:1.
E, precipitated products steps d obtained obtain white powder hydroxyethylamyle 130/0.4 after decolouring, ultrafiltration, drying.
Embodiment 9
Take ionic liquid as a preparation method for the hydroxyethylamyle 130/0.4 of reaction medium, comprise the steps:
A, side chain W-Gum 140g is joined in 1000mL ionic liquid, under agitation reaction solution is heated to 85 DEG C, makes it be uniformly dissolved, form homogeneous reaction system.
B, in the reaction system of step a, add the hydrochloric acid that concentration is 0.35mol/L, under agitation in 85 DEG C of reactions, when the kinematic viscosity of reaction solution is 12mm
2stop heating after/s, be cooled to rapidly 30 DEG C, add NaOH in process of cooling and be neutralized to reaction solution for neutral.
C, in the reacted reaction solution of step b, add NaOH, the concentration of NaOH is 1.0mol/L, and drips chloroethanol, insulation reaction 5 hours at 25 DEG C, and the mol ratio of side chain W-Gum and chloroethanol is 1:0.45.
D, in the reacted reaction solution of step c, add the dehydrated alcohol of 5 times of volumes and the mixture of methyl alcohol, make it precipitation, the volume ratio of described dehydrated alcohol and methyl alcohol is 1:1.
E, precipitated products steps d obtained obtain white powder hydroxyethylamyle 130/0.4 after decolouring, ultrafiltration, drying.
Hydroxyethylamyle 130/0.4 detected result prepared by embodiment 1 ~ 9 is as following table 1.
Claims (8)
1. be a preparation method for the hydroxyethylamyle 130/0.4 of reaction medium with ionic liquid, it is characterized in that comprising the following steps:
A, amylopectin joined ionic liquid and heating and stir, make it be uniformly dissolved, form homogeneous reaction system;
B, add hydrochloric acid to the reaction system of step a, the kinematic viscosity to reaction solution is 12 ~ 20mm
2stop heating after/s, cool rapidly, add NaOH in process of cooling and be neutralized to reaction solution for neutral; In every milliliter of ionic liquid, the weight of amylopectin is the concentration of 0.05 ~ 0.15g, HCl is 0.1 ~ 0.5mol/L;
C, in the reacted reaction solution of step b, add sodium hydroxide, and drip etherifying agent and carry out etherification reaction, obtain reaction solution; Described etherifying agent is chloroethanol; The add-on of etherifying agent is: the mol ratio of amylopectin and etherifying agent is 1:0.3 ~ 0.7, and the concentration of sodium hydroxide is 0.5 ~ 1.5mol/L;
Add alcohol compound in d, the reaction solution that obtains in step c, its add-on be 5 times to the dehydrated alcohol of reaction solution volume, make it precipitation;
E, the throw out of steps d is obtained hydroxyethylamyle 130/0.4 product after decolouring, ultrafiltration, drying;
Described ionic liquid is that two or more are composite for any in chlorination-1-allyl group-3-methylimidazole salt, 1-ethyl-3-methylimidazole acetic acid positive ion, 1-hydroxyethyl-3-methyl imidazolium tetrafluoroborate, 1-hydroxyethyl-3-Methylimidazole dodecane sulfonate, 1-hydroxyethyl-3-Methylimidazole villaumite, 1-hydroxyethyl-3-methylimidazolium hydrogen sulphate salt or 1-hydroxyethyl-3-methylimidazolium nitrate;
In described step a, type of heating is steam-heated cal(l)andria, and the temperature being heated to reaction solution is 80 ~ 90 DEG C.
2. a kind of as claimed in claim 1 take ionic liquid as the preparation method of the hydroxyethylamyle 130/0.4 of reaction medium, and it is characterized in that, in described step a, the temperature being heated to reaction solution is 80 DEG C.
3. a kind of as claimed in claim 1 take ionic liquid as the preparation method of the hydroxyethylamyle 130/0.4 of reaction medium, and it is characterized in that, in described step b, temperature of reaction is 80 ~ 90 DEG C.
4. a kind of as claimed in claim 3 take ionic liquid as the preparation method of the hydroxyethylamyle 130/0.4 of reaction medium, and it is characterized in that, in described step b, temperature of reaction is 85 DEG C.
5. a kind of as claimed in claim 1 take ionic liquid as the preparation method of the hydroxyethylamyle 130/0.4 of reaction medium, and it is characterized in that, in described step c, temperature of reaction is 15 ~ 30 DEG C, and the reaction times is 4 ~ 6 hours.
6. a kind of as claimed in claim 5 take ionic liquid as the preparation method of the hydroxyethylamyle 130/0.4 of reaction medium, and it is characterized in that, in described step c, temperature of reaction is 20 DEG C, and the reaction times is 4.5 hours.
7. a kind of as claimed in claim 1 take ionic liquid as the preparation method of the hydroxyethylamyle 130/0.4 of reaction medium, it is characterized in that, in described steps d, described alcohol compound is the mixture of any one or the two in dehydrated alcohol or methyl alcohol.
8. a kind of as claimed in claim 1 take ionic liquid as the preparation method of the hydroxyethylamyle 130/0.4 of reaction medium, it is characterized in that, comprises following concrete steps:
A, side chain W-Gum 100g is joined in 1000mL ionic liquid, under agitation reaction solution is heated to 85 DEG C, makes it be uniformly dissolved, form homogeneous reaction system;
B, in the reaction system of step a, add the hydrochloric acid that concentration is 0.3mol/L, under agitation in 85 DEG C of reactions, when the kinematic viscosity of reaction solution is 17mm
2stop heating after/s, be cooled to rapidly 30 DEG C, add NaOH in process of cooling and be neutralized to reaction solution for neutral;
C, in the reacted reaction solution of step b, add NaOH, the concentration of NaOH is 1.2mol/L, and drips chloroethanol, insulation reaction 4 hours at 20 DEG C, and the mol ratio of side chain W-Gum and chloroethanol is 1:0.55;
D, in the reacted reaction solution of step c, add dehydrated alcohol, the volume 5 of dehydrated alcohol, doubly to reaction solution, makes it precipitation;
E, precipitated products steps d obtained obtain white powder hydroxyethylamyle 130/0.4 after decolouring, ultrafiltration, drying.
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