CN105777920A - Method for preparing hydroxyethyl starch 200/0.5 - Google Patents
Method for preparing hydroxyethyl starch 200/0.5 Download PDFInfo
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- CN105777920A CN105777920A CN201610335589.XA CN201610335589A CN105777920A CN 105777920 A CN105777920 A CN 105777920A CN 201610335589 A CN201610335589 A CN 201610335589A CN 105777920 A CN105777920 A CN 105777920A
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- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B35/00—Preparation of derivatives of amylopectin
- C08B35/04—Ethers
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Abstract
The invention provides a method for preparing hydroxyethyl starch 200/0.5. According to the method, sticky rice starch is taken as a raw material, ethylene oxide is taken as an etherifying agent and isopropanol is taken as a reaction solvent. The production process of the method comprises steps such as mixing, gelatinization, hydrolysis, etherification, neutralization, refining, drying and the like. By adopting the method, dextran hydroxyethyl starch 200/0.5 of which the molecular weight and the substitution degree both meet the requirements can be prepared, and moreover the method is simple in preparation process, small in side reaction and high in product yield.
Description
Technical field
The preparation method that the present invention relates to a kind of Hetastarch 200/0.5.
Background technology
Amylase has been had repellence by the hetastarch after hydroxyethylation, and the size of its resistivity is relevant with substitution value height.The hetastarch with specified molecular weight and substitution value can use as plasma substitute.
Number of patent application is 201310057158.8(denomination of invention: Hetastarch 200/0.5 that can be used as plasma substitute and preparation method thereof), side reaction therein is more, and product yield is not very high.
Summary of the invention
The preparation method that the technical problem to be solved in the present invention is to provide a kind of Hetastarch 200/0.5, it is desirable to this preparation method safety, and preparation technology is simple, side reaction is few, product yield high.Prepared Hetastarch 200/0.5 index meets " State Food and Drug Administration's standard " (YBH03072007) requirement.
For solving above-mentioned technical problem, the preparation method that the present invention provides a kind of Hetastarch 200/0.5, comprise the following steps:
(1) mixing: under stirring, the deionized water of 100 weight portion glutinous rice starchs and 180 250 weight portions is joined in sealable reactor, stirs under 46 48 DEG C of conditions, obtain glutinous rice starch breast；
(2) gelatinizing: under stirring, heats the glutinous rice starch breast obtained by step (1) to continuing stirring 15 20min after 90 95 DEG C, obtains glutinous rice starch dextrin, be cooled to 40 45 DEG C standby；
(3) hydrolysis: under stirring, adding 1.5 2.5 weight portion concentration in the glutinous rice starch dextrin prepared by step (2) is the hydrochloric acid solution of 1mol/L, and temperature maintains 40 45 DEG C and is hydrolyzed；
In hydrolytic process, every the 10min viscosity measuring a dextrin, it is plotted against time with intrinsic viscosity, is extrapolated to the intrinsic viscosity time equal to 0.2 0.3dl/g, terminate hydrolysis and obtain glutinous rice starch hydrolyzed solution；
(4) neutralize: under stirring, 0.2 0.5 parts by weight of sodium hydroxide are added in the glutinous rice starch hydrolyzed solution prepared by step (3), after reaction 30min, add 300 400 weight portion dehydrated alcohol, temperature maintains 38 40 DEG C, stand 8 10h after stirring, remove the supernatant liquid after standing, obtain the satisfactory degraded glutinous rice starch of molecular weight；
(5) etherificate: maintain the temperature at 38 40 DEG C, under stirring condition, be sequentially added into 1.6 2.4 parts by weight of sodium hydroxide, 100 120 parts by weight of isopropyl alcohol, 14 15 parts by weight epoxy ethane in reactor, terminates reaction after reacting 18 19h；
(6) neutralize: under stirring, in the hydroxyethyl starch solution prepared by step (5), add proper amount of acetic acid, make solution ph adjust after 6.6 6.8 and filter to obtain thick Hetastarch 200/0.5；
(7) refining: at normal temperatures, thick Hetastarch 200/0.5 prepared by step (6) is dissolved in ethanol water refining, until the various water-solubility impurities of Hetastarch 200/0.5 all meet product standard requirement；
(8) dry: Hetastarch 200/0.5 prepared by step (7) is dissolved in 50 60 weight portion deionized waters, spray-dried namely obtain Hetastarch 200/0.5.
As further optimization, described thick Hetastarch 200/0.5 refined as being dissolved in thick Hetastarch 200/0.5 in the ethanol water that 60 70 weight portion mass percent concentrations are 84%, separate after standing 10 12h after stirring, so repeat this step repeatedly.
Described sodium hydroxide adopts mass percent concentration to be the sodium hydrate aqueous solution of 25%.
For the purpose of concise explanation problem, below to the preparation method of a kind of Hetastarch 200/0.5 of the present invention all referred to as this method.
Preparation can make the hetastarch of plasma substitute, it is necessary to amylopectin, glutinous rice starch is almost amylopectin entirely, and therefore, this method adopts glutinous rice starch.
The purpose of starch gelatinization is to allow starch molecule fully expand, and is beneficial to acid stepless action and makes the molecular weight of the sour starch degraded try one's best uniformly in the various piece of starch molecule.
Hydrolysing step in this method in order that the macromole of glutinous rice starch to be reduced to the starch that weight average molecular weight is 180,000 290000.
Hydrolysing step requires that equipment is acidproof.Alkalinization step requires that equipment is alkaline-resisting.
The weight average molecular weight of Hetastarch 200/0.5 prepared by the present invention to be strict controlled in 180,000 290000 scopes.This method, by studying the corresponding relation of starch molecule amount and intrinsic viscosity, utilizes the intrinsic viscosity of starch hydrolyzate to judge the molecular weight of starch.Specific practice is: be plotted against time with intrinsic viscosity, is extrapolated to the intrinsic viscosity time equal to 0.2 0.3dL/g, terminates hydrolysis.
The reason of hydrolysis time corresponding to extrapolation intrinsic viscosity is needed to be because the molecular size range of starch relevant to its intrinsic viscosity, the size of starch molecule amount is judged by measuring the intrinsic viscosity i.e. corresponding relation of the available starch molecule amount studied and intrinsic viscosity of different hydrolysis time starch, but intrinsic viscosity needs certain time, if etc. measurement result out after terminate hydrolysis again, then starch excessive hydrolysis.Therefore hydrolysis time need to be extrapolated, namely by measuring the intrinsic viscosity of different time, then according to the variation tendency between intrinsic viscosity and time, determine (prediction) amylolytic end time in advance.
The hydrolysing step of this method adopts hydrochloric acid to be hydrolyzed, and neutralization procedure adopts sodium hydroxide to be neutralized, and the sodium chloride that sodium hydroxide and hydrochloric acid generate is prone to washing and removes.
In this method, the starch after hydrolysis adopts oxirane to carry out hydroxyethylation, and side reaction is few so that the reaction yield of this method is high.
In sum, this method has the advantage that preparation technology is simple, side reaction is few, product yield is high, and prepared Hetastarch 200/0.5 index meets " State Food and Drug Administration's standard " (YBH03072007) requirement.
Detailed description of the invention
Below by specific embodiment, the invention will be further described:
Embodiment 1
The preparation method of a kind of Hetastarch 200/0.5, comprises the following steps:
(1) mixing: under stirring, the deionized water of 100kg glutinous rice starch and 180kg is joined in sealable reactor, stir under 46 DEG C of conditions, obtain glutinous rice starch breast；
(2) gelatinizing: under stirring, heats the glutinous rice starch breast obtained by step (1) to continuing stirring 15min after 90 DEG C, obtains glutinous rice starch dextrin, be cooled to 40 DEG C standby；
(3) hydrolysis: under stirring, adding 1.5kg concentration in the glutinous rice starch dextrin prepared by step (2) is the hydrochloric acid solution of 1mol/L, and temperature maintains 40 DEG C and is hydrolyzed；
In hydrolytic process, every the 10min viscosity measuring a dextrin, it is plotted against time with intrinsic viscosity, is extrapolated to the intrinsic viscosity time equal to 0.2dl/g, terminate hydrolysis and obtain glutinous rice starch hydrolyzed solution；
(4) neutralize: under stirring, 0.2kg sodium hydroxide is added in the glutinous rice starch hydrolyzed solution prepared by step (3), after reaction 30min, add 300kg dehydrated alcohol, temperature maintains 38 DEG C, stand 8h after stirring, remove the supernatant liquid after standing, obtain the satisfactory degraded glutinous rice starch of molecular weight；
(5) etherificate: maintain the temperature at 38 DEG C, under stirring condition, be sequentially added into 1.6kg sodium hydroxide, 100kg isopropanol, 14kg oxirane in reactor, terminate reaction after reaction 18h；
(6) neutralize: under stirring, in reactor, add proper amount of acetic acid, make solution ph adjust after 6.6 and filter to obtain thick Hetastarch 200/0.5；
(7) refining: at normal temperatures, thick Hetastarch 200/0.5 prepared by step (6) is dissolved in the ethanol water that 60kg mass percent concentration is 84%, separate after standing 10h after stirring, so repeat this purification step repeatedly, until the various water-solubility impurities of Hetastarch 200/0.5 all meet product standard requirement；
(8) dry: Hetastarch 200/0.5 prepared by step (7) is dissolved in 50kg deionized water, spray-dried namely obtain Hetastarch 200/0.5.
The weight average molecular weight of Hetastarch 200/0.5 prepared is 180,000 290000；Molar substitution is 0.43 0.55, meets " State Food and Drug Administration's standard " (YBH03072007) requirement.
Embodiment 2
The preparation method of a kind of Hetastarch 200/0.5, comprises the following steps:
(1) mixing: under stirring, the deionized water of 100kg glutinous rice starch and 250kg is joined in sealable reactor, stir under 48 DEG C of conditions, obtain glutinous rice starch breast；
(2) gelatinizing: under stirring, heats the glutinous rice starch breast obtained by step (1) to continuing stirring 20min after 95 DEG C, obtains glutinous rice starch dextrin, be cooled to 45 DEG C standby；
(3) hydrolysis: under stirring, adding 2.5kg concentration in the glutinous rice starch dextrin prepared by step (2) is the hydrochloric acid solution of 1mol/L, and temperature maintains 45 DEG C and is hydrolyzed；
In hydrolytic process, every the 10min viscosity measuring a dextrin, it is plotted against time with intrinsic viscosity, is extrapolated to the intrinsic viscosity time equal to 0.3dl/g, terminate hydrolysis and obtain glutinous rice starch hydrolyzed solution；
(4) neutralize: under stirring, 0.5kg sodium hydroxide is added in the glutinous rice starch hydrolyzed solution prepared by step (3), after reaction 30min, add 400kg dehydrated alcohol, temperature maintains 40 DEG C, stand 10h after stirring, remove the supernatant liquid after standing, obtain the satisfactory degraded glutinous rice starch of molecular weight；
(5) etherificate: maintain the temperature at 40 DEG C, under stirring condition, be sequentially added into 2.4kg sodium hydroxide, 120kg isopropanol, 15kg oxirane in reactor, terminate reaction after reaction 19h；
(6) neutralize: under stirring, in reactor, add proper amount of acetic acid, make solution ph adjust after 6.8 and filter to obtain thick Hetastarch 200/0.5；
(7) refining: at normal temperatures, thick Hetastarch 200/0.5 prepared by step (6) is dissolved in the ethanol water that 70kg mass percent concentration is 84%, separate after standing 12h after stirring, so repeat this purification step repeatedly, until the various water-solubility impurities of Hetastarch 200/0.5 all meet product standard requirement；
(8) dry: Hetastarch 200/0.5 prepared by step (7) is dissolved in 60kg deionized water, spray-dried namely obtain Hetastarch 200/0.5.
The weight average molecular weight of Hetastarch 200/0.5 prepared is 180,000 290000；Molar substitution is 0.43 0.55, meets " State Food and Drug Administration's standard " (YBH03072007) requirement.
Embodiment 3
The preparation method of a kind of Hetastarch 200/0.5, comprises the following steps:
(1) mixing: under stirring, the deionized water of 100kg glutinous rice starch and 220kg is joined in sealable reactor, stir under 47 DEG C of conditions, obtain glutinous rice starch breast；
(2) gelatinizing: under stirring, heats the glutinous rice starch breast obtained by step (1) to continuing stirring 18min after 93 DEG C, obtains glutinous rice starch dextrin, be cooled to 42 DEG C standby；
(3) hydrolysis: under stirring, adding 2.0kg concentration in the glutinous rice starch dextrin prepared by step (2) is the hydrochloric acid solution of 1mol/L, and temperature maintains 42 DEG C and is hydrolyzed；
In hydrolytic process, every the 10min viscosity measuring a dextrin, it is plotted against time with intrinsic viscosity, is extrapolated to the intrinsic viscosity time equal to 0.2dl/g, terminate hydrolysis and obtain glutinous rice starch hydrolyzed solution；
(4) neutralize: under stirring, 0.3kg sodium hydroxide is added in the glutinous rice starch hydrolyzed solution prepared by step (3), after reaction 30min, add 350kg dehydrated alcohol, temperature maintains 39 DEG C, stand 10h after stirring, remove the supernatant liquid after standing, obtain the satisfactory degraded glutinous rice starch of molecular weight；
(5) etherificate: maintain the temperature at 38 DEG C, under stirring condition, be sequentially added into 2.0kg sodium hydroxide, 110kg isopropanol, 15kg oxirane in reactor, terminate reaction after reaction 19h；
(6) neutralize: under stirring, in reactor, add proper amount of acetic acid, make solution ph adjust after 6.7 and filter to obtain thick Hetastarch 200/0.5；
(7) refining: at normal temperatures, thick Hetastarch 200/0.5 prepared by step (6) is dissolved in the ethanol water that 65kg mass percent concentration is 84%, separate after standing 11h after stirring, so repeat this purification step repeatedly, until the various water-solubility impurities of Hetastarch 200/0.5 all meet product standard requirement；
(8) dry: Hetastarch 200/0.5 prepared by step (7) is dissolved in 55kg deionized water, spray-dried namely obtain Hetastarch 200/0.5.
The weight average molecular weight of Hetastarch 200/0.5 prepared is 180,000 290000；Molar substitution is 0.43 0.55, meets " State Food and Drug Administration's standard " (YBH03072007) requirement.
Claims (3)
1. a preparation method for Hetastarch 200/0.5, comprises the following steps:
(1) mixing: under stirring, the deionized water of 100 weight portion glutinous rice starchs and 180 250 weight portions is joined in sealable reactor, stirs under 46 48 DEG C of conditions, obtain glutinous rice starch breast；
(2) gelatinizing: under stirring, heats the glutinous rice starch breast obtained by step (1) to continuing stirring 15 20min after 90 95 DEG C, obtains glutinous rice starch dextrin, be cooled to 40 45 DEG C standby；
(3) hydrolysis: under stirring, adding 1.5 2.5 weight portion concentration in the glutinous rice starch dextrin prepared by step (2) is the hydrochloric acid solution of 1mol/L, and temperature maintains 40 45 DEG C and is hydrolyzed；
In hydrolytic process, every the 10min viscosity measuring a dextrin, it is plotted against time with intrinsic viscosity, is extrapolated to the intrinsic viscosity time equal to 0.2 0.3dl/g, terminate hydrolysis and obtain glutinous rice starch hydrolyzed solution；
(4) neutralize: under stirring, 0.2 0.5 parts by weight of sodium hydroxide are added in the glutinous rice starch hydrolyzed solution prepared by step (3), after reaction 30min, add 300 400 weight portion dehydrated alcohol, temperature maintains 38 40 DEG C, stand 8 10h after stirring, remove the supernatant liquid after standing, obtain the satisfactory degraded glutinous rice starch of molecular weight；
(5) etherificate: maintain the temperature at 38 40 DEG C, under stirring condition, be sequentially added into 1.6 2.4 parts by weight of sodium hydroxide, 100 120 parts by weight of isopropyl alcohol, 14 15 parts by weight epoxy ethane in reactor, terminates reaction after reacting 18 19h；
(6) neutralize: under stirring, in the hydroxyethyl starch solution prepared by step (5), add proper amount of acetic acid, make solution ph adjust after 6.6 6.8 and filter to obtain thick Hetastarch 200/0.5；
(7) refining: at normal temperatures, thick Hetastarch 200/0.5 prepared by step (6) is dissolved in ethanol water refining, until the various water-solubility impurities of Hetastarch 200/0.5 all meet product standard requirement；
(8) dry: Hetastarch 200/0.5 prepared by step (7) is dissolved in 50 60 weight portion deionized waters, spray-dried namely obtain Hetastarch 200/0.5.
2. the preparation method of a kind of Hetastarch 200/0.5 according to claim 1, it is characterized in that: described thick Hetastarch 200/0.5 refined as being dissolved in thick Hetastarch 200/0.5 in the ethanol water that 60 70 weight portion mass percent concentrations are 84%, separate after standing 10 12h after stirring, so repeat this purification step repeatedly.
3. the preparation method of a kind of Hetastarch 200/0.5 according to claim 1, it is characterised in that: described sodium hydroxide adopts mass percent concentration to be the sodium hydrate aqueous solution of 25%.
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| CN201610335589.XA CN105777920A (en) | 2016-05-19 | 2016-05-19 | Method for preparing hydroxyethyl starch 200/0.5 |
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| CN201610335589.XA CN105777920A (en) | 2016-05-19 | 2016-05-19 | Method for preparing hydroxyethyl starch 200/0.5 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5218108A (en) * | 1989-06-16 | 1993-06-08 | Fresenius Ag | Hydroxylethylstarch (hes) as plasma expander and process for preparing hes |
| CN102887958A (en) * | 2011-07-19 | 2013-01-23 | 四川科伦药物研究有限公司 | Preparation method of hydroxyethyl starch |
| CN103087206A (en) * | 2013-02-20 | 2013-05-08 | 郑桂富 | Hydroxyethyl starch 200/0.5 capable of being used as dextran and preparation method thereof |
-
2016
- 2016-05-19 CN CN201610335589.XA patent/CN105777920A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5218108A (en) * | 1989-06-16 | 1993-06-08 | Fresenius Ag | Hydroxylethylstarch (hes) as plasma expander and process for preparing hes |
| CN102887958A (en) * | 2011-07-19 | 2013-01-23 | 四川科伦药物研究有限公司 | Preparation method of hydroxyethyl starch |
| CN103087206A (en) * | 2013-02-20 | 2013-05-08 | 郑桂富 | Hydroxyethyl starch 200/0.5 capable of being used as dextran and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 刘亚伟: "《玉米淀粉生产及转化技术（第1版）》", 28 February 2003, 化学工业出版社 * |
| 范望喜等: "《有机化学（第三版）》", 30 June 2015, 华中师范大学出版社 * |
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Application publication date: 20160720 |