CN107880140A - The preparation method and production control method of a kind of hydroxypropul starch - Google Patents
The preparation method and production control method of a kind of hydroxypropul starch Download PDFInfo
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- CN107880140A CN107880140A CN201711236953.8A CN201711236953A CN107880140A CN 107880140 A CN107880140 A CN 107880140A CN 201711236953 A CN201711236953 A CN 201711236953A CN 107880140 A CN107880140 A CN 107880140A
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- hydroxypropul starch
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B31/00—Preparation of derivatives of starch
- C08B31/08—Ethers
- C08B31/12—Ethers having alkyl or cycloalkyl radicals substituted by heteroatoms, e.g. hydroxyalkyl or carboxyalkyl starch
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Abstract
The invention provides a kind of preparation of hydroxypropul starch and control method, concrete technology includes：The expoxy propane of volatilization is adsorbed in starch reaction tank top ethanol solution；Directly reflect substitution value using brabender viscosity, control reaction is carried out.Preparing hydroxypropul starch using the preparation and control method not only can effectively utilize various resources, prevent the waste of raw material, higher substitution value can also be obtained, it is important that reaction process can be controlled according to required substitution value, and production technology operation is relatively simple, reaction condition is gentle, and yield is considerable, is adapted to industrialized production.
Description
Technical field
The present invention relates to Starch Production field, and in particular to a kind of preparation method of hydroxypropul starch and production controlling party
Method.
Background technology
Hydroxypropul starch (Hydroxypropyl Starch, abbreviation HPS) belongs to non-ionic starch derivative, starch molecule
Upper a certain amount of hydroxypropyl of introducing can strengthen the hydrophilic water retention property of gelatinized corn starch, improve the transparency and freeze-thaw stability of gelatinized corn starch
Property, it is a kind of safe modified food starch generally acknowledged both at home and abroad.Appropriate hydroxypropul starch is added in flour, can be effectively
Improve the quality of dough, and also have extensive application in konjak product, meat products and frozen food industry etc..In addition, hydroxyl
Propyl group starch can partly replace expensive natural gum (agar, gelatin, pectin etc.)；Hydroxypropul starch is used in textile industry
The warp sizing of fiber, is used as drilling fluid additive in petroleum industry, in daily-use chemical industry and cosmetics as thickener, suspend
Agent, it is used as binding agent etc. in construction material.
Industrial production hydroxypropul starch is to carry out etherification reaction in the basic conditions with expoxy propane using starch to enter
OK, etherification reaction is occurred mainly in starch on shrink glucose unit on C2 and C6 hydroxyl, the hydroxypropyl of prior art production
There is the not high problem of substitution value caused by the volatilization of raw material expoxy propane wastes in base starch, and production process is difficult to control, nothing
The problem of method controls the substitution value size of hydroxypropul starch and then controls reaction end according to demand.
In summary, how a kind of high hydroxypropul starch production method of raw material availability is provided and was accurately produced
The problem of process control method is those skilled in the art's urgent need to resolve.
The content of the invention
Problem regarding to the issue above, and course of reaction high it is an object of the invention to provide a kind of substitution value can be according to taking
The hydroxypropul starch production method of Dai Du demand modeling.
To achieve these goals, the present invention adopts the following technical scheme that：
A kind of preparation method of hydroxypropul starch, it is characterised in that comprise the following steps：
(1) corn starch milk is put into retort, adds water, is stirred, the cornstarch aqueous solution is made；
(2) then add sodium chloride；
(3) it is slowly added to sodium hydroxide solution；
(4) it is 18 DEG C -20 DEG C to control temperature of charge in retort, is slowly added to expoxy propane；
(5) ethanol solution is taken, is sprayed by the shower of reactor top, material in retort is warming up to 38 DEG C -40
DEG C, fully reaction, until terminating, obtain hydroxypropul starch.
Preferably, the amount that water is added in the step (1) is until corn starch milk to be modulated into 35wt%-40wt% water
Solution.
Preferably, the amount of the sodium chloride added in the step (2) is the 8%- of cornstarch dry weight in corn starch milk
10%.
Preferably, the concentration for sodium hydroxide solution being added in the step (3) is 3wt%-5wt%, and the amount of addition is straight
To pH value of solution to 11-12.
Preferably, the amount of the expoxy propane added in the step (4) is cornstarch dry weight in corn starch milk
5%-12%.
Preferably, ethanol solution concentration is 10-50% in the step (5).
The beneficial effect of such scheme is：In starch reaction device top add-back flow tube (shower), ethanol solution, profit are sprayed
With the expoxy propane to be volatilized in the similar principle absorbing reaction device that mixes, amidin that can also be in refluxing reactor fills
Divide the expoxy propane of absorption volatilization in the reactor, make full use of raw material expoxy propane, play its maximum benefit, managed
Substitution value in thinking.This preparation method, limited resources can be utilized to greatest extent, the waste of resource is avoided, realizes efficiency
Optimization.
It is another object of the present invention to provide a kind of control method of substitution value in hydroxypropul starch preparation process,
Material carried out in abundant course of reaction in retort described in step (5), comprises the following steps：
(5.1) sample, primary first-order equation material is taken into testing tube every the identical period, adjust testing tube reaction mass
The pH of solution, water washing is distilled, obtains test sample；
(5.2) test, test sample is configured to the amidin of dry matter content 5%-6% concentration, using Bradley class
Moral instrument detects amidin curve, must play paste temperature, and judge substitution value according to paste temperature is played；
(5.3) reach the pH that material in retort is adjusted after preferable substitution value, washing, dehydration, dry, packaging, obtain needed for
The hydroxypropul starch of substitution value.
Preferably, for regulation pH value of solution to 5.5-6.5, it is 37 μ s/cm-43 μ s/ to wash to electrical conductivity in the step (5.3)
cm。
The beneficial effect of above-mentioned technical proposal is：According to this production control method, hydroxypropul starch can be monitored in real time
The carry out degree of synthetic reaction, and the substitution value of the target product according to required for different clients, targetedly to synthesize
The hydroxypropul starch of corresponding substitution value, thus, it is ensured that the substitution value of hydroxypropul starch meets customer demand, and quality is high, this
Kind production control method is easy to operate, can accomplish to monitor in real time, be applicable the hydroxypropul starch of any substitution value scope.
In summary, the beneficial effects of the invention are as follows：It provide not only that a kind of raw material availability is high and height easy to operate
The preparation method of substitution value hydroxypropyl starch, and provide a kind of control prepared using the above method during hydroxypropul starch
Method processed, the substitution value of hydroxypropul starch can be monitored in real time, in order to which the substitution value needed for reasonably controls reaction process simultaneously
And terminate to react in time, it is ensured that the accurate compound customer demand of the substitution value of obtained hydroxypropul starch.
Embodiment
Just the embodiment of the present invention is described further below.
Unless otherwise instructed, the raw material employed in the present invention is commercially available or commonly used in the art, such as
Without special instruction, the method in following embodiments is the conventional method of this area.
The invention provides a kind of preparation method of hydroxypropul starch, comprise the following steps：
(1) corn starch milk is put into retort, adds water that corn starch milk is modulated into the water-soluble of 35wt%-40wt%
Liquid, stir；
(2) then add cornstarch dry weight 8%-10% sodium chloride；
(3) sodium hydroxide that concentration is 3wt%-5wt% is slowly added to, up to pH value of solution to 11.0-12.0；
(4) it is 18 DEG C -20 DEG C to control temperature of charge in retort, is slowly added to expoxy propane；
(5) ethanol solution that concentration is 10-50% is taken, is sprayed by the shower of reactor top, by thing in retort
Material is warming up to 38 DEG C -40 DEG C, fully reaction, until terminating, obtains hydroxypropul starch.
In retort material fully carries out course of reaction, include the production rate-determining steps of hydroxypropul starch, according to institute
Substitution value is needed to control the end of reaction, for example following embodiments of concrete operations.
Embodiment 1
The present embodiment provides preparation and the production control method of a kind of hydroxypropul starch, it is desirable to which substitution value is in 0.08-0.09
In the range of, its step includes：
A. course of reaction：In retort put into 1.5 tons of corn starch milks, add water degree of thickening into concentration be 35wt% it is water-soluble
Liquid, it is stirring evenly and then adding into 8% sodium chloride (120kg) for accounting for cornstarch dry weight；It is slow added into concentration 3wt% hydrogen-oxygen
Change sodium, regulation solution ph is cooled to 18 DEG C to 11.0；It is slow added into 5% expoxy propane for accounting for cornstarch dry weight
(75kg), the ethanol solution 100kg of 10% concentration is taken, is sprayed by the shower of reactor top, coutroi velocity 50kg/h,
2h is sprayed, 38 DEG C is then raised temperature to, continues to react.
B. process is monitored：In course of reaction, 100ml reaction materials are taken every 2h, are first adjusted with 10wt% hydrochloric acid solution anti-
The pH of solution should be expected to 5.5, then it is 37 μ s/cm to be washed with distilled water to electrical conductivity, obtains test sample.By test sample, match somebody with somebody
The amidin 500ml of the concentration of dry matter content 5% is set to, amidin curve is detected with brabender instrument, is risen
It is 61-62 DEG C to paste temperature, and at a temperature of this plays paste, substitution value, can terminating reaction in the range of 0.08-0.09；When it plays paste temperature
For 62.5-65 DEG C, at a temperature of this plays paste, when substitution value is in the range of 0.05-0.08, continue to react, repeat the step.
C. terminating reaction：After reaching substitution value 0.08-0.09, add 10wt% hydrochloric acid solution adjust reaction solution pH to
5.5, cyclone washing, dehydration, dry, packaging.
Embodiment 2
The present embodiment provides preparation and the production control method of a kind of hydroxypropul starch, it is desirable to which the substitution value of target product will
Ask more than 0.08, its step includes：
A. course of reaction：1.75 tons of corn starch milks are put into retort, add water degree of thickening into the water that concentration is 37wt%
Solution, it is stirring evenly and then adding into 9% sodium chloride (157.5kg) for accounting for cornstarch dry weight；It is slow added into concentration 4wt%'s
Sodium hydroxide, regulation solution ph are cooled to 19 DEG C to 11.5；It is slow added into account for cornstarch dry weight 10% epoxy third
Alkane (175kg), the ethanol solution 130kg of 30% concentration is taken, sprayed by the shower of reactor top, coutroi velocity is
65kg/h, 2h is sprayed, 39 DEG C is then raised temperature to, continues to react.
B. process is monitored：In course of reaction, 100ml reaction materials are taken every 2h, are first adjusted with 10wt% hydrochloric acid solution anti-
The pH of solution should be expected to 6.0, then it is 40 μ s/cm to be washed with distilled water to electrical conductivity, obtains test sample.By dried test
Sample, the amidin 500ml of the concentration of dry matter content 5.5% is reconfigured as, it is water-soluble to detect starch with brabender instrument
Liquid curve, it is 69 DEG C to have obtained pasting temperature, and at a temperature of this plays paste, substitution value is in the range of 0.04-0.045, because target product
Substitution value requirement more than 0.08, continue to react and repeat the step, when rise paste temperature in the range of 62 DEG C -63 DEG C when, this
When substitution value 0.08 or so, can terminating reaction.
C. terminating reaction：Add 10wt% hydrochloric acid solution to adjust the pH to 6.0 of reaction solution, cyclone washing, dehydration, do
Dry, packaging.
Embodiment 3
The present embodiment provides preparation and the production control method of a kind of hydroxypropul starch, it is desirable to which hydroxypropul starch substitution value exists
More than 0.1, its step includes：
A. course of reaction：In retort put into 1.6 tons of corn starch milks, add water degree of thickening into concentration be 40wt% it is water-soluble
Liquid, it is stirring evenly and then adding into 10% sodium chloride (160kg) for accounting for cornstarch dry weight；It is slow added into concentration 5wt% hydrogen
Sodium oxide molybdena, regulation solution ph are cooled to 20 DEG C to 12；It is slow added into 12% expoxy propane for accounting for cornstarch dry weight
(192kg), the ethanol solution 150kg of 50% concentration is taken, sprayed by the shower of reactor top, coutroi velocity 75kg/
H, 2h is sprayed, 40 DEG C is then raised temperature to, continues to react.
B. process is monitored：In course of reaction, 100ml reaction materials are taken every 2h, are first adjusted with 10wt% hydrochloric acid solution anti-
The pH of solution should be expected to 6.5, then it is 43 μ s/cm to be washed with distilled water to electrical conductivity, obtains test sample.By dried test
Sample, the amidin 500ml of the concentration of dry matter content 6% is reconfigured as, amidin is detected with brabender instrument
Curve, it is 65 DEG C to have obtained pasting temperature, and at a temperature of this plays paste, substitution value is 0.06 or so, because the substitution value of target product will
Ask more than 0.10, continue to react and repeat the step, when playing paste temperature at 60 DEG C ± 0.5 DEG C or so, now substitution value exists
0.1 or so, can terminating reaction.
C. terminating reaction：Add 10wt% hydrochloric acid solution to adjust the pH to 6.5 of reaction solution, cyclone washing, dehydration, do
Dry, packaging.
Above-described embodiment shows, using method provided by the invention, can not only be recycled by spraying ethanol solution
The raw material expoxy propane of volatilization, raw material is maximized the use value, avoid wasting, and can accurately make according to demand
The hydroxypropul starch of standby required substitution value, it is important that course of reaction simple operations are convenient, can accomplish to monitor in real time, suitable for appointing
The preparation of the hydroxypropul starch of what substitution value scope.
The general principle and principal character and advantages of the present invention of the present invention has been shown and described above.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the simply explanation described in above-described embodiment and specification is originally
The principle of invention, without departing from the spirit and scope of the present invention, various changes and modifications of the present invention are possible, these changes
Change and improvement all fall within the protetion scope of the claimed invention.
Claims (8)
1. a kind of preparation method of hydroxypropul starch, it is characterised in that comprise the following steps：
(1) corn starch milk is put into retort, adds water, is stirred, the cornstarch aqueous solution is made；
(2) then add sodium chloride；
(3) it is slowly added to sodium hydroxide solution；
(4) it is 18 DEG C -20 DEG C to control temperature of charge in retort, is slowly added to expoxy propane；
(5) ethanol solution is taken, is sprayed by the shower of reactor top, material in retort is warming up to 38 DEG C -40 DEG C, filled
Divide reaction, until terminating, obtain hydroxypropul starch.
2. the preparation method of a kind of hydroxypropul starch according to claim 1, it is characterised in that add in the step (1)
The amount of water is until corn starch milk to be modulated into the 35wt%-40wt% aqueous solution.
3. the preparation method of a kind of hydroxypropul starch according to claim 1, it is characterised in that add in the step (2)
The amount of the sodium chloride entered is the 8%-10% of cornstarch dry weight in corn starch milk.
4. the preparation method of a kind of hydroxypropul starch according to claim 1, it is characterised in that add in the step (3)
The concentration for entering sodium hydroxide solution is 3wt%-5wt%, and the amount of addition is up to pH value of solution to 11-12.
5. the preparation method of a kind of hydroxypropul starch according to claim 1, it is characterised in that characterized in that, described
The amount of the expoxy propane added in step (4) is the 5%-12% of cornstarch dry weight in corn starch milk.
A kind of 6. preparation method of hydroxypropul starch according to claim 1, it is characterised in that second in the step (5)
Alcoholic solution concentration is 10-50%.
A kind of 7. preparation method of hydroxypropul starch according to any one of claim 1 to 6, it is characterised in that step (5)
Described in retort material carry out fully reaction and comprise the following steps：
(5.1) sample, primary first-order equation material is taken into testing tube every the identical period, adjust testing tube reaction mass solution
PH, distill water washing, obtain test sample；
(5.2) test, test sample is configured to the amidin of dry matter content 5%-6% concentration, using brabender instrument
Device detects amidin curve, must play paste temperature, and judge substitution value according to paste temperature is played；
(5.3) reach the pH that material in retort is adjusted after preferable substitution value, washing, dehydration, dry, packaging, obtain required substitution
The hydroxypropul starch of degree.
8. the preparation method of a kind of hydroxypropul starch according to claim 7, it is characterised in that in the step (5.3)
PH value of solution is adjusted to 5.5-6.5, it is 37 μ s/cm-43 μ s/cm to wash to electrical conductivity.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711236953.8A CN107880140A (en) | 2017-11-30 | 2017-11-30 | The preparation method and production control method of a kind of hydroxypropul starch |
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| CN201711236953.8A CN107880140A (en) | 2017-11-30 | 2017-11-30 | The preparation method and production control method of a kind of hydroxypropul starch |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114891843A (en) * | 2022-05-05 | 2022-08-12 | 广西志盛寰宇科技有限公司 | Hydroxypropyl starch resistant dextrin and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101717451A (en) * | 2009-12-18 | 2010-06-02 | 张雷达 | Method for enhancing substitution degree of hydroxypropyl starch |
| CN106832012A (en) * | 2017-03-31 | 2017-06-13 | 山东福洋生物科技有限公司 | A kind of production control method and preparation method of the converted starch of particular characteristic |
| CN107162882A (en) * | 2017-07-04 | 2017-09-15 | 中国科学院过程工程研究所 | Spray column disc type reactor, system and technique with its production propylene glycol monomethyl ether |
-
2017
- 2017-11-30 CN CN201711236953.8A patent/CN107880140A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101717451A (en) * | 2009-12-18 | 2010-06-02 | 张雷达 | Method for enhancing substitution degree of hydroxypropyl starch |
| CN106832012A (en) * | 2017-03-31 | 2017-06-13 | 山东福洋生物科技有限公司 | A kind of production control method and preparation method of the converted starch of particular characteristic |
| CN107162882A (en) * | 2017-07-04 | 2017-09-15 | 中国科学院过程工程研究所 | Spray column disc type reactor, system and technique with its production propylene glycol monomethyl ether |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114891843A (en) * | 2022-05-05 | 2022-08-12 | 广西志盛寰宇科技有限公司 | Hydroxypropyl starch resistant dextrin and preparation method thereof |
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Application publication date: 20180406 |