CN109957034A - A kind of method of dry process octenyl succinic acid anhydride modified starch - Google Patents
A kind of method of dry process octenyl succinic acid anhydride modified starch Download PDFInfo
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- CN109957034A CN109957034A CN201711335071.7A CN201711335071A CN109957034A CN 109957034 A CN109957034 A CN 109957034A CN 201711335071 A CN201711335071 A CN 201711335071A CN 109957034 A CN109957034 A CN 109957034A
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- starch
- succinic acid
- acid anhydride
- octenyl succinic
- sodium
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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
- C08B31/02—Esters
- C08B31/04—Esters of organic acids, e.g. alkenyl-succinated starch
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- Life Sciences & Earth Sciences (AREA)
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- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
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- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention discloses a kind of method of dry process octenyl succinic acid anhydride modified starch, includes the following steps: to mix in a certain amount of starch, catalyst, octenyl succinic acid anhydride, dispersing agent and alkali, add water to moisture content and reach 18-25wt%；The mixed liquor of acquisition is sent into extruder and carries out extruding reaction；By extruded product, constant temperature and humidity reacts 6-8h at 40-50 DEG C, then dries；Desciccate is washed with volatile organic solvent, obtains the octenyl succinic acid anhydride modified starch after dried, crushed.The present invention utilizes the high temperature of extruder, high pressure, Strong shear power, improve reaction reagent and starch molecule degree of mixing, the starch chemical activity point of increase and interior shifting, breakthrough dry production converted starch mix uneven, product there are chemical reagent and starch and dissolve the technical problems such as difference.Products obtained therefrom has higher grafting rate and reaction efficiency, has production cost low, and simple operation and other advantages have good application value.
Description
Technical field
The present invention relates to field of starch modification, and in particular to the method for dry process octenyl succinic acid anhydride modified starch.
Background technique
Octenyl succinic acid anhydride modified starch is with octenyl succinic acid anhydride and starch through made from esterification, usually with
The form of starch ester or sodium starch occurs.With the modified starch of octenyl succinic acid anhydride, because with starch and octenyl amber
The property of amber acid groups has and is widely applied, and is a kind of excellent converted starch.
Octenyl succinic acid anhydride modified starch can use dry production at present, but dry production converted starch has chemistry
The technical problems such as reagent and uneven, the product dissolution difference of starch mixing.
Summary of the invention
The object of the present invention is to provide a kind of methods of dry process octenyl succinic acid anhydride modified starch, to solve background
Drawbacks described above existing for technology.
The present invention realizes by the following technical solutions:
A kind of method of dry process octenyl succinic acid anhydride modified starch, includes the following steps:
A certain amount of starch, catalyst, octenyl succinic acid anhydride, dispersing agent and alkali are mixed, add water to moisture by step 1
Content reaches 18-25wt%；
The mixed liquor that step 1 obtains is sent into extruder and carries out extruding reaction by step 2；
Step 3, the extruded product that step 2 is obtained constant temperature and humidity at 40-50 DEG C reacts 6-8h, then in same temperature
Spend lower drying；
The desciccate that step 3 obtains is washed with volatile organic solvent, obtains institute after dried, crushed by step 4
State octenyl succinic acid anhydride modified starch.
The mass content of each component is as follows as a preferred technical solution:
As a preferred technical solution, in step 2, extruding reaction is in 140-185 DEG C of jacket temperature, revolving speed 100-
It is carried out under 200r/min, product is extruded by the hole of diameter 0.01m.
As a preferred technical solution, in step 4, volatile organic solvent preferred alcohol, preferably 70% ethyl alcohol is molten
Liquid, to remove remaining reactant and further remove moisture.
The alkali is alkaline matter commonly used in the art, such as sodium hydroxide.
The starch is tapioca as a preferred technical solution, and partial size is less than 100 mesh.
As a preferred technical solution, the catalyst be selected from sodium bicarbonate, sodium carbonate, disodium hydrogen phosphate, sodium acetate and
Any one or a few in calcium hydroxide.
The dispersing agent is any in sodium chloride, potassium chloride, sodium sulphate and potassium sulfate as a preferred technical solution,
It is one or more of.
As a preferred technical solution, in step 4, product adds 1-2 portions of glidants after crushed.
The glidant is silica and bentonitic one or two as a preferred technical solution,.
The present invention using the high temperature of extruder, high pressure, Strong shear power effect to starch submicron particle " film ", " band or
The destruction of wall " and starch crystal dislocation is acted on, improve reaction reagent and starch molecule degree of mixing, increased and the shallow lake of interior shifting
Dusting active site, breaking through dry production converted starch, there are chemical reagent and starch to mix uneven, product dissolution difference etc.
Technical problem.Products obtained therefrom has higher grafting rate and reaction efficiency, has production cost low, simple operation and other advantages, tool
There is good application value.
Specific embodiment
The present invention is illustrated below by specific embodiment, but is not intended to limit the present invention.
Embodiment 1:
1. by mass, by 100 parts of starch, 5 parts of sodium bicarbonates, 2 parts of octenyl succinic acid anhydrides, 6 parts of sodium chloride, 1 part of alkali
Liquid is uniformly mixed in a high speed mixer, and moisturizing to moisture content is 18-25%.
2. 145 DEG C of control sleeve temperature and revolving speed 150r/min, start extruding reaction, sample passes through the hole diameter 0.01m quilt
It squeezes out.
3. extruded product constant temperature and humidity under the conditions of 40 DEG C reacts 8h, then dry under the conditions of 40 DEG C.
4. the ethanol solution with 70% washs 2-3 times, then product is put into 45 DEG C of baking oven and is dried, crushed, is added 2
Part silica, it is spare.
Embodiment 2:
1. by mass, 100 parts of starch, 5 sodium carbonate, 2 parts of octenyl succinic acid anhydrides, 5 parts of potassium chloride, 1 part of lye are existed
It is uniformly mixed in high-speed mixer, moisturizing to moisture content is 18-25%.
2. 155 DEG C of control sleeve temperature and revolving speed 175r/min, start extruding reaction, sample passes through the hole diameter 0.01m quilt
It squeezes out.
3. extruded product constant temperature and humidity under the conditions of 40 DEG C reacts 8h, then dry under the conditions of 40 DEG C.
4. the ethanol solution with 70% washs 2-3 times, then product is put into 45 DEG C of baking oven and is dried, crushed, is added 2
Part silica, it is spare.
Embodiment 3:
1. by mass, by 100 parts of starch, 5 parts of disodium hydrogen phosphates, 2 parts of octenyl succinic acid anhydrides, 5 parts of sodium sulphate, 1 part
Lye is uniformly mixed in a high speed mixer, and moisturizing to moisture content is 18-25%.
2. 165 DEG C of control sleeve temperature and revolving speed 180r/min, start extruding reaction, sample passes through the hole diameter 0.01m quilt
It squeezes out.
3. extruded product constant temperature and humidity under the conditions of 40 DEG C reacts 8h, then dry under the conditions of 40 DEG C.
4. the ethanol solution with 70% washs 2-3 times, then product is put into 45 DEG C of baking oven and is dried, crushed, is added 1
Part bentonite, it is spare.
Embodiment 4:
1. by mass, by 100 parts of starch, 3-5 parts of sodium acetates, 2 parts of octenyl succinic acid anhydrides, 5 parts of potassium sulfates, 1 part of alkali
Liquid is uniformly mixed in a high speed mixer, and moisturizing to moisture content is 18-25%.
2. 175 DEG C of control sleeve temperature and revolving speed 150r/min, start extruding reaction, sample passes through the hole diameter 0.01m quilt
It squeezes out.
3. extruded product constant temperature and humidity under the conditions of 40 DEG C reacts 8h, then dry under the conditions of 40 DEG C.
4. the ethanol solution with 70% washs 2-3 times, then product is put into 45 DEG C of baking oven and is dried, crushed, is added 1
Part bentonite, it is spare.
Comparative example:
Using the succinate modified starches of Aqueous phase preparation as comparative sample, compared with the degree of substitution of embodiment and reaction efficiency
Compared with.Aqueous phase prepares octenyl succinic acid anhydride modified starch: will contain 2% sodium chloride of starch quality and the dry para arrowroot of 10.0g
Powder is made into the starch milk that mass fraction is 40%, 30 DEG C of thermostatic control, then adjusts starch milk pH with 3% sodium hydrate aqueous solution
Value, is added portionwise 4% octenyl succinic acid anhydride of starch quality, while keeping pH value of starch milk constant.After reaction, hydrochloric acid is used
Neutralization reaction mixture using centrifugation, washing, drying, crushing, is sieved to pH value 6-7 up to product.
The substituted par of hydroxyl on degree of substitution, that is, each dehydrated glucose unit, octenyl succinic acid anhydride is modified to form sediment
The measurement of powder substituent group carries out detection esterification starch degree of substitution (DS) and reaction efficiency (RE) calculation formula using acid-base titration
It is as follows:
In formula: M-sample octenyl succinic acid anhydride acyl group percentage composition (%)；
V0And V1The volume (mL) of-ative starch and the consumed hydrochloric acid of esterification starch；
N-standard hydrochloric acid solution concentration (mol/L)；
W-esterification starch quality (g)；
The mass fraction of 162-glucose units；
210-octenyl succinic acid anhydride acyl moieties amounts；
10000=100 × octenyl succinic acid anhydride acyl group mass fraction；
Measurement result is as shown in table 1:
Table 1
The result shows that the present invention, under identical octenyl succinic acid anhydride dosage, product has higher grafting rate and reaction
Efficiency.
The above shows and describes the basic principle, main features and advantages of the invention.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this
The principle of invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these changes
Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its
Equivalent thereof.
Claims (10)
1. a kind of method of dry process octenyl succinic acid anhydride modified starch, which comprises the steps of:
A certain amount of starch, catalyst, octenyl succinic acid anhydride, dispersing agent and alkali are mixed, add water to moisture content by step 1
Reach 18-25wt%；
The mixed liquor that step 1 obtains is sent into extruder and carries out extruding reaction by step 2；
Step 3, the extruded product that step 2 is obtained constant temperature and humidity at 40-50 DEG C react 6-8h, then at the same temperature
It is dry；
The desciccate that step 3 obtains is washed with volatile organic solvent, is obtained after dried, crushed described pungent by step 4
Alkenyl succinic anhydride modified starch.
2. the method as described in claim 1, which is characterized in that the parts by weight of each component are as follows:
3. the method as described in claim 1, which is characterized in that in step 2, extruding reaction is in jacket temperature 140-185
DEG C, carry out under revolving speed 100-200r/min, product is extruded by the hole of diameter 0.01m.
4. the method as described in claim 1, which is characterized in that in step 4, the volatile organic solvent is ethyl alcohol.
5. method as claimed in claim 4, which is characterized in that the volatile organic solvent is that the ethyl alcohol of 70wt% is water-soluble
Liquid.
6. the method as described in claim 1, which is characterized in that the starch is tapioca, and partial size is less than 100 mesh.
7. the method as described in claim 1, which is characterized in that the catalyst is selected from sodium bicarbonate, sodium carbonate, phosphoric acid hydrogen two
Any one or a few in sodium, sodium acetate and calcium hydroxide.
8. the method as described in claim 1, which is characterized in that the dispersing agent is selected from sodium chloride, potassium chloride, sodium sulphate and sulphur
Any one or a few in sour potassium.
9. the method as described in claim 1, which is characterized in that in step 4, product adds 1-2 parts after crushed and helps stream
Agent.
10. method as claimed in claim 9, which is characterized in that the glidant be silica and it is bentonitic a kind of or
Two kinds.
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| CN201711335071.7A CN109957034A (en) | 2017-12-14 | 2017-12-14 | A kind of method of dry process octenyl succinic acid anhydride modified starch |
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| CN201711335071.7A CN109957034A (en) | 2017-12-14 | 2017-12-14 | A kind of method of dry process octenyl succinic acid anhydride modified starch |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113150458A (en) * | 2021-05-08 | 2021-07-23 | 浙江三和塑料有限公司 | Preparation method of baking-free high-strength bearing belt material |
| CN115211566A (en) * | 2022-03-23 | 2022-10-21 | 东北农业大学 | Method for preparing olive oil microcapsules by microfluidization of Pickering o/w emulsion |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101624423A (en) * | 2009-08-03 | 2010-01-13 | 甘肃圣大方舟马铃薯变性淀粉有限公司 | Method for preparing starch octenyl succinate anhydride |
| CN105837696A (en) * | 2016-06-20 | 2016-08-10 | 上海东升新材料有限公司 | Method for preparing succinic acid modified cassava starch by dry method |
| CN105859897A (en) * | 2016-06-20 | 2016-08-17 | 上海东升新材料有限公司 | Preparation method of succinic acid modified cassava starch |
-
2017
- 2017-12-14 CN CN201711335071.7A patent/CN109957034A/en not_active Withdrawn
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101624423A (en) * | 2009-08-03 | 2010-01-13 | 甘肃圣大方舟马铃薯变性淀粉有限公司 | Method for preparing starch octenyl succinate anhydride |
| CN105837696A (en) * | 2016-06-20 | 2016-08-10 | 上海东升新材料有限公司 | Method for preparing succinic acid modified cassava starch by dry method |
| CN105859897A (en) * | 2016-06-20 | 2016-08-17 | 上海东升新材料有限公司 | Preparation method of succinic acid modified cassava starch |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113150458A (en) * | 2021-05-08 | 2021-07-23 | 浙江三和塑料有限公司 | Preparation method of baking-free high-strength bearing belt material |
| CN115211566A (en) * | 2022-03-23 | 2022-10-21 | 东北农业大学 | Method for preparing olive oil microcapsules by microfluidization of Pickering o/w emulsion |
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