CN108239170A - A kind of cross-linking modified starch for adding succinic acid diepoxy propyl alcohol ester - Google Patents
A kind of cross-linking modified starch for adding succinic acid diepoxy propyl alcohol ester Download PDFInfo
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- CN108239170A CN108239170A CN201611229791.0A CN201611229791A CN108239170A CN 108239170 A CN108239170 A CN 108239170A CN 201611229791 A CN201611229791 A CN 201611229791A CN 108239170 A CN108239170 A CN 108239170A
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- starch
- succinic acid
- propyl alcohol
- alcohol ester
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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
- C08B31/003—Crosslinking of starch
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Abstract
The invention discloses a kind of cross-linking modified starch for adding succinic acid diepoxy propyl alcohol ester.The preparation method of the starch is:First using banana lily starch as raw material, after dissolving, being gelatinized, it is mixed with the miscella of cyclohexane chloroform, then carries out cross-linking reaction with succinic acid diepoxy propyl alcohol ester crosslinking agent again, finally can obtain a kind of cross-linking modified starch by centrifugation, washing, drying.
Description
Technical field
The present invention relates to a kind of cross-linking modified starch, more particularly to one kind adds succinic acid two using banana lily starch as raw material
Epoxy prapanol ester crosslinking agent prepares the technique of crosslinked starch, belongs to starch Chemical Industry field.
Background technology
Porous-starch is one kind of modified starch, porous to generate very big specific surface area, porous-starch and other adsorbents
It compares, in addition to good absorption property, also with biodegradable, simple production process, characteristics, the quilt such as is widely used
It is widely used in the industries such as food, medical and health, agricultural, papermaking, printing, cosmetics, detergent, adhesive.
At present, native starch is modified and prepares porous-starch and be mainly the following method:First, using machinery
Method, such as pass through the mechanical impacts such as ball-milling technology;Second is that physical method, such as pass through ultrasonic irradiation or spray art;
Third is biochemical method, such as alcohol is denaturalized or sour water solution, in above-mentioned several method, the machines such as ultrasonic irradiation, ball-milling technology
The production cost that tool hits method is higher, is not easy to realize industrial industrialization;And spray-on process and alcohol are denaturalized that be formed is a kind of reality
The popcorn polymer sphere of the heart, suction-operated are only occurred in the rough gully of spherome surface, and adsorbance is than relatively limited;Sour water solution
Method reaction rate under gelatinization point is slower, and degradation differs, and is not easy to be formed poroid.And enzyme degradation technique is used, it is made by adjusting
Standby process conditions and addition suitable adjuvants control spherex grain size and microcellular structure, the modified porous starch specific surface of preparation
Product is big, has wide application prospect.
Enzyme degradation technique method is to form it into porous-starch, but this method can make shallow lake in starch using diastatic action
Powder structure shows as resistance to mechanical destroys force difference, anti-Swelling Capacity weakens etc. by a degree of destruction.In order to make up porous shallow lake
These in powder structure are insufficient, by adding crosslinking agent, carry out chemical modification to it, and the alcoholic extract hydroxyl group of starch molecule is in containing binary
Or the chemical reagent reaction of polynary functional group, make to join together to form sediment so as to prepare a kind of crosslinking between the hydroxyl of different starch molecules
Powder, the present invention is using banana lily starch as raw material, by adding succinic acid diepoxy propyl alcohol ester crosslinking agent, to the porous-starch of preparation into
Row crosslinking, the relative molecular mass of porous-starch becomes larger after crosslinking, influences have high stability to heat, acid and shearing force.
Invention content
The object of the present invention is to provide one kind using banana lily starch as raw material, addition crosslinking agent prepares the technique of crosslinked starch,
Its step of preparation process is as follows:
(1) suitable banana lily starch is taken to add a certain amount of distilled water, heating for dissolving is configured to starch solution as raw material first;
(2) a certain amount of NaOH solution is added in after dissolving, and adjusting PH makes solution be in for alkalescent;
(3) the heating of above-mentioned solution is fully gelatinized;
(4) a certain proportion of cyclohexane chloroform mixing is taken to be made into oil phase, and heated under constant agitation again,
It is to be emulsified completely after, mixed with above-mentioned starch solution, and be uniformly dispersed;
(5) after being uniformly dispersed, add in succinic acid diepoxy propyl alcohol ester and carry out cross-linking reaction, and be stirred continuously carry out cross-linking reaction;
(6) fully after reaction, the solution after reaction is centrifuged;
(7) upper solution is removed after centrifuging, and lower sediment acetone, absolute ethyl alcohol wash for several times repeatedly;
(8) finally it is dried at a certain temperature, up to a kind of edible canna crosslinked starch after drying.
Preferentially, step (1) in, mode of heating is heating water bath, and heating and temperature control is at 40-60 DEG C.
Preferentially, step (1) in, the starch quality score of the starch solution of preparation is 5%-10%.
Preferentially, step (2) in, the NaOH solution solubility of addition is 0.1-0.5mol/L, and the pH controls for adjusting solution are 9-
11。
Preferentially, step (3) in, mode of heating is heating water bath, and heating and temperature control is in 70-90 DEG C, heating time
30-60min。
Preferentially, step (4) in, the volume mixture ratio of cyclohexane chloroform is 4:1, mode of heating adds for water-bath
Heat, heating and temperature control is at 40-60 DEG C.
Preferentially, step (5) in, the adding proportion of succinic acid diepoxy propyl alcohol ester is the 1-2% of starch quality, cross-linking reaction
Between 3-5h.
Preferentially, step (8) in, drying temperature control is 40-60 DEG C.
The present invention has following advantages and characteristic:
(1) the crosslinked starch stability prepared is good;
(2) preparation process is simple, easy to operate;
(3) abundant raw material, it is cheap.
Specific embodiment
Embodiment one:
5g banana lily starches are taken first as raw material, addition 95ml distilled water is dissolved, and place it in 60 DEG C of environment into
Row heating water bath is configured to starch solution, then adds the NaOH solution of 0.1mol/L, and the PH for making solution is 9, then by solution
The heating water bath 60min under the conditions of 70 DEG C, and be stirred continuously with blender, amylum body is made to be swollen in water, is divided, is formed uniformly
Paste starch solution.The hexamethylene and the mixing of 40ml chloroforms for taking 10ml again are made into oil phase, and constantly stirred under the conditions of 60 DEG C
Mix mixing, it is to be emulsified completely after, mix with prepared starch solution, and be constantly stirred, after being uniformly dispersed, addition
The succinic acid diepoxy propyl alcohol ester of 0.1g carries out cross-linking reaction, and is stirred continuously, and centrifuges reactant after reacting 3h, removes
Upper solution, lower sediment carry out washing 1 time with acetone, are then washed 1 time with absolute ethyl alcohol, be finally placed in washed product again
It is dried under the conditions of 60 DEG C, a kind of cross-linking modified starch can be obtained after dry.
Embodiment two:
Taking 10g banana lily starches first, addition 190ml distilled water is dissolved, and place it in 50 DEG C of environment as raw material
Heating water bath is carried out, is configured to starch solution, then adds the NaOH solution of 0.3mol/L, the PH for making solution is 10, then will
Solution heating water bath 40min under the conditions of 80 DEG C, and be stirred continuously with blender, amylum body is made to be swollen in water, divide, is formed
Homogeneous paste starch solution.The hexamethylene and the mixing of 80ml chloroforms for taking 20ml again are made into oil phase, and under the conditions of 50 DEG C not
It is disconnected to be stirred, it is to be emulsified completely after, mix with prepared starch solution, and be constantly stirred, after being uniformly dispersed, add
The succinic acid diepoxy propyl alcohol ester for entering 0.2g carries out cross-linking reaction, and be stirred continuously, and centrifuges reactant after reacting 4h, goes
Except upper solution, lower sediment carries out washing 1 time with acetone, is then washed 1 time with absolute ethyl alcohol, finally puts washed product again
It is dried under the conditions of 50 DEG C, a kind of cross-linking modified starch can be obtained after dry.
Embodiment three:
Taking 50g banana lily starches first, addition 950ml distilled water is dissolved, and place it in 40 DEG C of environment as raw material
Heating water bath is carried out, is configured to starch solution, then adds the NaOH solution of 0.5mol/L, the PH for making solution is 11, then will
Solution heating water bath 30min under the conditions of 90 DEG C, and be stirred continuously with blender, amylum body is made to be swollen in water, divide, is formed
Homogeneous paste starch solution.The hexamethylene and the mixing of 400ml chloroforms for taking 100ml again are made into oil phase, and under the conditions of 40 DEG C
Be stirred continuously mixing, it is to be emulsified completely after, mixed with prepared starch solution, and be constantly stirred, after being uniformly dispersed,
The succinic acid diepoxy propyl alcohol ester for adding in 0.5g carries out cross-linking reaction, and be stirred continuously, and centrifuges reactant after reacting 3h,
Upper solution is removed, lower sediment carries out washing 1 time with acetone, then washed 1 time with absolute ethyl alcohol again, finally by washed product
It is dried under the conditions of being placed in 40 DEG C, a kind of cross-linking modified starch can be obtained after dry.
Claims (8)
- A kind of 1. cross-linking modified starch for adding succinic acid diepoxy propyl alcohol ester, it is characterised in that the preparation work of cross-linking modified starch Skill carries out as follows:(1) suitable banana lily starch is taken to add a certain amount of distilled water, heating for dissolving is configured to starch solution as raw material first;(2) a certain amount of NaOH solution is added in after dissolving, and adjusting PH makes solution be in for alkalescent;(3) the heating of above-mentioned solution is fully gelatinized;(4) a certain proportion of cyclohexane chloroform mixing is taken to be made into oil phase, and heated under constant agitation again, It is to be emulsified completely after, mixed with above-mentioned starch solution, and be uniformly dispersed;(5) after being uniformly dispersed, add in succinic acid diepoxy propyl alcohol ester and carry out cross-linking reaction, and be stirred continuously carry out cross-linking reaction;(6) fully after reaction, the solution after reaction is centrifuged;(7) upper solution is removed after centrifuging, and lower sediment acetone, absolute ethyl alcohol wash for several times repeatedly;(8) finally it is dried at a certain temperature, up to a kind of edible canna crosslinked starch after drying.
- A kind of 2. cross-linking modified starch for adding succinic acid diepoxy propyl alcohol ester as described in claim 1, which is characterized in that step Suddenly (1) in, mode of heating is heating water bath, and heating and temperature control is at 40-60 DEG C.
- A kind of 3. cross-linking modified starch for adding succinic acid diepoxy propyl alcohol ester as described in claim 1, which is characterized in that step Suddenly (1) in, the starch quality score of the starch solution of preparation is 5%-10%.
- A kind of 4. cross-linking modified starch for adding succinic acid diepoxy propyl alcohol ester as described in claim 1, which is characterized in that step Suddenly (2) in, the NaOH solution solubility of addition is 0.1-0.5mol/L, and the pH controls for adjusting solution are 9-11.
- A kind of 5. cross-linking modified starch for adding succinic acid diepoxy propyl alcohol ester as described in claim 1, which is characterized in that step Suddenly (3) in, mode of heating is heating water bath, and heating and temperature control is at 70-90 DEG C, heating time 30-60min.
- A kind of 6. cross-linking modified starch for adding succinic acid diepoxy propyl alcohol ester as described in claim 1, which is characterized in that step Suddenly (4) in, the volume mixture ratio of cyclohexane chloroform is 4:1.
- A kind of 7. cross-linking modified starch for adding succinic acid diepoxy propyl alcohol ester as described in claim 1, which is characterized in that step Suddenly (5) in, the adding proportion of succinic acid diepoxy propyl alcohol ester is the 1-2% of starch quality, and cross-linking reaction is between 3-5h.
- A kind of 8. cross-linking modified starch for adding succinic acid diepoxy propyl alcohol ester as described in claim 1, which is characterized in that step Suddenly (8) in, drying temperature control is 40-60 DEG C.
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Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105384834A (en) * | 2015-12-15 | 2016-03-09 | 陈虹 | Preparation technology of water chestnut starch succinate |
CN105504074A (en) * | 2015-12-12 | 2016-04-20 | 廖芳 | Method for preparing crosslinked starch through succinic acid diepoxide propyl ester |
-
2016
- 2016-12-27 CN CN201611229791.0A patent/CN108239170A/en active Pending
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105504074A (en) * | 2015-12-12 | 2016-04-20 | 廖芳 | Method for preparing crosslinked starch through succinic acid diepoxide propyl ester |
CN105384834A (en) * | 2015-12-15 | 2016-03-09 | 陈虹 | Preparation technology of water chestnut starch succinate |
Non-Patent Citations (3)
Title |
---|
刘晓恒: ""新型交联剂合成玉米淀粉微球的工艺及应用研究"", 《中国学位论文全文数据库》 * |
刘晓桓等: ""肠用载药淀粉微球的合成及性能研究"", 《陕西科技大学学报(自然科学版)》 * |
李新华等: ""淀粉微球合成条件的研究"", 《粮油食品科技》 * |
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