CN104017094B - A kind of continuous feeding legal system is for the method for carboxymethyl Starch rice - Google Patents
A kind of continuous feeding legal system is for the method for carboxymethyl Starch rice Download PDFInfo
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Abstract
The invention discloses the method for a kind of continuous feeding legal system for carboxymethyl Starch rice.Take Starch rice as raw material, aqueous isopropanol is reaction medium, add NaOH and catalyzer makes starch alkalize, drip continuously within a certain period of time and be mixed with a certain amount of chloroacetic Virahol mixed solution, and in etherification procedure, keep the alkaline environment of system, optionally regulate stirring velocity, control temperature of reaction and time.After reaction terminates, cooling, adjust pH, suction filtration, washing, is dried to constant weight, sieves.The present invention takes continuous feeding to drip the Mono Chloro Acetic Acid be dissolved in Virahol in the process of Starch rice etherificate, and in reaction process, regulate stirring velocity and keep the alkaline environment of reaction system to replace once adding reactant Mono Chloro Acetic Acid, improve the stability of reaction system, ensure that reaction is normally carried out, efficiently solve in reaction process and cause conglomeration problem because viscosity increases too fast, obtained carboxymethyl starch substitution value (DS) can reach 0.76.
Description
Technical field
The present invention relates to a kind of preparation method of carboxymethyl Starch rice.
Technical background
Rice is one of topmost grain variety of China, and starch is the main component of rice, and content reaches more than 90%.Although three of starch industry large raw materials are corn, wheat and potato, rice starch only accounts for 13%.Cracking rice is the inevitable by product produced in the rice course of processing, and be used as feed for a long time, comprehensive utilization ratio is lower.Crack rice substantially identical with the main component of rice, but price is more cheap than rice many, starch is its main component.Rice starch, but because of the character and utilization of its uniqueness, has good market outlook.Starch and its derivative are used in food and non-food product processing usually.But, containing the complex region such as crystallization, amorphous in native starch particles, in starch molecular structure, Hydrogen bonding forces is strong, has very strong resistivity to media such as water, cause that starch poor mechanical property, dispersiveness are strong, seepage force is weak, make its directly application be subject to many restrictions.And starch can obtain the derivative of different properties after the physics such as damp and hot, acidolysis, oxidation, esterification, etherificate, grafting or chemical process denaturing treatment.Carboxymethyl starch is one of principal item of modified starch, it is soluble in water, have good dispersion force and bonding force, water-absorbent and water swellability are strong, viscosity is high, adhesion is strong, emulsifying property is good, not easily corruption go mouldy, stable chemical performance, have broad application prospects in industries such as weaving, papermaking, food, process hides, medicine, metallurgy, petroleum drilling, washing composition.China's carboxymethyl starch ultimate production in 2007 only accounts for 0.07% of modified starch.Therefore, research and develop carboxymethyl starch and there is important commercial value.
The research of carboxymethyl starch starts from nineteen twenty-four, and the development of China's carboxymethyl starch starts from the mid-80 in last century.Through the development of nearly 20 years, although China's carboxymethyl starch industry obtains tremendous development, and have been reported with wheat starch, W-Gum, tapioca (flour) research, but the research of carboxymethyl starch is also in the primary stage, and especially the carboxymethyl modified research of Starch rice is not yet reported.Just because of the high crystalline of Starch rice and particle tiny, its reaction system viscosity after adding Mono Chloro Acetic Acid is caused to increase too fast, starch in reactor is easy to form floc sedimentation, cause reaction system unstable, finally make substitution value low, reaction terminates after product and is difficult to cleaning, drying, sometimes can not get qualified carboxymethyl starch product even at all.
Summary of the invention
, reaction system viscosity unstable to reaction system in new Raw Materials Rice starch carboxymethyl-modification process for existing technology hydrophily method increases too fast, conglomeration problem and causes the problems such as products collection efficiency is low, reaction can not normally be carried out, substitution value is not high, the invention provides the method for a kind of continuous feeding legal system for carboxymethyl Starch rice.
The technical solution adopted in the present invention is:
Continuous feeding legal system, for a method for rice carboxymethyl starch, comprises the steps:
(1) take Starch rice as raw material, aqueous isopropanol is reaction medium, according to the mass fraction, 45 ~ 60 parts of NaOH and 4 ~ 7 part catalyzer are added in 100 parts of Starch rices, pour 1200 ~ 1250 parts of aqueous isopropanols into, and 50 ~ 60 parts of distilled water, stirring velocity is 200 ~ 250r/min, in the water-bath of 50 DEG C, abundant stirring heating 30 ~ 40min, fully alkalizes to make starch;
(2) after being warming up to 60 DEG C, add total 50 ~ 200 parts as follows and be mixed with 40 ~ 90 portions of chloroacetic Virahol mixed solutions, first will wherein 20 ~ 50 portions of mixed solutions be disposable adds, adjust agitator 300 ~ 600r/min immediately and stir 5 ~ 15min, regulate agitator stirring velocity to 200 ~ 300r/min, then reaction 15 ~ 30min is continued, residual mixed liquor is dripped continuously in 40 ~ 120min, after dripping, continue reaction for some time, control total etherification time at 180 ~ 210min.In reaction process, NaOH particle should be added to keep the reaction environment of alkalescence in reaction system.After reaction 180 ~ 210min, be cooled to room temperature, with Glacial acetic acid adjust pH to 6.5 ~ 7.0, filter, the filter cake ethanolic soln washes clean of 90% ~ 95% volume fraction, is dried to constant weight in 45 DEG C ~ 55 DEG C baking ovens, grinding, and sieve with 80 object sieves.
Above-mentioned continuous feeding legal system is for the method for rice carboxymethyl starch, and described Starch rice is the separation Starch rice that market is bought, substantially not containing crude protein.Described catalyzer is cetyl trimethylammonium bromide, it can combine with the ion in aqueous phase, and utilizes self to the affinity of organic solvent, by the reactant transfer in aqueous phase in organic phase, impel reaction to occur, accelerate the speed of response of heterogeneous organic reaction.
Above-mentioned continuous feeding legal system is for the method for rice carboxymethyl starch, and described alkalinization completes and is warming up to the etherification reaction temperature time and is not counted in the etherification reaction time, and this temperature-rise period approximately needs 10min.
Above-mentioned continuous feeding legal system is for the method for rice carboxymethyl starch, drip the overwhelming majority in described method within a certain period of time continuously and be mixed with chloroacetic Virahol mixed solution, adopt constant pressure funnel slowly to drip, the half the time that the speed of dropping starts be the 1.1-1.3 of half the time below doubly.
Above-mentioned continuous feeding legal system for the method for rice carboxymethyl starch, the alkaline environment in described maintenance reaction process be between section add sodium hydrate particle, and by accurate pH detection paper, the pH of reaction system is remained between 7 ~ 8.
Beneficial effect of the present invention is:
(1) preparation method of the present invention, in the process of Starch rice etherificate, take continuous feeding to drip the Mono Chloro Acetic Acid be dissolved in Virahol, and in reaction process, regulate stirring velocity and keep the alkaline environment of reaction system to replace once adding reactant Mono Chloro Acetic Acid, improve the stability of reaction system significantly, reaction is normally carried out, efficiently solve in reaction process and cause conglomeration problem because viscosity increases too fast, obtained carboxymethyl starch substitution value (DS) can reach more than 0.70, and its substitution value can adjust between 0.4 ~ 0.76 according to demand and compare be easier to control.
(2) preparation method of the present invention has simple, reacts more stable, product substitution value high, and the deep processing that can be Starch rice provides a kind of new method.
Accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention.
Fig. 2 is major experimental equipment drawing of the present invention.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in further details, but the present invention is not limited to this.
Embodiment 1
According to the mass fraction, 55 parts of NaOH and 6 part catalyzer cetyl trimethylammonium bromide is added in 100 parts of Starch rices, pour 1200 parts of aqueous isopropanols and 55 parts of distilled water into, stirring velocity is 200r/min abundant stirring heating 35min in the water-bath of 50 DEG C, fully alkalize to make starch, then after being warming up to 60 DEG C, then add total 150 parts as follows and be mixed with 80 portions of chloroacetic Virahol mixed solutions, first will wherein 35 portions of mixed solutions be disposable adds, adjust agitator 500r/min immediately and stir 5min, regulate agitator stirring velocity to 300r/min, after continuing reaction 15min, add 10 parts of NaOH particles to keep the reaction environment of alkalescence, then after continuing reaction 15min, residual mixed liquor is dripped continuously in 100min, the speed that the first half time drips is 1.2 times of the later half time, in order to keep the reaction environment of alkalescence, when 1/3 time of beginning dripped and 2/3 time time add 10 parts of NaOH particles.After dripping, continue reaction for some time, control total etherification time at 200min.After reaction terminates, be cooled to room temperature, with Glacial acetic acid adjust pH to 7.0, filter, the filter cake ethanolic soln washes clean of 95% volume fraction, is dried to constant weight in 45 DEG C of baking ovens, grinding, and sieves with 80 object sieves.Obtained carboxymethyl starch substitution value (DS) is 0.73.
Embodiment 2
According to the mass fraction, 55 parts of NaOH and 5 part catalyzer cetyl trimethylammonium bromide is added in 100 parts of Starch rices, pour 1250 parts of aqueous isopropanols and 45 parts of distilled water into, stirring velocity is 250r/min abundant stirring heating 30min in the water-bath of 50 DEG C, fully alkalize to make starch, then after being warming up to 60 DEG C, then add total 120 parts as follows and be mixed with 70 portions of chloroacetic Virahol mixed solutions, first will wherein 30 portions of mixed solutions be disposable adds, adjust agitator 400r/min immediately and stir 10min, regulate agitator stirring velocity to 300r/min, after continuing reaction 15min, add 10 parts of NaOH particles to keep the reaction environment of alkalescence, then after continuing reaction 10min, residual mixed liquor is dripped continuously in 90min, the speed that the first half time drips is 1.1 times of the later half time, in order to keep the reaction environment of alkalescence, when 1/3 time of beginning dripped and 2/3 time time add 10 parts and 5 parts of NaOH particles respectively.After dripping, continue reaction for some time, control total etherification time at 180min.After reaction terminates, be cooled to room temperature, with Glacial acetic acid adjust pH to 7.0, filter, the filter cake ethanolic soln washes clean of 95% volume fraction, is dried to constant weight in 50 DEG C of baking ovens, grinding, and sieves with 80 object sieves.Obtained carboxymethyl starch substitution value (DS) is 0.59.
Embodiment 3
According to the mass fraction, 60 parts of NaOH and 7 part catalyzer cetyl trimethylammonium bromide is added in 100 parts of Starch rices, pour 1200 parts of aqueous isopropanols and 55 parts of distilled water into, stirring velocity is 250r/min abundant stirring heating 35min in the water-bath of 50 DEG C, fully alkalize to make starch, then after being warming up to 60 DEG C, then add total 160 parts as follows and be mixed with 85 portions of chloroacetic Virahol mixed solutions, first will wherein 40 portions of mixed solutions be disposable adds, adjust agitator 450r/min immediately and stir 10min, regulate agitator stirring velocity to 350r/min, after continuing reaction 10min, add 10 parts of NaOH particles to keep the reaction environment of alkalescence, then after continuing reaction 10min, residual mixed liquor is dripped continuously in 110min, the speed that the first half time drips is 1.1 times of the later half time, in order to keep the reaction environment of alkalescence, when 1/3 time of beginning dripped and 2/3 time time add 10 parts of NaOH particles.After dripping, continue reaction for some time, control total etherification time at 200min.After reaction terminates, be cooled to room temperature, with Glacial acetic acid adjust pH to 7.0, filter, the filter cake ethanolic soln washes clean of 95% volume fraction, is dried to constant weight in 45 DEG C of baking ovens, grinding, and sieves with 80 object sieves.Obtained carboxymethyl starch substitution value (DS) is 0.76.
Embodiment 4
According to the mass fraction, 50 parts of NaOH and 6 part catalyzer cetyl trimethylammonium bromide is added in 100 parts of Starch rices, pour 1200 parts of aqueous isopropanols and 55 parts of distilled water into, stirring velocity is 200r/min abundant stirring heating 35min in the water-bath of 50 DEG C, fully alkalize to make starch, then after being warming up to 60 DEG C, then add total 100 parts as follows and be mixed with 60 portions of chloroacetic Virahol mixed solutions, first will wherein 25 portions of mixed solutions be disposable adds, adjust agitator 400r/min immediately and stir 10min, regulate agitator stirring velocity to 300r/min, after continuing reaction 10min, add 10 parts of NaOH particles to keep the reaction environment of alkalescence, then after continuing reaction 10min, residual mixed liquor is dripped continuously in 120min, the speed that the first half time drips is 1.2 times of the later half time, in order to keep the reaction environment of alkalescence, when 1/3 time of beginning dripped and 2/3 time time add 10 parts of NaOH particles.After dripping, continue reaction for some time, control total etherification time at 200min.After reaction terminates, be cooled to room temperature, with Glacial acetic acid adjust pH to 6.7, filter, the filter cake ethanolic soln washes clean of 95% volume fraction, is dried to constant weight in 50 DEG C of baking ovens, grinding, and sieves with 80 object sieves.Obtained carboxymethyl starch substitution value (DS) is 0.49.
Embodiment 5
According to the mass fraction, 50 parts of NaOH and 6 part catalyzer cetyl trimethylammonium bromide is added in 100 parts of Starch rices, pour 1250 parts of aqueous isopropanols and 55 parts of distilled water into, stirring velocity is 250r/min abundant stirring heating 30min in the water-bath of 50 DEG C, fully alkalize to make starch, then after being warming up to 60 DEG C, then add total 100 parts as follows and be mixed with 50 portions of chloroacetic Virahol mixed solutions, first will wherein 40 portions of mixed solutions be disposable adds, adjust agitator 400r/min immediately and stir 15min, regulate agitator stirring velocity to 300r/min, after continuing reaction 10min, add 10 parts of NaOH particles to keep the reaction environment of alkalescence, then after continuing reaction 10min, residual mixed liquor is dripped continuously in 80min, the speed that the first half time drips is 1.3 times of the later half time, in order to keep the reaction environment of alkalescence, when 1/3 time of beginning dripped and 2/3 time time add 10 parts and 5 parts of NaOH particles respectively.After dripping, continue reaction for some time, control total etherification time at 200min.After reaction terminates, be cooled to room temperature, with Glacial acetic acid adjust pH to 6.8, filter, the filter cake ethanolic soln washes clean of 95% volume fraction, is dried to constant weight in 45 DEG C of baking ovens, grinding, and sieves with 80 object sieves.Obtained carboxymethyl starch substitution value (DS) is 0.41.
Embodiment 6
According to the mass fraction, 60 parts of NaOH and 6 part catalyzer cetyl trimethylammonium bromide is added in 100 parts of Starch rices, pour 1250 parts of aqueous isopropanols and 55 parts of distilled water into, stirring velocity is 200r/min abundant stirring heating 35min in the water-bath of 50 DEG C, fully alkalize to make starch, then after being warming up to 60 DEG C, then add total 100 parts as follows and be mixed with 75 portions of chloroacetic Virahol mixed solutions, first will wherein 25 portions of mixed solutions be disposable adds, adjust agitator 400r/min immediately and stir 15min, regulate agitator stirring velocity to 300r/min, after continuing reaction 10min, add 10 parts of NaOH particles to keep the reaction environment of alkalescence, then after continuing reaction 10min, residual mixed liquor is dripped continuously in 120min, the speed that the first half time drips is 1.25 times of the later half time, in order to keep the reaction environment of alkalescence, when 1/3 time of beginning dripped and 2/3 time time add 10 parts and 10 parts of NaOH particles respectively.After dripping, continue reaction for some time, control total etherification time at 210min.After reaction terminates, be cooled to room temperature, with Glacial acetic acid adjust pH to 7.0, filter, the filter cake ethanolic soln washes clean of 90% volume fraction, is dried to constant weight in 50 DEG C of baking ovens, grinding, and sieves with 80 object sieves.Obtained carboxymethyl starch substitution value (DS) is 0.67.
Below be only better embodiment of the present invention, according to above-mentioned design of the present invention, those skilled in the art also can make various amendment and conversion to this.Such as, chloroacetic interpolation time, mode and speed, the blending ratio of Mono Chloro Acetic Acid and Virahol amount, the consumption of catalyzer, proportioning, the means regulating pH and consumption between alkalization and etherification reaction temperature and time, each component, the size of stirring velocity and drying temperature and mode etc. in reaction process; But similar this conversion and amendment all belong to essence of the present invention.
Claims (7)
1. continuous feeding legal system is for a method for carboxymethyl Starch rice, it is characterized in that comprising the steps:
(1) according to the mass fraction, in 100 parts of Starch rices, add 50 ~ 60 parts of NaOH and 4 ~ 7 part catalyzer, then pour 1200 ~ 1250 parts of aqueous isopropanols into it, and 45 ~ 55 parts of distilled water, then stirring heating in a water bath, starch is alkalized;
(2) after being warming up to 60 DEG C, add total 50 ~ 200 parts as follows and be mixed with 40 ~ 90 portions of chloroacetic Virahol mixed solutions, first will wherein 20 ~ 50 portions of mixed solutions be disposable adds, adjust agitator 300 ~ 600r/min immediately and stir 5 ~ 15min, regulate agitator stirring velocity to 200 ~ 300r/min, then reaction 15 ~ 30min is continued, again residual mixed liquor is dripped continuously in 40 ~ 120min, after dripping, continue reaction for some time, control total etherification time at 180 ~ 200min, in reaction process, the reaction environment that NaOH particle maintains alkalescence is added in reaction system, after reaction 180 ~ 200min, be cooled to room temperature, adjust pH to 6.5 ~ 7.0, filter, filter cake ethanolic soln washes clean, constant weight is dried in baking oven, grinding, and sieve,
The reaction environment that described NaOH particle maintains alkalescence is that pH controls 7 ~ 8;
Described continuous dropping adopts constant pressure funnel, and the speed that the first half time drips is 1.1-1.3 times of the later half time.
2. continuous feeding legal system according to claim 1 is for the method for carboxymethyl Starch rice, it is characterized in that: described catalyzer is cetyl trimethylammonium bromide.
3. continuous feeding legal system according to claim 1 is for the method for carboxymethyl Starch rice, it is characterized in that: the stirring velocity of described step (1) is 200 ~ 250r/min, and bath temperature is 50 DEG C, and heat-up time is 30 ~ 40min.
4. continuous feeding legal system according to claim 1 is for the method for carboxymethyl Starch rice, it is characterized in that: the volume fraction of the ethanolic soln of described step (2) is 90% ~ 95%.
5. continuous feeding legal system according to claim 1 is for the method for carboxymethyl Starch rice, it is characterized in that: the oven drying temperature of described step (2) is 45 ~ 55 DEG C.
6. continuous feeding legal system according to claim 1 is for the method for carboxymethyl Starch rice, it is characterized in that: the screening of described step (2) adopts 80 object sieves.
7. continuous feeding legal system according to claim 1 is for the method for carboxymethyl Starch rice, it is characterized in that: described step (2) reaction terminates rear tune pH and adopts Glacial acetic acid.
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| CN1274718C (en) * | 2004-08-06 | 2006-09-13 | 王美岭 | Production method of sodium carboxy methy starch |
| CN101585883B (en) * | 2009-06-19 | 2011-03-30 | 山东一滕化工有限公司 | High-purity sodium carboxymethyl starch, preparation method thereof and application thereof |
| CN103554282B (en) * | 2012-12-07 | 2017-06-30 | 新疆光大山河化工科技有限公司 | The preparation method of substituted carboxymethyl starch sodium high |
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Effective date of registration: 20210827 Address after: 535000 zone 3, Real Madrid Industrial Park, Qinbei District, Qinzhou City, Guangxi Zhuang Autonomous Region Patentee after: Guangxi libaixing Food Co.,Ltd. Address before: Donkey pond in Hunan province Xiangtan City Yuhu District 411105 Patentee before: XIANGTAN University |
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Address after: 535000 zone 3, Real Madrid Industrial Park, Qinbei District, Qinzhou City, Guangxi Zhuang Autonomous Region Patentee after: Guangxi Libaixing Food Group Co.,Ltd. Address before: 535000 zone 3, Real Madrid Industrial Park, Qinbei District, Qinzhou City, Guangxi Zhuang Autonomous Region Patentee before: Guangxi libaixing Food Co.,Ltd. |