CN101670276A - Amorphophallus glucomannan drying agent and preparation method thereof - Google Patents
Amorphophallus glucomannan drying agent and preparation method thereof Download PDFInfo
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- CN101670276A CN101670276A CN200910112599A CN200910112599A CN101670276A CN 101670276 A CN101670276 A CN 101670276A CN 200910112599 A CN200910112599 A CN 200910112599A CN 200910112599 A CN200910112599 A CN 200910112599A CN 101670276 A CN101670276 A CN 101670276A
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Abstract
The invention relates to an amorphophallus glucomannan drying agent which consists of amorphophallus glucomannan, propenoic acid, sodium hydroxide, ethanol, hydrochloric acid, potassium persulfate, N,N-methylene-bisacrylamide, calcium chloride and water. The preparation method of the drying agent comprises the steps of: preparing deacetylation amorphophallus glucomannan and deacetylation amorphophallus glucomannan-propenoic acid copolymer; mixing the deacetylation amorphophallus glucomannan and the deacetylation amorphophallus glucomannan-propenoic acid copolymer according to a proportion; andcrushing and pelleting after expansion. The drying agent has the advantages of reasonable formula, low cost, strong water absorption, safety, no toxicity, no harm to skin and eyes, biodegradability and the like, and can be widely applied to the fields such as food, medicine, chemical industry and the like.
Description
Technical field
The present invention relates to a kind of drier and preparation method thereof, being specifically related to a kind of is the Amorphophallus glucomannan drying agent and preparation method thereof of primary raw material with the konjaku glucomannan.
Background technology
Is primary raw material in view of traditional drier is commonly used with silica gel, quick lime, molecular sieve and polymer water-absorbent etc.But owing to have shortcoming separately, low as the silica gel water absorption capacity, when higher levels of humidity, water absorption is very easy to reach capacity; Quick lime becomes the aqueous solution gradually in moisture absorption process; The price of polymer water-absorbent is high, has greatly limited their extensive uses in fields such as food.Therefore, a kind of research of novel drier receives much attention, and particularly edible deciccant becomes one of focus direction of drier development of manufacturing.A new generation's novel drier is a raw material with the natural material, is divided into the natural inorganic material being the drier of raw material and being two kinds in the drier of raw material with the natural organic.With the natural inorganic material is the drier of raw material, and as natural sepiolite drier, montmorillonite active drying agent and chicken coop rock and ore drier etc., the wettability power of this class drier is stronger, but exists rock salt to pollute and environment is hard to tolerate query such as receives.With the natural organic is the drier of raw material, the drier of doing as native starch drier, fry starch of konjak drier and coconut crust etc.; This class drier is regenerated resources, but natural degradation, the main flow of having represented the current drying agent to develop, but moisture absorption finite capacity.
Application number is 200510018580.8 patent of invention " edible deciccant " (date of application: 2005.04.19), introduce a kind of drier of edibility.This drier will be mixed evenly in proportion by water-absorbing material and auxiliary material, and will be expanded in bulking machine, go in the pulverizer and pulverize, granulation then, screening, packing.This edible deciccant is at 25 ℃, advantage such as under the environmental condition of RH=90%, hydroscopicity can reach 35%～150%, and it is strong to have water-retaining property, eats safety by mistake, and skin, eyes are not had injury, and is biodegradable.But the moisture absorption finite capacity is not suitable for using in the low wet environment.
Application number is 200610018377.5 patent of invention " a kind of drier and preparation method " (date of application: 2006.02.17); introduce a kind of by water-absorbing material, after easily deliquescence material and plant polyose three class materials carry out preliminary treatment or mix, compressing tablet, granulation or directly pack.This edible deciccant is at 25 ℃, and under the environmental condition of RH=90%, hydroscopicity can reach 50%～750%.
People such as Li Wanfen deliver at " EI " and propose with the konjaku glucomannan in " the moisture-absorption characteristics research of konjaku glucomannan-acrylic acid graft copolymer " is raw material, the acrylic graft-modified konjaku super strength water absorbent that synthesized, has strong water imbibition, also has wettability power, but the konjaku glucomannan swelling is slow slightly, and the konjaku super strength water absorbent is not suitable for using in the low wet environment.
Summary of the invention
The purpose of this invention is to provide a kind of Nonpoisonous, non-environmental-pollution, fully biodegradable, and edible Amorphophallus glucomannan drying agent and preparation method thereof.
Amorphophallus glucomannan drying agent of the present invention, by konjaku glucomannan, acrylic acid, NaOH, ethanol, hydrochloric acid, potassium peroxydisulfate, N, N-methylene-bisacrylamide, calcium chloride and water are formed.Employed reagent is chemical pure.
The preparation method of Amorphophallus glucomannan drying agent of the present invention, be made up of following steps:
(1) preparation of deacetylation konjaku glucomannan: konjaku glucomannan is dried by the fire 2.5～3h in 60～70 ℃ of environment, be with solid sodium hydroxide to mix at 45～50: 1 by mass ratio then; Put mixture in the sand cylinder of dry type vibratory mill, after the modification of 25min deacetylation is handled, 3～5min in the ethanolic solution of immersion 50% (V/V); The quality of described ethanolic solution is 4.5～5 times of konjaku glucomannan quality; Be neutralized to pH=7 with HCl solution, then washing; Ethanolic solution with 50% (V/V) washs 3 times, and each washing is all carried out under stirring condition, and the rotating speed of agitator is 300～500r/min, and wash time is 25～30min; 3 washing back vacuum filtrations under the condition of vacuum 0.7～0.8Mpa are until using AgNO
3Solution checks its supernatant liquor not contain Cl
-Products therefrom is dry under 60～70 ℃ of conditions, get the deacetylation konjaku glucomannan;
(2) deacetylation konjaku glucomannan-acrylic copolymer preparation: add the deacetylation konjaku glucomannan in acrylic acid, the addition of deacetylation konjaku glucomannan and acrylic acid mass ratio are 1: 35～45; Logical nitrogen and electronic stirring 15～20min under 35～40 ℃ of environmental conditions, speed of agitator is 300～500r/min; Adding initator and crosslinking agent then, after stirring, is under 60～65 ℃ the condition behind graft polymerization reaction 4～5min at bath temperature, takes out product, oven dry, pulverizes, crosses 100～140 mesh sieves, deacetylation konjaku glucomannan-acrylic copolymer; Described acrylic acid, for in the NaOH and after degree of neutralization be 70～80% acrylic acid solution; Described initator is a potassium peroxydisulfate, and addition is 0.5%～0.6% of deacetylation konjaku glucomannan and an acrylic acid gross mass; Described crosslinking agent is N, the N-methylene-bisacrylamide, and addition is 0.1%～0.12% of deacetylation konjaku glucomannan and an acrylic acid gross mass;
(3) preparation of Amorphophallus glucomannan drying agent: deacetylation konjaku glucomannan-acrylic copolymer and calcium chloride are 6～9.5: 0.05～4 fully mixing by its mass ratio that accounts for total material, expanded then, pulverize granulation, packing.
Advantages such as the drier that utilizes the method to make is filled a prescription rationally, and with low cost, it is strong to have water imbibition, and safety non-toxic does not have injury to skin, eyes, and is biodegradable.The primary raw material that the most important thing is this drier is edible konjaku glucan.Konjaku is the characteristic resources of China, its main component konjaku glucomannan, be by glucose and mannose with the heteroglycan that β-glycosidic bond is formed by connecting, have good water imbibition and moisture retention, also have functions such as antibiotic, health care.Konjaku glucomannan is carried out the modification of mechanical force and chemical deacetylation, can reduce the thixotropy of the konjaku glucomannan hydrosol, improved the water imbibition of konjaku glucomannan.And deacetylation konjaku glucomannan and acrylic graft-modified synthetic copolymer have superpower aqueous water adsorption capacity.Be not suitable for characteristics in the low wet environment at deacetylation konjaku glucomannan-acrylic copolymer, added calcium chloride.Calcium chloride is a kind of widely used drier, but owing to its easy deliquescence, becomes solution after stain article, thereby limited its use, after still using with deacetylation konjaku glucomannan-acrylic copolymer is composite, and CaCl
2In water can be absorbed by deacetylation konjaku glucomannan-acrylic copolymer, deacetylation konjaku glucomannan-acrylic copolymer plays the effect of water conservation, has prevented CaCl
2Deliquescence, can guarantee again that simultaneously this drier uses in low wet environment.
Specific embodiment
In order fully to disclose Amorphophallus glucomannan drying agent of the present invention and preparation method thereof, be illustrated below in conjunction with embodiment.
The preparation method of Amorphophallus glucomannan drying agent of the present invention, be made up of following steps:
(1) preparation of deacetylation konjaku glucomannan: mix with the NaOH of 0.4g behind 60 ℃ of bakings of the konjaku glucomannan 3h with 20g, put mixture in the sand cylinder of dry type vibratory mill, after carrying out 25min deacetylation modification processing, 5min in the ethanolic solution of 50% (V/V) that immerse 100ml through modified product; Be neutralized to pH=7 with 6mol/L HCl solution again, use the ethanolic solution of 50% (V/V) to wash then 3 times, wash 30min at every turn, washing while stirring, the rotating speed of stirring is 400r/min; 3 washings are vacuum filtration under the 0.7Mpa condition in vacuum later, until the supernatant liquor of getting suction filtration, use AgNO
3The solution check does not contain Cl
-Till, products therefrom in 60 ℃ of dryings, is got the deacetylation konjaku glucomannan.
(2) preparation of deacetylation konjaku glucomannan-acrylic copolymer: put 10g deacetylation konjaku glucomannan in the 500ml erlenmeyer flask, add the 400g acrylic acid solution; 35 ℃ of down logical nitrogen and electronic stirring 15min, speed of agitator 400r/min and one straight-through nitrogen between the stage of reaction make deacetylation konjaku glucomannan swelling; After adding initator and crosslinking agent then and stirring, be under 60 ℃ the condition behind the graft polymerization reaction 4min at bath temperature, take out product, oven dry, pulverize, cross 120 mesh sieves, deacetylation konjaku glucomannan-acrylic copolymer; Described acrylic acid solution, for in the NaOH and after degree of neutralization be 80% acrylic acid solution; Described initator is a potassium peroxydisulfate, and addition is 2.05g; Described crosslinking agent is N, the N-methylene-bisacrylamide, and addition is 0.42g.
(3) preparation of drier: deacetylation konjaku glucomannan-acrylic copolymer and calcium chloride are fully mixing in 9: 1 by its mass ratio, expanded then, pulverize granulation, the granulation diameter is 1mm, at last packing.Described bulking process: raw material is put into Bulking tank, be heated to 90 ℃, stagnate 6min again, open the valve between Bulking tank and the vacuum tank, instantaneous vacuumizing, the pressure of Bulking tank is reduced rapidly, thereby cause that material is expanded, continue to keep vacuum to carry out drying, to raw material puffed even, dry tack free, no aqueous vapor stop heating when evaporating, feed cooling water subsequently and make temperature of charge reduce to room temperature in the interlayer of Bulking tank.
According to the drier of method preparation of the present invention, at T=20 ℃, the relative humidity of environment is under the condition of RH=90%, and hydroscopicity can reach 40%; At T=25 ℃, under the condition of the relative humidity RH=95% of environment, hydroscopicity can reach 53%.Safety non-toxic does not have injury to human body, and is biodegradable.This drier can be widely used in fields such as food, medicine, chemical industry.
Claims (5)
1, a kind of preparation method of Amorphophallus glucomannan drying agent is characterized in that being made up of following steps:
(1) preparation of deacetylation konjaku glucomannan: konjaku glucomannan is dried by the fire 2.5～3h in 60～70 ℃ of environment, be with solid sodium hydroxide to mix at 45～50: 1 by mass ratio then; Put mixture in the sand cylinder of dry type vibratory mill, after the modification of 25min deacetylation is handled, 3～5min in the ethanolic solution of immersion 50% (V/V); The quality of described ethanolic solution is 4.5～5 times of konjaku glucomannan quality; Be neutralized to pH=7 with HCl solution, then washing; Ethanolic solution with 50% (V/V) washs 3 times, and each washing is all carried out under stirring condition, and the rotating speed of agitator is 300～500r/min, and wash time is 25～30min; 3 washing back vacuum filtrations under the condition of vacuum 0.7～0.8Mpa are until using AgNO
3Solution checks its supernatant liquor not contain Cl-; Products therefrom is dry under 60～70 ℃ of conditions, get the deacetylation konjaku glucomannan;
(2) deacetylation konjaku glucomannan-acrylic copolymer preparation: add the deacetylation konjaku glucomannan in acrylic acid, the addition of deacetylation konjaku glucomannan and acrylic acid mass ratio are 1: 35～45; Logical nitrogen and electronic stirring 15～20min under 35～40 ℃ of environmental conditions, speed of agitator is 300～500r/min; Adding initator and crosslinking agent then, after stirring, is under 60～65 ℃ the condition behind graft polymerization reaction 4～5min at bath temperature, takes out product, oven dry, pulverizes, crosses 100～140 mesh sieves, deacetylation konjaku glucomannan-acrylic copolymer;
(3) preparation of Amorphophallus glucomannan drying agent: deacetylation konjaku glucomannan-acrylic copolymer and calcium chloride are 6～9.5: 0.05～4 fully mixing by its mass ratio that accounts for total material, expanded then, pulverize granulation, packing.
2, the preparation method of a kind of Amorphophallus glucomannan drying agent according to claim 1 is characterized in that described acrylic acid, for in the NaOH and after degree of neutralization be 70～80% acrylic acid solution.
3, the preparation method of a kind of Amorphophallus glucomannan drying agent according to claim 1 is characterized in that described initator is a potassium peroxydisulfate, and addition is 0.5%～0.6% of deacetylation konjaku glucomannan and an acrylic acid gross mass.
4, the preparation method of a kind of Amorphophallus glucomannan drying agent according to claim 1 is characterized in that described crosslinking agent is N, the N-methylene-bisacrylamide, and addition is 0.1%～0.12% of deacetylation konjaku glucomannan and an acrylic acid gross mass.
5, by the Amorphophallus glucomannan drying agent of claim 1,2,3, the preparation of 4 method.
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Cited By (12)
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| CN101843311A (en) * | 2010-05-05 | 2010-09-29 | 陕西省科学院酶工程研究所 | Method for preparing hippophae rhamnoides seed micro powder capsules |
| CN102600705A (en) * | 2012-04-10 | 2012-07-25 | 福建省中医药研究院 | Edible plant dryer |
| CN102658091A (en) * | 2012-04-20 | 2012-09-12 | 浙江理工大学 | Preparation method of museum environmental-protection humidifying agent |
| CN105032135A (en) * | 2015-08-10 | 2015-11-11 | 湖北一致魔芋生物科技有限公司 | Biological desiccant and preparing method of biological desiccant |
| CN105601819A (en) * | 2016-01-29 | 2016-05-25 | 深圳职业技术学院 | Low-temperature gel-state phase-changing cold storage agent and preparation method thereof |
| CN105983397A (en) * | 2016-01-18 | 2016-10-05 | 明光市飞洲新材料有限公司 | Drying agent for automobile brake system and preparation method thereof |
| CN105983396A (en) * | 2016-01-18 | 2016-10-05 | 明光市飞洲新材料有限公司 | Anticorrosive and anti-rust drying agent for metal spare and accessory parts and method for preparing anticorrosive and anti-rust drying agent |
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| CN109045548A (en) * | 2018-09-17 | 2018-12-21 | 蚌埠市龙泰消防有限公司 | A kind of long-acting dry powder fire extinguishing agent |
| CN109497460A (en) * | 2018-12-29 | 2019-03-22 | 福建农林大学 | A kind of bionical roe of konjaku glucomannan and preparation method thereof |
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| CN101843311A (en) * | 2010-05-05 | 2010-09-29 | 陕西省科学院酶工程研究所 | Method for preparing hippophae rhamnoides seed micro powder capsules |
| CN102600705A (en) * | 2012-04-10 | 2012-07-25 | 福建省中医药研究院 | Edible plant dryer |
| CN102600705B (en) * | 2012-04-10 | 2014-06-04 | 福建省中医药研究院 | Edible plant dryer |
| CN102658091A (en) * | 2012-04-20 | 2012-09-12 | 浙江理工大学 | Preparation method of museum environmental-protection humidifying agent |
| CN102658091B (en) * | 2012-04-20 | 2014-04-02 | 浙江理工大学 | Preparation method of museum environmental-protection humidifying agent |
| CN105032135A (en) * | 2015-08-10 | 2015-11-11 | 湖北一致魔芋生物科技有限公司 | Biological desiccant and preparing method of biological desiccant |
| CN105983396A (en) * | 2016-01-18 | 2016-10-05 | 明光市飞洲新材料有限公司 | Anticorrosive and anti-rust drying agent for metal spare and accessory parts and method for preparing anticorrosive and anti-rust drying agent |
| CN105983397A (en) * | 2016-01-18 | 2016-10-05 | 明光市飞洲新材料有限公司 | Drying agent for automobile brake system and preparation method thereof |
| CN105601819A (en) * | 2016-01-29 | 2016-05-25 | 深圳职业技术学院 | Low-temperature gel-state phase-changing cold storage agent and preparation method thereof |
| CN108384275A (en) * | 2018-03-06 | 2018-08-10 | 上海交通大学 | A method of improving black rice pigments stability |
| CN108384275B (en) * | 2018-03-06 | 2019-09-10 | 上海交通大学 | A method of improving black rice pigments stability |
| CN109045548A (en) * | 2018-09-17 | 2018-12-21 | 蚌埠市龙泰消防有限公司 | A kind of long-acting dry powder fire extinguishing agent |
| CN109497460A (en) * | 2018-12-29 | 2019-03-22 | 福建农林大学 | A kind of bionical roe of konjaku glucomannan and preparation method thereof |
| CN110150162A (en) * | 2019-06-25 | 2019-08-23 | 福建农林大学 | A kind of konjaku glucomannan cat litter and preparation method thereof |
| CN114958223A (en) * | 2022-04-07 | 2022-08-30 | 湖北亿谦食品科技有限公司 | Moisture absorption patch, preparation method thereof and application thereof in meal packaging |
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