CN105017544A - Preparation of water-blocking biodegradable membrane containing low-viscosity rice-hull-based carboxymethyl cellulose - Google Patents
Preparation of water-blocking biodegradable membrane containing low-viscosity rice-hull-based carboxymethyl cellulose Download PDFInfo
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- CN105017544A CN105017544A CN201510496288.0A CN201510496288A CN105017544A CN 105017544 A CN105017544 A CN 105017544A CN 201510496288 A CN201510496288 A CN 201510496288A CN 105017544 A CN105017544 A CN 105017544A
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- rice husk
- carboxymethyl cellulose
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Abstract
Grain processing waste, namely, rice hulls, serves as raw materials, rice hull cellulose is obtained through chemical pretreatment, and then low-viscosity rice-hull-based carboxymethyl cellulose is prepared through a solvent method. The substitution degree of the rice-hull-based carboxymethyl cellulose obtained under different preparation conditions is 0.65 to 0.85, the viscosity of 2% of CMC is 20 MPa to 45 MPa.s, and the purity of 2% of CMC is 90% to 94%. The rice-hull-based carboxymethyl cellulose can serve as plasticizer by the addition of glycerinum through a simple method, and the biodegradable carboxymethyl cellulose membrane with the good water-blocking property is prepared. The water vapor transmission (MVP) is 0.1-0.5 g.mm.m<-2>.d<-1>.Pa<-1>, the oil transmission coefficient (P0) is 7.2-11.0 g.mm.m-<2>d<-1>, the breaking strength is 13-28 MPa, the elongation at break is 28-86%, and it is found that the weight loss ratio of the membrane after the membrane is buried with soil for 8 weeks is 25-40% by measuring the weight loss rate of the membrane through a soil burying method.
Description
Technical field
The present invention relates to a kind of preparation method containing the blocking water of low viscosity rice husk base carboxymethyl cellulose, biodegradable film, obtained rice husk base carboxymethyl cellulose film may be used for food packaging applications, such as food fresh keeping etc.
Background technology
Food fresh keeping film needs membrane product can have the characteristics such as water preventing ability, grease-proof transport property, retaining food product local flavor, physical strength are good, and at present due to the sternness of problem of environmental pollution, the biodegradable performance of membrane product is also subject to people's most attention.The raw materials of tradition preservative film is generally polypropylene, polyethylene, polyester and Low Density Polyethylene etc., although fresh keeping property is good, but biodegradable performance is poor, so how to find one of good raw material study hotspot becoming food packaging applications of alternative biological degradability.Because carboxymethyl cellulose (CMC) has a lot of premium properties, as thickening, suspend, fall the characteristics such as dehydration, chemical stability are good, biodegradable, can be used for the preparation of antistaling film.
Main production raw material due to traditional carboxymethyl cellulose is purified cotton, be subject to the restriction of the condition such as geography, ginnings, and the range of application of CMC is wide, makes its raw material supply quantity not sufficient.At present, domestic have Many researchers to stress raw-material exploitation to replace traditional starting material, and deep seafood in Guangxi adopts bagasse as starting material, take KI/NaAC as catalyzer, in ethanolic soln, and H
2o
2for oxygenant, obtained product effective constituent 85% ~ 95%, substitution value is 0.65 ~ 0.80; He also prepares CMC with bamboo tankage, and substitution value is greater than 0.65, and effective constituent is greater than 85%; University Of Science and Technology Of Tianjin king ten thousand is gloomy take stalk as starting material, and obtained CMC effective constituent massfraction is greater than 80%, substitution value 0.6 ~ 0.7; Chinese Academy Of Sciences Process Engineering Research Institute Yang Ye adopts gas explosion maize straw to be starting material, obtains the carboxymethyl cellulose that substitution value is 0.91; The Xie Wenwei in Henan adopts three etherification methods, adds H
2o
2activation, obtained product substitution value can reach 1.3.
External also have scientific worker to find different starting material to produce CMC being engaged in.Fevzi Y. etc. are raw material with orange peel, and through degreasing, deproteinize, colloid, hemicellulose, xylogen, obtain orange peel Mierocrystalline cellulose, adopt sodium hydroxide, isopropylcarbinol and Mono Chloro Acetic Acid to be the CMC that reaction reagent obtains that substitution value is 0.6705; V.Pushpamalar etc. are with sago palm residue for raw material, and Virahol is the CMC that reaction solvent obtains that substitution value is 0.821; Hasan
take isopropylcarbinol as solvent, the obtained substitution value of garden beet slurry is the CMC of 0.6670.
Summary of the invention
In order to alleviate the raw-material restricted problem of carboxymethyl cellulose, this patent adopts this modal grain processing by product of rice husk to prepare low viscosity CMC, and by simple thin film-forming method research CMC plastic film mulch performance, find that its water preventing ability, biodegradable are good, can be used for the fields such as food fresh keeping.
Technical scheme of the present invention is as follows:
A preparation containing the blocking water of low viscosity rice husk base carboxymethyl cellulose, biodegradable film, concrete steps are as follows:
(1) be crushed to 100 orders after being cleaned by rice husk, configuration quality mark is the dilution heat of sulfuric acid of 5%.
(2) be that 1:10 mixes by above-mentioned pulverizing rice husk and sulphuric acid soln with mass ratio, filter after reacting 3h under backflow boiling conditions, filter residue is washed till neutrality.The object of this step is used to remove part colloid, hemicellulose and the inorganic metal salt in rice husk.
(3) configuration quality mark is the sodium hydroxide solution of 12-18%, mix with the ratio that solid-liquid mass ratio is 1:10 with the rice husk residue in above-mentioned steps (2), filter after back flow reaction 4h at 120 DEG C, residue obtainedly wash into neutrality, now the main component of residue is rice husk cellulose.The object of this step is used to remove colloid, xylogen and the silicon class material in rice husk.
(4) by the rice husk cellulose of step (3) gained with 30% superoxol at 90-95 DEG C, solid-liquid mass ratio is mix 7-9h under the ratio of 1:15-1:20, the dry rice husk cellulose obtaining white after gained solid washed several times with water.The object of this step is to remove residual lignin, and rice husk cellulose is decoloured.
(5) preparation of rice husk base CMC adopts solvent method, is divided into alkalization, two stages of etherificate.Wherein basification stage concrete operations mode is: mixed with ethanol solution by the white rice husk cellulose of gained in step (4), setting alkalization temperature is 30 DEG C, dropwise add the massfraction accounting for volumes of aqueous ethanol 15-25% be the sodium hydroxide solution of 30-50% in above-mentioned system, after stirring and refluxing 1-2h, quaternization completes.Etherification stage concrete operations mode is: when above-mentioned system continuation intensification is reached the etherification temperature 70-80 DEG C of setting, the sodium chloroacetate solution being 15-70% by the massfraction accounting for initial volumes of aqueous ethanol 15-25% dropwise joins in above-mentioned reaction system, and after stirring and refluxing 3h, etherification reaction completes.
(6) the rice husk CMC raw product of gained in step (5) is extremely neutral with Glacial acetic acid process, with the ethanolic soln of 70-80% be under the ratio of 1:5 with solid-to-liquid ratio, agitator treating 20min at 45 DEG C, wash 2 times, filter the residue obtained ethanolic soln repetitive scrubbing more than twice continued with 75% methyl alcohol and 75%.
(7) solid washed in step (6) is placed in the dry 3h of baking oven of 105 DEG C, gained white solid is rice husk base carboxymethyl cellulose.
(8) by massfraction be 2-8% step (7) in the glycerine of rice husk base CMC and 0-5% at 65 DEG C, high-speed stirring 30min makes it form homogeneous film formation liquid.Then by film-forming soln under the vacuum tightness of 0.09MPa degassed 20min to drive away in whipping process the air be dissolved in film forming liquid.
(9) take a certain amount of film forming liquid curtain coating in step (8) and on the smooth clean glass dish of certain area, be positioned over dry certain hour in the vacuum drying oven of 40 DEG C, namely make rice husk base carboxymethyl cellulose film.
Under different preparation condition, the substitution value of the rice husk base carboxymethyl cellulose of gained is 0.65-0.85, and the CMC viscosity of 2% is 20-45MPa.s, and purity is 90-94%.The water vapor transmission (MVP) of the rice husk base carboxymethyl cellulose film made is 0.1-0.5gmmm
– 2d
– 1pa
– 1, saturating oily coefficient (P
0) be 7.2-11.0gmmm
-2d
– 1, breaking tenacity is 13-28MPa, elongation at break 28-86%, and the rate of weight loss measuring film through soil method of burying finds, the rate of weight loss that soil buries 8 weeks caudacorias is 25-40%.
The present invention has the following advantages:
(1) abundant raw material source, cheapness, renewable;
(2) the rice husk base CMC of gained is functional;
(3) rice husk base CMC plastic film mulch is easy, and simultaneously obtained CMC film water preventing ability, biodegradable performance are good.
Specific embodiments
Embodiment 1:
Be that 1:10 mixes by the sulphuric acid soln of 100 order rice husks and 5% with mass ratio, filter after reacting 3h under backflow boiling conditions, filter residue is washed till neutrality.The residue obtained ratio that is 1:10 with solid-liquid mass ratio, adds the sodium hydroxide solution that massfraction is 12%, filters at 120 DEG C after back flow reaction 4h, washing residue become neutral after dry.Then use the superoxol of 30% at 90 DEG C, solid-liquid mass ratio is mix 9h under the ratio of 1:20, and the dry rice husk cellulose obtaining white after gained solid washed several times with water, productive rate is 29.8%.
Get above-mentioned white rice husk cellulose to mix with ethanol solution, setting alkalization temperature is 30 DEG C, dropwise add the massfraction accounting for volumes of aqueous ethanol 20% be the sodium hydroxide solution of 50% in above-mentioned system, after stirring and refluxing 2h, quaternization completes.When then above-mentioned system continuation intensification being reached the etherification temperature 80 DEG C of setting, the sodium chloroacetate solution being 60% by the massfraction accounting for initial volumes of aqueous ethanol 15% dropwise joins in above-mentioned reaction system, and after stirring and refluxing 3h, etherification reaction completes.The rice husk CMC raw product of gained is extremely neutral with Glacial acetic acid process, ethanolic soln with 80% is under the ratio of 1:5 with solid-to-liquid ratio, agitator treating 20min at 45 DEG C, washs 2 times, filters residue obtained the continuation methyl alcohol of 75% and the ethanolic soln repetitive scrubbing more than twice of 75%.Gained solid is placed in the dry 3h of baking oven of 105 DEG C, and gained white solid is rice husk base carboxymethyl cellulose, its substitution value be 0.67,2% CMC viscosity be 38MPa.s, purity is 92%.
By massfraction be the glycerine of the rice husk base CMC and 3% of 2% at 65 DEG C, high-speed stirring 30min makes it form homogeneous film formation liquid.Then by film-forming soln degassed 20min under the vacuum tightness of 0.09MPa.Get a certain amount of film forming liquid curtain coating on the smooth clean glass dish of certain area, be positioned over dry certain hour in the vacuum drying oven of 40 DEG C, namely make rice husk base carboxymethyl cellulose film.The water vapor transmission (MVP) of this film is 0.2gmmm
– 2d
– 1pa
– 1, saturating oily coefficient (P
0) be 8.7gmmm
-2d
– 1, breaking tenacity is 20MPa, elongation at break 68%, and the rate of weight loss measuring film through soil method of burying finds, the rate of weight loss that soil buries 8 weeks caudacorias is 28%.
Embodiment 2:
Be that 1:10 mixes by the sulphuric acid soln of 100 order rice husks and 5% with mass ratio, filter after reacting 3h under backflow boiling conditions, filter residue is washed till neutrality.The residue obtained ratio that is 1:10 with solid-liquid mass ratio, adds the sodium hydroxide solution that massfraction is 18%, filters at 120 DEG C after back flow reaction 4h, washing residue become neutral after dry.Then use the superoxol of 30% at 95 DEG C, solid-liquid mass ratio is mix 9h under the ratio of 1:15, and the dry rice husk cellulose obtaining white after gained solid washed several times with water, productive rate is 26.2%.
Get above-mentioned white rice husk cellulose to mix with ethanol solution, setting alkalization temperature is 30 DEG C, dropwise add the massfraction accounting for volumes of aqueous ethanol 25% be the sodium hydroxide solution of 45% in above-mentioned system, after stirring and refluxing 1h, quaternization completes.When then above-mentioned system continuation intensification being reached the etherification temperature 70 DEG C of setting, the sodium chloroacetate solution being 70% by the massfraction accounting for initial volumes of aqueous ethanol 25% dropwise joins in above-mentioned reaction system, and after stirring and refluxing 3h, etherification reaction completes.The rice husk CMC raw product of gained is extremely neutral with Glacial acetic acid process, ethanolic soln with 75% is under the ratio of 1:5 with solid-to-liquid ratio, agitator treating 20min at 45 DEG C, washs 2 times, filters residue obtained the continuation methyl alcohol of 75% and the ethanolic soln repetitive scrubbing more than twice of 75%.Gained solid is placed in the dry 3h of baking oven of 105 DEG C, and gained white solid is rice husk base carboxymethyl cellulose, its substitution value be 0.85,2% CMC viscosity be 21MPa.s, purity is 94%.
By massfraction be the glycerine of the rice husk base CMC and 4% of 4% at 65 DEG C, high-speed stirring 30min makes it form homogeneous film formation liquid.Then by film-forming soln under the vacuum tightness of 0.09MPa degassed 20min to drive away air in film forming liquid.Get a certain amount of film forming liquid curtain coating on the smooth clean glass dish of certain area, be positioned over dry certain hour in the vacuum drying oven of 40 DEG C, namely make rice husk base carboxymethyl cellulose film.The water vapor transmission (MVP) of this film is 0.4gmmm
– 2d
– 1pa
– 1, saturating oily coefficient (P
0) be 7.2gmmm
-2d
– 1, breaking tenacity is 16MPa, elongation at break 80%, and the rate of weight loss measuring film through soil method of burying finds, the rate of weight loss that soil buries 8 weeks caudacorias is 37%.
Embodiment 3:
Be that 1:10 mixes by the sulphuric acid soln of 100 order rice husks and 5% with mass ratio, filter after reacting 3h under backflow boiling conditions, filter residue is washed till neutrality.The residue obtained ratio that is 1:10 with solid-liquid mass ratio, adds the sodium hydroxide solution that massfraction is 15%, filters at 120 DEG C after back flow reaction 4h, washing residue become neutral after dry.Then use the superoxol of 30% at 92 DEG C, solid-liquid mass ratio is mix 9h under the ratio of 1:18, and the dry rice husk cellulose obtaining white after gained solid washed several times with water, productive rate is 28.8%.
Get above-mentioned white rice husk cellulose to mix with ethanol solution, setting alkalization temperature is 30 DEG C, dropwise add the massfraction accounting for volumes of aqueous ethanol 20% be the sodium hydroxide solution of 40% in above-mentioned system, after stirring and refluxing 1.5h, quaternization completes.When then above-mentioned system continuation intensification being reached the etherification temperature 75 DEG C of setting, the sodium chloroacetate solution being 30% by the massfraction accounting for initial volumes of aqueous ethanol 25% dropwise joins in above-mentioned reaction system, and after stirring and refluxing 3h, etherification reaction completes.The rice husk CMC raw product of gained is extremely neutral with Glacial acetic acid process, ethanolic soln with 80% is under the ratio of 1:5 with solid-to-liquid ratio, agitator treating 20min at 45 DEG C, washs 2 times, filters residue obtained the continuation methyl alcohol of 75% and the ethanolic soln repetitive scrubbing more than twice of 75%.Gained solid is placed in the dry 3h of baking oven of 105 DEG C, and gained white solid is rice husk base carboxymethyl cellulose, its substitution value be 0.65,2% CMC viscosity be 20MPa.s, purity is 91%.
By massfraction be the glycerine of the rice husk base CMC and 1% of 8% at 65 DEG C, high-speed stirring 30min makes it form homogeneous film formation liquid.Then by film-forming soln degassed 20min under the vacuum tightness of 0.09MPa.Get a certain amount of film forming liquid curtain coating on the smooth clean glass dish of certain area, be positioned over dry certain hour in the vacuum drying oven of 40 DEG C, namely make rice husk base carboxymethyl cellulose film.The water vapor transmission (MVP) of this film is 0.1gmmm
– 2d
– 1pa
– 1, saturating oily coefficient (P
0) be 10.3gmmm
-2d
– 1, breaking tenacity is 28MPa, elongation at break 31%, and the rate of weight loss measuring film through soil method of burying finds, the rate of weight loss that soil buries 8 weeks caudacorias is 35%.
Claims (3)
1. the preparation containing the blocking water of low viscosity rice husk base carboxymethyl cellulose, biodegradable film, is characterized in that concrete steps are as follows:
A. pretreatment stage
(1) being ground into particle diameter after being cleaned by rice husk is 100 orders, and configuration quality mark is the dilution heat of sulfuric acid of 5%.
(2) be that 1:10 mixes by above-mentioned pulverizing rice husk and sulphuric acid soln with mass ratio, filter after reacting 3h under backflow boiling conditions, filter residue is washed till neutrality.
(3) configuration quality mark is the sodium hydroxide solution of 12-18%, mix with the ratio that solid-liquid mass ratio is 1:10 with the rice husk residue in above-mentioned steps (2), filter after back flow reaction 4h at 120 DEG C, residue obtainedly wash into neutrality, now the main component of residue is rice husk cellulose.
(4) by the rice husk cellulose of step (3) gained with 30% superoxol at 90-95 DEG C, solid-liquid mass ratio is mix 7-9h under the ratio of 1:15-1:20, the dry rice husk cellulose obtaining white after gained solid washed several times with water.
B. rice husk base carboxymethyl cellulose preparatory phase
(5) adopt solvent method, be divided into alkalization, two stages of etherificate.Wherein basification stage concrete operations mode is: mixed with ethanol solution by the white rice husk cellulose of gained in step (4), setting alkalization temperature is 30 DEG C, dropwise add the massfraction accounting for volumes of aqueous ethanol 15-25% be the sodium hydroxide solution of 30-50% in above-mentioned system, after stirring and refluxing 1-2h, quaternization completes.Etherification stage concrete operations mode is: when above-mentioned system continuation intensification is reached the etherification temperature 70-80 DEG C of setting, the sodium chloroacetate solution being 15-70% by the massfraction accounting for initial volumes of aqueous ethanol 15-25% dropwise joins in above-mentioned reaction system, and after stirring and refluxing 3h, etherification reaction completes.
(6) the rice husk base carboxymethyl cellulose raw product of gained in step (5) is extremely neutral with Glacial acetic acid process, with the ethanolic soln of 70-80% be under the ratio of 1:5 with solid-to-liquid ratio, agitator treating 20min at 45 DEG C, wash 2 times, filter the residue obtained ethanolic soln repetitive scrubbing more than twice continued with 75% methyl alcohol and 75%.
(7) solid washed in step (6) is placed in the dry 3h of baking oven of 105 DEG C, gained white solid is rice husk base carboxymethyl cellulose.
C. the rice husk base carboxymethyl cellulose masking stage
(8) by massfraction be 2-8% step (7) in the glycerine of rice husk base carboxymethyl cellulose and 0-5% at 65 DEG C, high-speed stirring 30min makes it form homogeneous film formation liquid.Then by film-forming soln under the vacuum tightness of 0.09MPa degassed 20min to drive away in whipping process the air be dissolved in film forming liquid.
(9) take a certain amount of film forming liquid curtain coating in step (8) and on the smooth clean glass dish of certain area, be positioned over dry certain hour in the vacuum drying oven of 40 DEG C, namely make rice husk base carboxymethyl cellulose film.
2. a kind of preparation containing the blocking water of low viscosity rice husk base carboxymethyl cellulose, biodegradable film according to claim 1, is characterized in that the rice husk in step (1) can adopt other stalk biomass to replace.
3. a kind of preparation containing the blocking water of low viscosity rice husk base carboxymethyl cellulose, biodegradable film according to claim 2, is characterized in that other stalk biomass described comprise straw, rice straw.
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Cited By (4)
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| CN105884907A (en) * | 2016-06-29 | 2016-08-24 | 中国科学院广州能源研究所 | Method for separating components of straws to prepare ultralow-viscosity carboxymethyl cellulose |
| CN106750558A (en) * | 2017-02-11 | 2017-05-31 | 黑龙江八农垦大学 | A kind of degradable antibacterial film based on rice husk and preparation method thereof |
| CN107057096A (en) * | 2017-03-22 | 2017-08-18 | 汪家秀 | A kind of environmentally friendly packaging material for food and its preparation technology of the rice-straw fibre that adulterates |
| CN111945455A (en) * | 2020-07-29 | 2020-11-17 | 中北大学 | Method for extracting bran cellulose and method for preparing bran fiber membrane |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105884907A (en) * | 2016-06-29 | 2016-08-24 | 中国科学院广州能源研究所 | Method for separating components of straws to prepare ultralow-viscosity carboxymethyl cellulose |
| CN106750558A (en) * | 2017-02-11 | 2017-05-31 | 黑龙江八农垦大学 | A kind of degradable antibacterial film based on rice husk and preparation method thereof |
| CN107057096A (en) * | 2017-03-22 | 2017-08-18 | 汪家秀 | A kind of environmentally friendly packaging material for food and its preparation technology of the rice-straw fibre that adulterates |
| CN111945455A (en) * | 2020-07-29 | 2020-11-17 | 中北大学 | Method for extracting bran cellulose and method for preparing bran fiber membrane |
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