CN108102146A - A kind of preparation method of regenerated cellulose/inorganic nano material composite membrane - Google Patents
A kind of preparation method of regenerated cellulose/inorganic nano material composite membrane Download PDFInfo
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- CN108102146A CN108102146A CN201711445510.XA CN201711445510A CN108102146A CN 108102146 A CN108102146 A CN 108102146A CN 201711445510 A CN201711445510 A CN 201711445510A CN 108102146 A CN108102146 A CN 108102146A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2301/02—Cellulose; Modified cellulose
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/346—Clay
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
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Abstract
The invention discloses a kind of preparation methods of regenerated cellulose/inorganic nano material composite membrane, prepare the aqueous suspension of inorganic nano material first and it is mixed with ionic liquid aqueous solution, removes water concentration；Then the ionic liquid suspension of the inorganic nano material after above-mentioned concentration with cellulosic material is mixed, and is dehydrated, deaeration processing, obtain cellulose/inorganic nano material solution of homogeneous transparent；Above-mentioned cellulose/inorganic nano material solution is finally subjected to regeneration film forming, obtains regenerated cellulose/inorganic nano material composite membrane.The preparation method of the present invention improves the defects of conventional regeneration cellulose membrane slippery is low, pliability is poor, low temperature and high relative humidity condition performance is poor, improves the quality of cellulose membrane；Solve the problems, such as high energy consumption, the high pollution of conventional regeneration cellulose membrane preparation process simultaneously.
Description
Technical field
The present invention relates to a kind of preparation methods of regenerated cellulose/inorganic nano material composite membrane.
Background technology
Under the Environmental Protection Situation of current rigorous, the application of regenerated cellulose film is more and more wider, particularly in food and medicine bag
Dress field, cellulose membrane with its unique easy tear, easily distortion, good permeability, to print composite performance excellent and receive favor.
European and American developed countries, regenerated cellulose film dosage maximum surely belong to the meat products such as ham packaging and two big field of medical packaging,
But with the continuous improvement of production efficiency, regenerated cellulose film under particular service requirement there are slippery is low, pliability is poor,
The limitations such as low temperature and high relative humidity condition performance difference.
According to the survey, ham when meat productions or processing when, it is necessary to environment temperature below 15 DEG C, use cellulose membrane
The meat products temperature requirement of packaging is at 0-5 DEG C, and relative humidity is in 70%RH or so, under the conditions of such low temperature and high relative humidity, to fiber
The slippery requirement of plain film is quite high；In medical packaging field, the namely regenerated cellulose of consumptive material and polyethylene of full-automatic medicine dispensing machine
Composite membrane, product processing and stringent to the slippery of regenerated cellulose film, pliability requirement using process.
At present, industrial traditional cellulose membrane is prepared using multi-step, complicated adhering process.The technique is high
Energy consumption, the technology of heavily contaminated, complex process is tediously long, and condition is difficult to control, chemical kind used is more, toxicity and corrosivity are strong,
Consumption is big；Large quantity of exhaust gas can be generated in production process and acidity is big, refractory reason waste water.Therefore researcher turns to green high-efficient
Cellulose membrane production new technique, at this stage using ion liquid dissolving production cellulosic material method obtain extensive concern.
The present invention provides a kind of preparation method that regenerated cellulose/inorganic nano material composite membrane is prepared using ionic liquid as solvent,
Both solved requirement of the food medical packaging to regenerated cellulose film slippery, pliability, and in turn avoided conventional regeneration cellulose membrane
High energy consumption, the high pollution problem of preparation.
The content of the invention
The present invention provides a kind of using ionic liquid as the preparation side of regenerated cellulose/inorganic nano material composite membrane of solvent
Method improves the defects of conventional regeneration cellulose membrane slippery is low, pliability is poor, low temperature and high relative humidity condition performance is poor, improves fine
The quality of the plain film of dimension；Solve the problems, such as high energy consumption, the high pollution of conventional regeneration cellulose membrane preparation process simultaneously.
To achieve the above object, the present invention uses following technical scheme：
A kind of preparation method of regenerated cellulose/inorganic nano material composite membrane prepares the water of inorganic nano material first
It simultaneously with ionic liquid aqueous solution is mixed, removes water concentration by suspension；Then by the inorganic nano after above-mentioned concentration
The ionic liquid suspension of material is mixed with cellulosic material, and is dehydrated, deaeration processing, obtains the fibre of homogeneous transparent
Tie up element/inorganic nano material solution；Above-mentioned cellulose/inorganic nano material solution is finally subjected to regeneration film forming, is regenerated
Cellulose/inorganic nano material composite membrane.
The preparation method of above-mentioned regenerated cellulose/inorganic nano material composite membrane, specifically includes following steps：
(1) prepared by the aqueous suspension of inorganic nano material：Inorganic nano material is dispersed in water and is mixed to get uniformly
Suspension；
(2) prepared by the ionic liquid suspension of inorganic nano material：The water for the inorganic nano material that step (1) is obtained mixes
Suspension is sufficiently stirred with ionic liquid aqueous solution, carries out water removal concentration after mixing；
(3) preparation of cellulose/inorganic nano material solution：The inorganic nano that cellulosic material and step (2) are obtained
The ionic liquid suspension of material is mixed according to a certain percentage, is dehydrated after mixing, deaeration, obtains homogeneous transparent
Cellulose/inorganic nano material solution；
(4) regeneration film forming：Cellulose/inorganic nano material solution figuration prepared by step (3), and in coagulating bath again
Produced film；
(5) post-process：Cellulose membrane prepared by regeneration obtains regenerated cellulose/nothing by washing, plasticizing, dry damping
Machine nano material complex film.
Preferably, the inorganic nano material in the step (1) includes nano clay, nano-oxide, nano combined oxygen
Compound, nano metal.
Preferably, the mass percentage of inorganic nano material is 0.5-10% in the suspension of the step (1), described
Hybrid mode is stirred using high speed machine or ultrasonic power, and the mixing temperature is 30-50 DEG C, incorporation time 10-30min.
Preferably, the intermediate ion liquid of the step (2) is any one or more combination in following ionic liquid：1-
Pi-allyl -3- methylimidazole villaumites, 1- ethyl-3-methylimidazoles acetate, 1- butyl -3- methylimidazoles acetate, 1- ethyls -
3- methylimidazole villaumites, 1- ethyl-3-methylimidazoles bromide, 1- butyl -3- methylimidazole villaumites.
Preferably, the mass concentration of step (2) the intermediate ion liquid aqueous solution be 40-60%, the inorganic nano material
Material accounts for the mass percent of pure ionic liquid as 0.05-0.15%, described to be stirred the time as 10-60min.Using certain dense
The ionic liquid aqueous solution of degree is mixed with the aqueous suspension of inorganic nano material, if ionic liquid aqueous solution excessive concentration,
The viscosity of two systems differs greatly, be unfavorable for two systems mixing and inorganic nano material in ionic liquid aqueous solution
It is scattered；If ionic liquid aqueous solution concentration is too low, the dehydration load of subsequent step can be increased, increases energy consumption.
Preferably, water removal concentration is carried out in the step (2) by the way of heating in vacuum, after removing water concentration
The water content of the ionic liquid suspension of gained inorganic nano material is 90-98%.
Preferably, the mass percentage of cellulosic material is 5-15% in the step (3), and the mixing temperature is
30-60 DEG C, incorporation time 20-50min.
Preferably, the ionic liquid suspension for the inorganic nano material being uniformly mixed in the step (3) is added using vacuum
The mode of heat is dehydrated, deaeration.
Preferably, in the step (4), coagulating bath is the aqueous solution of water or ionic liquid, coagulation bath temperature 30-60
DEG C, the aqueous solution intermediate ion liquid quality percentage composition of the ionic liquid is 0-60%.
In technical solution of the present invention, inorganic nano material is used to improve slippery, the pliability of regenerated cellulose film.
The present invention advantageous effects be：The present invention uses native cellulose as raw material, using ionic liquid as solvent system
Standby regenerated cellulose film/inorganic nano composite material, without using toxic, harmful acid, alkali and volatile organic solvent,
In practical application, production process clean environment firendly, ionic liquid can recycle repeatedly, and production cost is low, and product is degradable；This hair
The bright technical solution has many advantages, such as that step is simple, easy to operation, pollution-free；Products obtained therefrom of the present invention is non-toxic and tasteless, slippery
Well, pliability is good, tensile strength is good, adapts to the automatic high-speed packaging of food, drug.
Specific embodiment
With reference to specific embodiment, the invention will be further described.
Embodiment 1
A kind of preparation method of regenerated cellulose/lithium diatomaceous earth nano material complex film, comprises the following steps：
(1) prepared by the aqueous suspension of lithium diatomaceous earth：Lithium diatomaceous earth nano material is dispersed in water, high speed dispersion 30min is obtained
Uniform suspension, the mass percentage of lithium diatomaceous earth nano material is 2%；
(2) preparation of 1- pi-allyl -3- methylimidazole villaumites (AmimCl) ionic liquid suspension of lithium diatomaceous earth：It will prepare
The aqueous suspension of good lithium diatomaceous earth is added in the ionic liquid aqueous solution that mass fraction is 60.0%, and lithium diatomaceous earth addition accounts for pure
The mass percentage 0.05% of AmimCl, is stirred 30min, then carries out water removal concentration to solution water content and is
95%；
(3) preparation of cellulose/lithium diatomaceous earth-ionic liquid solution：According to the ratio of cellulose mass percentage 10%
Cellulosic material with the AmimCl ionic liquid suspensions of the lithium diatomaceous earth after concentration is mixed, is taken off after mixing
Water, deaeration make cellulose dissolution, obtain cellulose/lithium diatomaceous earth solution of homogeneous transparent；
(4) regeneration film forming：The cellulose of homogeneous transparent/lithium diatomaceous earth solution is delivered to spray film device, by spraying film device
Spray seam by solution penetrating ionic liquid mass percentage be 10%, in the coagulating bath that temperature is 40 DEG C prepare form a film；
(5) post-process：Cellulose membrane prepared by regeneration obtains regenerated cellulose/lithium by washing, plasticizing, dry damping
Diatomaceous earth nano material complex film.
The performance indicator of regenerated cellulose/lithium diatomaceous earth nano material complex film obtained by the present invention is detected, gained is multiple
Close film performance indicator be：It is quantitative：41.5g/m2, moisture：6.2%, machine direction tensile strength：49.5N/15mm longitudinal tensile strain rate
19.4%, dry friction coefficient：0.087, wet friction coefficient：0.124, and pliability (longitudinal direction/laterally)：114/52.Examination criteria is such as
Under：It is quantitative according to《451.2 paper of GB/T and the quantitative assay method of cardboard》It is detected；Moisture according to《462 paper of GB/T and paper
The measure of plate moisture》It is detected；Tensile strength, elongation according to《The measure of 12914 paper of GB/T and cardboard tensile strength》Into
Row detection；Dry and wet coefficient of friction according to《10006 plastic films of GB and thin slice measuring friction coefficient method》It is detected；It is soft
Degree according to《The measure of 8942 paper pliabilitys of GB/T》It is detected.
Reference examples 1
A kind of preparation method for the regenerated cellulose film for not adding inorganic nano material, comprises the following steps：
(1) prepared by cellulose/1- pi-allyl -3- methylimidazole villaumites (AmimCl) ionic liquid solution：According to cellulose
The ratio of mass percentage 10% mixes cellulosic material with 95% AmimCl aqueous solution rows, is taken off after mixing
Water, deaeration make cellulose dissolution, obtain the cellulose-AmimCl solution of homogeneous transparent.
(2) regeneration film forming：Cellulose-AmimCl the solution of homogeneous transparent is delivered to spray film device, by spraying film device
Spray seam by solution penetrating ionic liquid mass percentage be 10%, in the coagulating bath that temperature is 40 DEG C prepare form a film.
(3) post-process：Cellulose membrane prepared by regeneration obtains regenerated cellulose film by washing, plasticizing, dry damping.
The performance indicator of gained regenerated cellulose film is detected, the performance indicator of gained film is：It is quantitative：41.0g/
m2, moisture：6.0%, machine direction tensile strength：47.5N/15mm longitudinal tensile strain rate 20.1%, dry friction coefficient：0.3, wet friction
Coefficient：0.5, and pliability (longitudinal direction/laterally)：160/85.Examination criteria is as follows：It is quantitative according to《451.2 paper of GB/T and cardboard are determined
The assay method of amount》It is detected；Moisture according to《The measure of 462 paper of GB/T and moisture of paper board》It is detected；Tensile strength,
Elongation according to《The measure of 12914 paper of GB/T and cardboard tensile strength》It is detected；Dry and wet coefficient of friction according to《GB
10006 plastic films and thin slice measuring friction coefficient method》It is detected；Pliability according to《8942 paper pliabilitys of GB/T
It measures》It is detected.
It is compared by embodiment 1 and reference examples 1, regenerated cellulose/nano material complex film of 1 gained of the embodiment of the present invention
Tensile strength improve, have good slippery and pliability.
Embodiment 2
A kind of preparation method of regenerated cellulose/silica nano material composite membrane, comprises the following steps：
(1) prepared by the aqueous suspension of silica：Silica nano material is dispersed in water, high speed dispersion 15min,
Uniform suspension is obtained, the mass percentage of silica nano material is 0.5%；
(2) preparation of 1- butyl -3- methylimidazoles acetate (BmimAc) ionic liquid suspension of silica：It will system
The aqueous suspension for the silica got ready is added in the ionic liquid aqueous solution that mass fraction is 40.0%, and silica adds in
Amount accounts for the mass percentage 0.15% of pure BmimAc, is stirred 50min, and it is aqueous to solution then to carry out water removal concentration
It measures as 98%；
(3) preparation of cellulose/silica-ionic liquid solution：According to the ratio of cellulose mass percentage 15%
Example mixes cellulosic material with the ionic liquid suspension of the silica after concentration, be dehydrated after mixing,
Deaeration makes cellulose dissolution, obtains cellulose/silicon dioxde solution of homogeneous transparent；
(4) regeneration film forming：Cellulose/silicon dioxde solution of homogeneous transparent is delivered to spray film device, is filled by spraying film
Solution penetrating ionic liquid mass percentage is 60%, is prepared into film in the coagulating bath that temperature is 60 DEG C by the spray seam put；
(5) post-process：Cellulose membrane prepared by regeneration obtains regenerated cellulose/bis- by washing, plasticizing, dry damping
Silica nano material complex film.
The performance indicator of regenerated cellulose film/silicon dioxide nano composite material obtained by the present invention is detected, gained
The performance indicator of regenerated cellulose film/silicon dioxide nano composite material is：It is quantitative：30.2g/m2, moisture：6.0%, longitudinal direction is anti-
Zhang Qiangdu：41.2N/15mm longitudinal tensile strain rate 16.8%, dry friction coefficient：0.156, and pliability (longitudinal direction/laterally)：90/50.
Examination criteria is as follows：It is quantitative according to《451.2 paper of GB/T and the quantitative assay method of cardboard》It is detected；Moisture according to《GB/T
The measure of 462 paper and moisture of paper board》It is detected；Tensile strength, elongation according to《12914 paper of GB/T and cardboard tensile strength
Measure》It is detected；Dry and wet coefficient of friction according to《10006 plastic films of GB and thin slice measuring friction coefficient method》It carries out
Detection；Pliability according to《The measure of 8942 paper pliabilitys of GB/T》It is detected.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all skills in the present invention
On the basis of art scheme, the various modifications or variations that can be made by those skilled in the art with little creative work still exists
In protection scope of the present invention.
Claims (10)
1. the preparation method of a kind of regenerated cellulose/inorganic nano material composite membrane, which is characterized in that prepare inorganic nano first
It simultaneously with ionic liquid aqueous solution is mixed, removes water concentration by the aqueous suspension of material；It then will be after above-mentioned concentration
The ionic liquid suspension of inorganic nano material is mixed with cellulosic material, and is dehydrated, deaeration processing, is obtained uniformly
Transparent cellulose/inorganic nano material solution；Above-mentioned cellulose/inorganic nano material solution is finally subjected to regeneration film forming,
Obtain regenerated cellulose/inorganic nano material composite membrane.
2. a kind of preparation method of regenerated cellulose/inorganic nano material composite membrane according to claim 1, feature exist
In specifically including following steps：
(1) prepared by the aqueous suspension of inorganic nano material：Inorganic nano material is dispersed in water and is mixed to get uniform suspension
Liquid；
(2) prepared by the ionic liquid suspension of inorganic nano material：The aqueous suspension for the inorganic nano material that step (1) is obtained
It is sufficiently stirred with ionic liquid aqueous solution, carries out water removal concentration after mixing；
(3) preparation of cellulose/inorganic nano material solution：The inorganic nano material that cellulosic material and step (2) are obtained
Ionic liquid suspension mixed according to a certain percentage, be dehydrated after mixing, deaeration, obtain the fibre of homogeneous transparent
Tie up element/inorganic nano material solution；
(4) regeneration film forming：Cellulose/inorganic nano material solution figuration prepared by step (3), and regenerated in coagulating bath
Film；
(5) post-process：Cellulose membrane prepared by regeneration obtains regenerated cellulose/inorganic and receives by washing, plasticizing, dry damping
Rice Material cladding film.
3. a kind of preparation method of regenerated cellulose/inorganic nano material composite membrane according to claim 2, feature exist
In the inorganic nano material in the step (1) includes nano clay, nano-oxide, nano composite oxide, nanogold
Belong to.
4. a kind of preparation method of regenerated cellulose/inorganic nano material composite membrane according to claim 2, feature exist
In the mass percentage of inorganic nano material is 0.5-10% in the suspension of the step (1), and the hybrid mode uses
High speed machine stirs or ultrasonic power, and the mixing temperature is 30-50 DEG C, incorporation time 10-30min.
5. a kind of preparation method of regenerated cellulose/inorganic nano material composite membrane according to claim 2, feature exist
In the intermediate ion liquid of the step (2) is any one or more combination in following ionic liquid：1- pi-allyl -3- first
Base imidazoles villaumite, 1- ethyl-3-methylimidazoles acetate, 1- butyl -3- methylimidazoles acetate, 1- ethyl-3-methylimidazoles
Villaumite, 1- ethyl-3-methylimidazoles bromide, 1- butyl -3- methylimidazole villaumites.
6. a kind of preparation method of regenerated cellulose/inorganic nano material composite membrane according to claim 2, feature exist
In the mass concentration of step (2) the intermediate ion liquid aqueous solution is 40-60%, and the inorganic nano material accounts for pure ionic liquid
The mass percent of body is 0.05-0.15%, described to be stirred the time as 10-60min.
7. a kind of preparation method of regenerated cellulose/inorganic nano material composite membrane according to claim 2, feature exist
In the step (2) is middle to carry out water removal concentration by the way of heating in vacuum, removes water gained inorganic nano after concentration
The water content of the ionic liquid suspension of material is 90-98%.
8. a kind of preparation method of regenerated cellulose/inorganic nano material composite membrane according to claim 2, feature exist
In the mass percentage of cellulosic material is 5-15% in the step (3), and the mixing temperature is 30-60 DEG C, during mixing
Between be 20-50min.
9. a kind of preparation method of regenerated cellulose/inorganic nano material composite membrane according to claim 2, feature exist
In, in the step (3) be uniformly mixed inorganic nano material ionic liquid suspension be dehydrated by the way of heating in vacuum,
Deaeration.
10. a kind of preparation method of regenerated cellulose/inorganic nano material composite membrane according to claim 2, feature
It is, coagulating bath is water or the aqueous solution of ionic liquid in the step (4), and coagulation bath temperature is 30-60 DEG C, the ionic liquid
The aqueous solution intermediate ion liquid quality percentage composition of body is 0-60%.
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Cited By (1)
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| CN109942868A (en) * | 2019-02-25 | 2019-06-28 | 王雪峰 | A kind of preparation method of waterproof tensile fiber type element packaging film |
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Effective date of registration: 20200821 Address after: 261100 North District of Lingang Industrial Park, Guti sub district office, Hanting District, Weifang City, Shandong Province Applicant after: Shandong Zhongke Heng Lian biological base material Co.,Ltd. Applicant after: INSTITUTE OF CHEMISTRY, CHINESE ACADEMY OF SCIENCES Address before: Dragon Road, 261100 Shandong city of Weifang province Hanting District No. 328 Applicant before: SHANDONG HENGLIAN NEW MATERIALS Co.,Ltd. Applicant before: INSTITUTE OF CHEMISTRY, CHINESE ACADEMY OF SCIENCES |
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