CN109576810A - A kind of preparation method of carboxymethylated cellulosic nanofibrils - Google Patents
A kind of preparation method of carboxymethylated cellulosic nanofibrils Download PDFInfo
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- CN109576810A CN109576810A CN201811487460.6A CN201811487460A CN109576810A CN 109576810 A CN109576810 A CN 109576810A CN 201811487460 A CN201811487460 A CN 201811487460A CN 109576810 A CN109576810 A CN 109576810A
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
- D01F2/24—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from cellulose derivatives
- D01F2/28—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from cellulose derivatives from organic cellulose esters or ethers, e.g. cellulose acetate
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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Abstract
The invention discloses a kind of preparation methods of carboxymethylated cellulosic nanofibrils, include the following steps: to clean carboxymethyl cellulose, filtering and drying, then reactor is added, it is added in citric acid solution, 75-85 degrees Celsius at a temperature of at the uniform velocity stir 120-180min, then it filters, it is dried under 70-80 degrees Celsius of oven environment again, and it is mixed in 40-55 degrees Celsius of environment, graphene slurry and mixed aid will be added in slurry after the displacement of environment acid, and under conditions of 35-40 degrees Celsius after mixing, obtain mixed slurry, then it is added in deionized water and carboxymethyl cellulose into mixed slurry after being dispersed with stirring, and 2h is placed in the environment of room temperature.The invention can avoid the pollutions to environment, and are not necessarily to a large amount of water to dialyse compared with the mechanical the preparation method without chemical pretreatment, and preparation condition is mild, easy to operate, at low cost and pollution is small.
Description
Technical field
The present invention relates to nanofibrils preparation technical field more particularly to a kind of systems of carboxymethylated cellulosic nanofibrils
Preparation Method.
Background technique
Carboxymethyl cellulose is that the polysaccharide most wide, content is most, source very abundant are distributed in nature.Current fibre
The modification technology of element is concentrated mainly on two aspect of etherificate and esterification.Carboxymethylation reaction is one kind of etherification technology.Cellulose warp
Obtained after carboxy methylation carboxymethyl cellulose (CMC), aqueous solution have thickening, film forming, gluing, water tariff collection, colloid protect,
The effects of emulsification and suspension, it is widely used in the industries such as petroleum, food, medicine, textile and paper, is most important cellulose ether
One of class.Traditional technology is not practical natural material in the preparation, excessively high so as to cause cost, and the utilization rate of waste
It is not high.For this purpose, we have proposed a kind of preparation methods of carboxymethylated cellulosic nanofibrils.
Summary of the invention
The invention proposes a kind of preparation methods of carboxymethylated cellulosic nanofibrils, to solve in above-mentioned background technique
The problem of proposition.
The invention proposes a kind of preparation methods of carboxymethylated cellulosic nanofibrils, include the following steps:
S1: raw material is chosen, and chooses carboxymethyl cellulose, acetylbutyrylcellulose, polyacrylonitrile-based carbon fibre, graphene slurry
Material and mixed aid, and the not homogeneous raw material of selection stored respectively spare into sterile normal temperature environment；
S2: a certain amount of carboxymethyl cellulose is chosen in proportion, and is placed it in cleaning device, at 32-38 degrees Celsius
Environment in cleaned, after the completion, be filtered and dry, by the carboxymethyl cellulose after over cleaning, filtering, drying
Reactor is added, it is molten that the citric acid that concentration is 0.5-1mol/L is added by the carboxymethyl cellulose of solid-to-liquid ratio 1-20:10-15g/ml
In liquid, 75-85 degrees Celsius at a temperature of at the uniform velocity stir 120-180min, then filter, and adopt and be washed with deionized at least 3
It is secondary, it is dried under 70-80 degrees Celsius of oven environment again, and drying time is 2h, it is 60- that partial size is ground to after cooling
80 μm, modified carboxy methyl cellulose can be obtained；
S3: modified carboxy methyl cellulose obtained in S2 is placed in sterile container, and adds acetate butyrate thereto
Cellulose and polyacrylonitrile-based carbon fibre are placed in one, and are mixed in 40-55 degrees Celsius of environment, and stir
Time is 15-30min, is subsequently placed in acidic environment and stands 120-180min, complete so as to utilize environment acid replacement Treatment
Cheng Hou obtains slurry；
S4: graphene slurry and mixed aid, and 35-40 degrees Celsius of item will be added in the slurry after the displacement of environment acid
Under part after mixing, mixed slurry is obtained, is then added in deionized water and carboxymethyl cellulose and stirs into mixed slurry
After dispersion, and 2h is placed in the environment of room temperature, washes off extra citric acid using clear water, obtain wet feed；
S5: after carrying out high speed shear, friction treatment to treated in S4 wet feed, nanoporous is obtained by freeze-drying
Conduit filtration catalytic carrier fibre, at white powder object, as carboxymethylated cellulosic nanofibrils.
Preferably, the pH value of the white powder object in S5 is neutrality.
Preferably, the carboxymethyl cellulose in S1, acetylbutyrylcellulose, polyacrylonitrile-based carbon fibre, graphene slurry
The molal weight ratio of material and mixed aid is 10:1:1:0.5:0.1.
Preferably, the mixed aid is specially the mixture of fire retardant, corrosion-resistant agent, binder and catalyst,
And fire retardant, corrosion-resistant agent, binder and catalyst molal weight ratio be 2:1:0.1:0.1.
Preferably, the partial size of the carboxymethylated cellulosic nanofibrils is 10 μm or more and 1cm is hereinafter, bulk density is
0.20g/cm3More than, and middle pore volume is 0.10cm3/ g or more.
A kind of preparation method of carboxymethylated cellulosic nanofibrils proposed by the present invention, beneficial effect are:
(1), air is adsorbed using the design feature after citric acid-modified, after citric acid-modified, carboxymethyl
Impurity in cellulose duct itself is dissolved, and a large amount of holes occurs, to greatly improve adsorption efficiency.And carboxymethyl cellulose
Plain raw material cotton China reserves very abundant, it is cheap, and effect is preferable, it is pollution-free.
(2), it is analyzed from angle of sustainable development, the carboxymethyl cellulose used can be mentioned from forestry waste
It takes, the method increase the utilization rates of forestry waste, reduce the waste of natural plant fibre raw material, meet energy-saving and emission-reduction
It is required that advantageously accounting for the problem that China's forest resourceies are increasingly reduced, resource utilization is not high.
(3), it is analyzed from economic benefit, using forestry waste as raw material, low production cost promotes its output value, tool
There are preferable social benefit and environmental benefit.
(4), the present invention is relative to traditional use organic solution and mineral acid hydrolysis method, and there is no remaining in preparation system
Acid, avoid pollution of the acid to environment, and dialyse without a large amount of water；It is made with without the machinery of chemical pretreatment
Standby method is compared, and preparation condition is mild, easy to operate, at low cost and pollution is small；With wide industrial applications prospect.
Specific embodiment
It is next combined with specific embodiments below that the present invention will be further described.
Embodiment 1
The invention proposes a kind of preparation methods of carboxymethylated cellulosic nanofibrils, include the following steps:
S1: raw material is chosen, and chooses carboxymethyl cellulose, acetylbutyrylcellulose, polyacrylonitrile-based carbon fibre, graphene slurry
Material and mixed aid, and the not homogeneous raw material of selection stored respectively spare into sterile normal temperature environment；
S2: a certain amount of carboxymethyl cellulose is chosen in proportion, and is placed it in cleaning device, at 32-38 degrees Celsius
Environment in cleaned, after the completion, be filtered and dry, by the carboxymethyl cellulose after over cleaning, filtering, drying
Reactor is added, it is molten that the citric acid that concentration is 0.5-1mol/L is added by the carboxymethyl cellulose of solid-to-liquid ratio 1-20:10-15g/ml
In liquid, 75 degrees Celsius at a temperature of at the uniform velocity stir 120min, then filter, and adopt and be washed with deionized at least 3 times, again
It is dried under 70 degrees Celsius of oven environment, and drying time is 2h, it is 60-80 μm that partial size is ground to after cooling, can
Obtain modified carboxy methyl cellulose；
S3: modified carboxy methyl cellulose obtained in S2 is placed in sterile container, and adds acetate butyrate thereto
Cellulose and polyacrylonitrile-based carbon fibre are placed in one, and are mixed in 40 degrees Celsius of environment, and when stirring
Between be 15min, be subsequently placed in acidic environment and stand 120min, so as to be obtained after the completion using environment acid replacement Treatment
Slurry；
S4: graphene slurry and mixed aid, and 35 degrees Celsius of condition will be added in the slurry after the displacement of environment acid
Under after mixing, obtain mixed slurry, stirring point in deionized water and carboxymethyl cellulose be then added into mixed slurry
After dissipating, and 2h is placed in the environment of room temperature, washes off extra citric acid using clear water, obtain wet feed；
S5: after carrying out high speed shear, friction treatment to treated in S4 wet feed, nanoporous is obtained by freeze-drying
Conduit filtration catalytic carrier fibre, at white powder object, as carboxymethylated cellulosic nanofibrils.
The pH value of white powder object in S5 is neutrality.
Carboxymethyl cellulose, acetylbutyrylcellulose, polyacrylonitrile-based carbon fibre, graphene slurry in S1 and mixed
The molal weight ratio for closing auxiliary agent is 10:1:1:0.5:0.1.
The mixed aid is specially the mixture of fire retardant, corrosion-resistant agent, binder and catalyst, and fire-retardant
Agent, corrosion-resistant agent, binder and catalyst molal weight ratio be 2:1:0.1:0.1.
The partial size of the carboxymethylated cellulosic nanofibrils is 10 μm or more and 1cm is hereinafter, bulk density is 0.20g/cm3
More than, and middle pore volume is 0.10cm3/ g or more.
Embodiment 2
The invention proposes a kind of preparation methods of carboxymethylated cellulosic nanofibrils, include the following steps:
S1: raw material is chosen, and chooses carboxymethyl cellulose, acetylbutyrylcellulose, polyacrylonitrile-based carbon fibre, graphene slurry
Material and mixed aid, and the not homogeneous raw material of selection stored respectively spare into sterile normal temperature environment；
S2: choosing a certain amount of carboxymethyl cellulose in proportion, and place it in cleaning device, in 34 degrees Celsius of ring
It is cleaned in border, after the completion, is filtered and dries, the carboxymethyl cellulose after over cleaning, filtering, drying is added
The citric acid solution that concentration is 0.5-1mol/L is added by the carboxymethyl cellulose of solid-to-liquid ratio 1-20:10-15g/ml in reactor
In, 78 degrees Celsius at a temperature of at the uniform velocity stir 140min, then filter, and adopt and be washed with deionized at least 3 times, exist again
It is dried under 74 degrees Celsius of oven environment, and drying time is 2h, it is 60-80 μm that partial size is ground to after cooling, can be obtained
To modified carboxy methyl cellulose；
S3: modified carboxy methyl cellulose obtained in S2 is placed in sterile container, and adds acetate butyrate thereto
Cellulose and polyacrylonitrile-based carbon fibre are placed in one, and are mixed in 45 degrees Celsius of environment, and when stirring
Between be 20min, be subsequently placed in acidic environment and stand 140min, so as to be obtained after the completion using environment acid replacement Treatment
Slurry；
S4: graphene slurry and mixed aid, and the condition of 36 degrees Celsius will be added in the slurry after the displacement of environment acid
Under after mixing, obtain mixed slurry, stirring point in deionized water and carboxymethyl cellulose be then added into mixed slurry
After dissipating, and 2h is placed in the environment of room temperature, washes off extra citric acid using clear water, obtain wet feed；
S5: after carrying out high speed shear, friction treatment to treated in S4 wet feed, nanoporous is obtained by freeze-drying
Conduit filtration catalytic carrier fibre, at white powder object, as carboxymethylated cellulosic nanofibrils.
The pH value of white powder object in S5 is neutrality.
Carboxymethyl cellulose, acetylbutyrylcellulose, polyacrylonitrile-based carbon fibre, graphene slurry in S1 and mixed
The molal weight ratio for closing auxiliary agent is 10:1:1:0.5:0.1.
The mixed aid is specially the mixture of fire retardant, corrosion-resistant agent, binder and catalyst, and fire-retardant
Agent, corrosion-resistant agent, binder and catalyst molal weight ratio be 2:1:0.1:0.1.
The partial size of the carboxymethylated cellulosic nanofibrils is 10 μm or more and 1cm is hereinafter, bulk density is 0.20g/cm3
More than, and middle pore volume is 0.10cm3/ g or more.
Embodiment 3
The invention proposes a kind of preparation methods of carboxymethylated cellulosic nanofibrils, include the following steps:
S1: raw material is chosen, and chooses carboxymethyl cellulose, acetylbutyrylcellulose, polyacrylonitrile-based carbon fibre, graphene slurry
Material and mixed aid, and the not homogeneous raw material of selection stored respectively spare into sterile normal temperature environment；
S2: choosing a certain amount of carboxymethyl cellulose in proportion, and place it in cleaning device, in the ring of 36 degrees Celsius
It is cleaned in border, after the completion, is filtered and dries, the carboxymethyl cellulose after over cleaning, filtering, drying is added
The citric acid solution that concentration is 0.5-1mol/L is added by the carboxymethyl cellulose of solid-to-liquid ratio 1-20:10-15g/ml in reactor
In, 82 degrees Celsius at a temperature of at the uniform velocity stir 160min, then filter, and adopt and be washed with deionized at least 3 times, exist again
It is dried under 77 degrees Celsius of oven environment, and drying time is 2h, it is 60-80 μm that partial size is ground to after cooling, can be obtained
To modified carboxy methyl cellulose；
S3: modified carboxy methyl cellulose obtained in S2 is placed in sterile container, and adds acetate butyrate thereto
Cellulose and polyacrylonitrile-based carbon fibre are placed in one, and are mixed in 50 degrees Celsius of environment, and when stirring
Between be 25min, be subsequently placed in acidic environment and stand 160min, so as to be obtained after the completion using environment acid replacement Treatment
Slurry；
S4: graphene slurry and mixed aid, and 38 degrees Celsius of condition will be added in the slurry after the displacement of environment acid
Under after mixing, obtain mixed slurry, stirring point in deionized water and carboxymethyl cellulose be then added into mixed slurry
After dissipating, and 2h is placed in the environment of room temperature, washes off extra citric acid using clear water, obtain wet feed；
S5: after carrying out high speed shear, friction treatment to treated in S4 wet feed, nanoporous is obtained by freeze-drying
Conduit filtration catalytic carrier fibre, at white powder object, as carboxymethylated cellulosic nanofibrils.
The pH value of white powder object in S5 is neutrality.
Carboxymethyl cellulose, acetylbutyrylcellulose, polyacrylonitrile-based carbon fibre, graphene slurry in S1 and mixed
The molal weight ratio for closing auxiliary agent is 10:1:1:0.5:0.1.
The mixed aid is specially the mixture of fire retardant, corrosion-resistant agent, binder and catalyst, and fire-retardant
Agent, corrosion-resistant agent, binder and catalyst molal weight ratio be 2:1:0.1:0.1.
The partial size of the carboxymethylated cellulosic nanofibrils is 10 μm or more and 1cm is hereinafter, bulk density is 0.20g/cm3
More than, and middle pore volume is 0.10cm3/ g or more.
Embodiment 4
The invention proposes a kind of preparation methods of carboxymethylated cellulosic nanofibrils, include the following steps:
S1: raw material is chosen, and chooses carboxymethyl cellulose, acetylbutyrylcellulose, polyacrylonitrile-based carbon fibre, graphene slurry
Material and mixed aid, and the not homogeneous raw material of selection stored respectively spare into sterile normal temperature environment；
S2: choosing a certain amount of carboxymethyl cellulose in proportion, and place it in cleaning device, in 38 degrees Celsius of ring
It is cleaned in border, after the completion, is filtered and dries, the carboxymethyl cellulose after over cleaning, filtering, drying is added
The citric acid solution that concentration is 0.5-1mol/L is added by the carboxymethyl cellulose of solid-to-liquid ratio 1-20:10-15g/ml in reactor
In, 85 degrees Celsius at a temperature of at the uniform velocity stir 180min, then filter, and adopt and be washed with deionized at least 3 times, exist again
It is dried under 80 degrees Celsius of oven environment, and drying time is 2h, it is 60-80 μm that partial size is ground to after cooling, can be obtained
To modified carboxy methyl cellulose；
S3: modified carboxy methyl cellulose obtained in S2 is placed in sterile container, and adds acetate butyrate thereto
Cellulose and polyacrylonitrile-based carbon fibre are placed in one, and are mixed in 55 degrees Celsius of environment, and when stirring
Between be 30min, be subsequently placed in acidic environment and stand 180min, so as to be obtained after the completion using environment acid replacement Treatment
Slurry；
S4: graphene slurry and mixed aid, and 40 degrees Celsius of condition will be added in the slurry after the displacement of environment acid
Under after mixing, obtain mixed slurry, stirring point in deionized water and carboxymethyl cellulose be then added into mixed slurry
After dissipating, and 2h is placed in the environment of room temperature, washes off extra citric acid using clear water, obtain wet feed；
S5: after carrying out high speed shear, friction treatment to treated in S4 wet feed, nanoporous is obtained by freeze-drying
Conduit filtration catalytic carrier fibre, at white powder object, as carboxymethylated cellulosic nanofibrils.
The pH value of white powder object in S5 is neutrality.
Carboxymethyl cellulose, acetylbutyrylcellulose, polyacrylonitrile-based carbon fibre, graphene slurry in S1 and mixed
The molal weight ratio for closing auxiliary agent is 10:1:1:0.5:0.1.
The mixed aid is specially the mixture of fire retardant, corrosion-resistant agent, binder and catalyst, and fire-retardant
Agent, corrosion-resistant agent, binder and catalyst molal weight ratio be 2:1:0.1:0.1.
The partial size of the carboxymethylated cellulosic nanofibrils is 10 μm or more and 1cm is hereinafter, bulk density is 0.20g/cm3
More than, and middle pore volume is 0.10cm3/g or more.
The present invention is relative to traditional use organic solution and mineral acid hydrolysis method, and there is no remainings in preparation system
Acid avoids pollution of the acid to environment, and is not necessarily to a large amount of water to dialyse；It is prepared with without the machinery of chemical pretreatment
Method is compared, and preparation condition is mild, easy to operate, at low cost and pollution is small；With wide industrial applications prospect.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (5)
1. a kind of preparation method of carboxymethylated cellulosic nanofibrils, which comprises the following steps:
S1: raw material choose, choose carboxymethyl cellulose, acetylbutyrylcellulose, polyacrylonitrile-based carbon fibre, graphene slurry with
And mixed aid, and the not homogeneous raw material of selection stored respectively spare into sterile normal temperature environment；
S2: choosing a certain amount of carboxymethyl cellulose in proportion, and place it in cleaning device, in 32-38 degrees Celsius of ring
It is cleaned in border, after the completion, is filtered and dries, the carboxymethyl cellulose after over cleaning, filtering, drying is added
The citric acid solution that concentration is 0.5-1mol/L is added by the carboxymethyl cellulose of solid-to-liquid ratio 1-20:10-15g/ml in reactor
In, 75-85 degrees Celsius at a temperature of at the uniform velocity stir 120-180min, then filter, and adopt and be washed with deionized at least 3
It is secondary, it is dried under 70-80 degrees Celsius of oven environment again, and drying time is 2h, it is 60- that partial size is ground to after cooling
80 μm, modified carboxy methyl cellulose can be obtained；
S3: modified carboxy methyl cellulose obtained in S2 being placed in sterile container, and adds acetate butyrate fiber thereto
Element and polyacrylonitrile-based carbon fibre are placed in one, and are mixed in 40-55 degrees Celsius of environment, and mixing time
It for 15-30min, is subsequently placed in acidic environment and stands 120-180min, so as to utilize environment acid replacement Treatment, complete
Afterwards, slurry is obtained；
S4: graphene slurry and mixed aid will be added in the slurry after the displacement of environment acid, and under conditions of 35-40 degrees Celsius
After mixing, mixed slurry is obtained, is then added in deionized water and carboxymethyl cellulose and is dispersed with stirring into mixed slurry
Afterwards, and in the environment of room temperature 2h is placed, washes off extra citric acid using clear water, obtains wet feed；
S5: after carrying out high speed shear, friction treatment to treated in S4 wet feed, nanoporous conduit is obtained by freeze-drying
Filtration catalytic carrier fibre, at white powder object, as carboxymethylated cellulosic nanofibrils.
2. a kind of preparation method of carboxymethylated cellulosic nanofibrils according to claim 1, it is characterised in that: in S5
In white powder object pH value be neutrality.
3. a kind of preparation method of carboxymethylated cellulosic nanofibrils according to claim 1, it is characterised in that: in S1
In carboxymethyl cellulose, acetylbutyrylcellulose, polyacrylonitrile-based carbon fibre, graphene slurry and mixed aid mole
Mass ratio is 10:1:1:0.5:0.1.
4. a kind of preparation method of carboxymethylated cellulosic nanofibrils according to claim 1, it is characterised in that: described
Mixed aid be specially fire retardant, corrosion-resistant agent, binder and catalyst mixture, and it is fire retardant, corrosion-resistant agent, viscous
The molal weight ratio for tying agent and catalyst is 2:1:0.1:0.1.
5. a kind of preparation method of carboxymethylated cellulosic nanofibrils according to claim 1, it is characterised in that: described
The partial size of carboxymethylated cellulosic nanofibrils is 10 μm or more and 1cm is hereinafter, bulk density is 0.20g/cm3More than, and in
Pore volume is 0.10cm3/ g or more.
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| CN111172615A (en) * | 2020-01-20 | 2020-05-19 | 天津科技大学 | Flame-retardant nano-cellulose composite fiber prepared by wet spinning and preparation process thereof |
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