CN108864630A - A method of composite membrane is prepared using coffee shell - Google Patents
A method of composite membrane is prepared using coffee shell Download PDFInfo
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- CN108864630A CN108864630A CN201810791841.7A CN201810791841A CN108864630A CN 108864630 A CN108864630 A CN 108864630A CN 201810791841 A CN201810791841 A CN 201810791841A CN 108864630 A CN108864630 A CN 108864630A
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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
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2333/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
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Abstract
The invention discloses a kind of methods for preparing composite membrane using coffee shell, are related to Novel environment-friendlymaterial material field, include the following steps：(1) coffee shell crushes；(2) acid oxidase is handled；(3) hydrogen peroxide surface oxidation treatment；(4) alkali impregnates；(5) preparation of coffee case fibre element；(6) preparation of coffee shell nano-cellulose；(7) preparation of coffee shell nano-cellulose film；(8) preparation of composite membrane；The present invention is using coffee shell as raw material, after being impregnated using acidic oxidation and alkali, after activating coffee shell surface, it grinds and coffee shell nano-cellulose is made, coffee case fibre element film is made after dilution filters to impregnate in acrylic resin, composite membrane is made, there is good translucidus and toughness, can be applied to the wide range of areas such as Electronic Paper.
Description
Technical field
The present invention relates to Novel environment-friendlymaterial material fields, and in particular to a method of composite membrane is prepared using coffee shell.
Background technique
Coffee is instantly popular one of main drink, thus coffee tree is worldwide planted extensively again.According to statistics,
2016, which are only Yunnan Province of China, saves coffee total output up to 140,000 tons, and it is remaining to generate a large amount of processing during preliminary working for coffee
Product, such as pericarp, pectin, beans shell and waste water；Coffee bean shell, if coffee bean shell does not have as waste a kind of in production process
It is handled by scientific and effective, is not only resulted in waste of resources, but also bring serious pollution to environment.Therefore, for preferably
Solve the problems, such as this, more and more scientific research scholar open types are keen to study the potential use of coffee shell in recent years.
Chinese patent CN104119136A discloses the culture medium for golden mushroom and preparation method thereof that a kind of coffee shell is raw material,
It is made from the following raw materials in parts by weight：Coffee shell 30-35, hardwood sawdust 50-55, wood shavings 20-22, straw powder 35-40, tea seed
Powder 12-15, Apple Seeds powder 18-20, corn flour 14-15, laterite 15-16, humic acid potassium 0.4-0.5, cellulose ether 0.3-0.4,
Wilsonii 2-3, perilla leaf 3-4, Radix Angelicae Sinensis 1-2, cassia seed 4-5, flower of kudzuvine 3-4, male and female grass 2-3, nutritional additive 6-7.The present invention
There are certain water imbibition and preferable drainage properties using coffee shell, replace part sawdust using it, widened raw material
Available sources, at the same in the life such as solve the problems, such as coffee shell, stalk waste recycling.
Chinese patent CN106540655A discloses a kind of microwave and the composite modified coffee shell of activator prepares formaldehyde absorbing
The method of agent obtains composite activating agent firstly, potassium hydroxide solution is mixed with liquor alumini chloridi；Then, by coffee shell and again
Close activator be mixed in a certain ratio, impregnate after dry, heated after drying, obtain carbonized material, carbonized material is placed in microwave heating
In reactor, it is passed through steam heating, material is washed with hydrochloric acid solution and is in neutrality, is washed and is detected until with pH test paper
Carbonized material is neutrality, and material is dried.Using microwave and the composite modified coffee shell of activator, coffee shell formaldehyde adsorption is optimized
Performance provides a kind of preparation method of novel air cleanser, realizes the resource recycling of coffee shell, there is good ring
Border benefit and application prospect.
Summary of the invention
Aiming at the problems existing in the prior art, the present invention provides a kind of method for preparing composite membrane using coffee shell,
The present invention is using coffee shell as raw material, after being impregnated using acidic oxidation and alkali, after activating coffee shell surface, grinds obtained coffee shell and receives
Rice cellulose is made coffee case fibre element film after dilution filters and impregnates in acrylic resin, composite membrane is made, and has good
Translucidus and toughness, can be applied to the wide range of areas such as Electronic Paper.
In order to achieve the above object, the present invention is achieved through the following technical solutions：
A method of composite membrane being prepared using coffee shell, is included the following steps：
(1) coffee shell is put into pulverizer summarizes and crush, cross 80-100 mesh to get coffee shell powder；
(2) coffee shell powder is added in the liquor natrii hypochloritis of mass fraction 1.5%, is uniformly mixed, appropriate ice is added
Acetic acid is adjusted to pH value to 4-5, is placed in temperature control in water-bath and, with 400-600 revs/min of speed, stirs mixed to 72-78 degrees Celsius
Reaction 4-5 hours is closed, filtering, it is neutral that filtrate, which is cleaned repeatedly with deionized water to filtrate,；
(3) product made from step (2) is put into 2% hydrogen peroxide of mass fraction, is uniformly mixed, merging 80 is Celsius
It in the water bath with thermostatic control of degree, handles 2-3 hours, filtering cleans filtrate 3-5 times with deionized water repeatedly；
(4) product made from step (3) is added in potassium hydroxide solution, after impregnating 12 hours, is put into 95 DEG C waters
Heating stirring 2 hours in bath, filtering, it is neutral that filtrate, which is cleaned repeatedly with deionized water to filtrate,；
(5) liquor natrii hypochloritis of mass fraction 1.5% is added in product made from step (4) and is uniformly mixed, is added
Glacial acetic acid is stirred reaction, until product surface, at white, filtering is cleaned repeatedly with filtrate to filtrate to solution pH value to 4-5
To neutrality to get coffee case fibre element；
(6) step (5) coffee case fibre element is added in superfine powder grinder, with 500-600 revs/min of speed, is ground
Mill 15-20 hours, obtains coffee shell nano-cellulose；
(7) coffee shell nano-cellulose made from step (6) is weighed, being diluted with water to concentration is 0.2%, stirs 30 points
Clock keeps its evenly dispersed, and vacuum filtration removes moisture removal, obtains wet film；Wet film is taken out, is placed between two panels metal mesh, by metal
Net is placed between two pieces of glass plates after pressing, is placed in drying in baking oven and is taken out to get coffee shell nano fibrous membrane；
(8) coffee shell nano fibrous membrane is put into alcohol and is impregnated, to remove surface impurity, take out nanometer coir fibre film
It after air-drying, is placed in acrylic resin soln, after thin-film transparent, taking-up, which is placed in two blocks of sheet glass, to be flattened, by ultra-violet curing
Machine solidifies to get composite membrane.
Preferably, the dosage quality of the liquor natrii hypochloritis of the mass fraction 1.5% in the step (2) and coffee shell powder
Than being 20:1.
Preferably, the method in the step (2) in liquor natrii hypochloritis's addition coffee shell of mass fraction 1.5% is：
The sodium hypochlorite of mass fraction 1.5% is divided into 4 parts, the hypochlorous acid of a mass fraction 1.5% was added at interval of one hour
Sodium solution, and at the same time suitable glacial acetic acid, which is added, is adjusted to pH value to 4-5.
Preferably, it is specially under the power of 25-30KW, with 300-500 revs/min that 2-3 hours are handled in the step (3)
The speed of clock stirs, and ultrasonic mixing 2-3 hours.
Preferably, the potassium hydroxide solution that potassium hydroxide solution is mass fraction 5-8% in the step (4).
Preferably, in the step (5) product made from the sodium hypochlorite of mass fraction 1.5% and step (4) dosage
Mass ratio is 10:1, liquor natrii hypochloritis's Adding Way of mass fraction 1.5% is：By the sodium hypochlorite of mass fraction 1.5%
Solution is divided into 2 parts, and the liquor natrii hypochloritis of a mass fraction 1.5% was added at interval of one hour, and at the same time being added suitable
The glacial acetic acid of amount is adjusted to pH value to 4-5.
Preferably, the drying in the step (7) is specially and is dried in vacuo 48 hours under 80-90 degrees Celsius.
Preferably, soaking time is 2-5 minutes in step (8) the merging alcohol.
Preferably, the uv curing machine irradiation intensity in the step (8) is 7-9 watts/square centimeter, irradiation time 3-
7 minutes.
Preferably, the uv curing machine irradiation intensity in the step (8) is 7.8 watts/square centimeter, irradiation time 5
Minute.
The present invention has following beneficial effect：
(1) present invention is using coffee shell as raw material, after being impregnated using acidic oxidation and alkali, after activating coffee shell surface, and grinding
Coffee shell nano-cellulose is made, coffee case fibre element film is made after dilution filters and is impregnated in acrylic resin, is made multiple
Film is closed, there is good translucidus and toughness, can be applied to the wide range of areas such as Electronic Paper.
(2) the lignin difficulty in coffee shell removes, and after handling in the present invention using liquor natrii hypochloritis, successively uses dioxygen again
After water process, potassium hydroxide treatment, after being reprocessed again with liquor natrii hypochloritis, the content purity of obtained coffee case fibre
Height facilitates the surface homogeneity of composite membrane.
(3) for the present invention using acrylic resin soln dipping coffee case fibre element end, acrylic resin caking property is good, transparent
Degree is high, and the composite membrane after being impregnated using acrylic resin, stable structure, surface acrylic resin layer is not easily to fall off, has protection
The effect of coffee case fibre element film, while improving the light transmission rate of composite membrane.
Specific embodiment
Below with reference to embodiment, further description of the specific embodiments of the present invention, and following embodiment is only used for more
Technical solution of the present invention is clearly demonstrated, and not intended to limit the protection scope of the present invention.
Embodiment 1
A method of composite membrane being prepared using coffee shell, is included the following steps：
(1) coffee shell is put into pulverizer summarizes and crush, cross 80 meshes to get coffee shell powder；
(2) coffee shell powder is added in the liquor natrii hypochloritis of mass fraction 1.5%, is uniformly mixed, appropriate ice is added
Acetic acid is adjusted to pH value to 4-5, is placed in temperature control in water-bath and, with 400 revs/min of speed, is stirred reaction 4 to 72 degrees Celsius
Hour, filtering, it is neutral that filtrate, which is cleaned repeatedly with deionized water to filtrate,；
(3) product made from step (2) is put into 2% hydrogen peroxide of mass fraction, is uniformly mixed, merging 80 is Celsius
It in the water bath with thermostatic control of degree, handles 2 hours, filtering cleans filtrate 3 times repeatedly with deionized water；
(4) product made from step (3) is added in potassium hydroxide solution, after impregnating 12 hours, is put into 95 DEG C waters
Heating stirring 2 hours in bath, filtering, it is neutral that filtrate, which is cleaned repeatedly with deionized water to filtrate,；
(5) liquor natrii hypochloritis of mass fraction 1.5% is added in product made from step (4) and is uniformly mixed, is added
Glacial acetic acid is stirred reaction, until product surface, at white, filtering is cleaned repeatedly to filtrate extremely with filtrate to solution pH value to 4
Neutrality is to get coffee case fibre element；
(6) step (5) coffee case fibre element is added in superfine powder grinder, with 500 revs/min of speed, grinding 15
Hour, obtain coffee shell nano-cellulose；
(7) coffee shell nano-cellulose made from step (6) is weighed, being diluted with water to concentration is 0.2%, stirs 30 points
Clock keeps its evenly dispersed, and vacuum filtration removes moisture removal, obtains wet film；Wet film is taken out, is placed between two panels metal mesh, by metal
Net is placed between two pieces of glass plates after pressing, is placed in drying in baking oven and is taken out to get coffee shell nano fibrous membrane；
(8) coffee shell nano fibrous membrane is put into alcohol and is impregnated, to remove surface impurity, take out nanometer coir fibre film
It after air-drying, is placed in acrylic resin soln, after thin-film transparent, taking-up, which is placed in two blocks of sheet glass, to be flattened, by ultra-violet curing
Machine solidifies to get composite membrane.
The liquor natrii hypochloritis of mass fraction 1.5% in step (2) and the dosage mass ratio of coffee shell powder are 20:1.
In step (2) mass fraction 1.5% liquor natrii hypochloritis be added coffee shell in method be：By mass fraction
1.5% sodium hypochlorite is divided into 4 parts, and the liquor natrii hypochloritis of a mass fraction 1.5% was added at interval of one hour, and
Suitable glacial acetic acid, which is added, is adjusted to pH value to 4-5 simultaneously.
Processing 2 hours in step (3) are specially to be stirred under the power of 25KW with 300 revs/min of speed, and ultrasound is mixed
It closes 2 hours.
Potassium hydroxide solution is the potassium hydroxide solution of mass fraction 5% in step (4).
The dosage mass ratio of product made from the sodium hypochlorite of mass fraction 1.5% and step (4) is 10 in step (5):
1, liquor natrii hypochloritis's Adding Way of mass fraction 1.5% is：The liquor natrii hypochloritis of mass fraction 1.5% is divided into 2
Part, the liquor natrii hypochloritis of a mass fraction 1.5% was added at interval of one hour, and at the same time suitable glacial acetic acid tune is added
Section is to pH value to 4-5.
Drying in step (7) is specially at 80 degrees celsius, to be dried in vacuo 48 hours.
It is 2 minutes that step (8), which is placed in soaking time in alcohol,.
Uv curing machine irradiation intensity in step (8) is 7 watts/square centimeter, and irradiation time is 3 minutes.
Embodiment 2
(1) coffee shell is put into pulverizer summarizes and crush, sieve with 100 mesh sieve to get coffee shell powder；
(2) coffee shell powder is added in the liquor natrii hypochloritis of mass fraction 1.5%, is uniformly mixed, appropriate ice is added
Acetic acid is adjusted to pH value to 5, is placed in temperature control in water-bath and, with 600 revs/min of speed, it is small to be stirred reaction 5 to 78 degrees Celsius
When, filtering, it is neutral that filtrate, which is cleaned repeatedly with deionized water to filtrate,；
(3) product made from step (2) is put into 2% hydrogen peroxide of mass fraction, is uniformly mixed, merging 80 is Celsius
It in the water bath with thermostatic control of degree, handles 3 hours, filtering cleans filtrate 5 times repeatedly with deionized water；
(4) product made from step (3) is added in potassium hydroxide solution, after impregnating 12 hours, is put into 95 DEG C waters
Heating stirring 2 hours in bath, filtering, it is neutral that filtrate, which is cleaned repeatedly with deionized water to filtrate,；
(5) liquor natrii hypochloritis of mass fraction 1.5% is added in product made from step (4) and is uniformly mixed, is added
Glacial acetic acid is stirred reaction, until product surface, at white, filtering is cleaned repeatedly to filtrate extremely with filtrate to solution pH value to 5
Neutrality is to get coffee case fibre element；
(6) step (5) coffee case fibre element is added in superfine powder grinder, with 600 revs/min of speed, grinding 20
Hour, obtain coffee shell nano-cellulose；
(7) coffee shell nano-cellulose made from step (6) is weighed, being diluted with water to concentration is 0.2%, stirs 30 points
Clock keeps its evenly dispersed, and vacuum filtration removes moisture removal, obtains wet film；Wet film is taken out, is placed between two panels metal mesh, by metal
Net is placed between two pieces of glass plates after pressing, is placed in drying in baking oven and is taken out to get coffee shell nano fibrous membrane；
(8) coffee shell nano fibrous membrane is put into alcohol and is impregnated, to remove surface impurity, take out nanometer coir fibre film
It after air-drying, is placed in acrylic resin soln, after thin-film transparent, taking-up, which is placed in two blocks of sheet glass, to be flattened, by ultra-violet curing
Machine solidifies to get composite membrane.
The liquor natrii hypochloritis of mass fraction 1.5% in step (2) and the dosage mass ratio of coffee shell powder are 20:1.
In step (2) mass fraction 1.5% liquor natrii hypochloritis be added coffee shell in method be：By mass fraction
1.5% sodium hypochlorite is divided into 4 parts, and the liquor natrii hypochloritis of a mass fraction 1.5% was added at interval of one hour, and
Suitable glacial acetic acid, which is added, is adjusted to pH value to 4-5 simultaneously.
Processing 3 hours in step (3) are specially to be stirred under the power of 30KW with 500 revs/min of speed, and ultrasound is mixed
It closes 3 hours.
Potassium hydroxide solution is the potassium hydroxide solution of mass fraction 8% in step (4).
The dosage mass ratio of product made from the sodium hypochlorite of mass fraction 1.5% and step (4) is 10 in step (5):
1, liquor natrii hypochloritis's Adding Way of mass fraction 1.5% is：The liquor natrii hypochloritis of mass fraction 1.5% is divided into 2
Part, the liquor natrii hypochloritis of a mass fraction 1.5% was added at interval of one hour, and at the same time suitable glacial acetic acid tune is added
Section is to pH value to 4-5.
Drying in step (7) is specially to be dried in vacuo 48 hours under 90 degrees Celsius.
It is 5 minutes that step (8), which is placed in soaking time in alcohol,.
Uv curing machine irradiation intensity in step (8) is 9 watts/square centimeter, and irradiation time is 7 minutes.
Embodiment 3
(1) coffee shell is put into pulverizer summarizes and crush, cross 90 meshes to get coffee shell powder；
(2) coffee shell powder is added in the liquor natrii hypochloritis of mass fraction 1.5%, is uniformly mixed, appropriate ice is added
Acetic acid is adjusted to pH value to 4.2, is placed in temperature control in water-bath and, with 480 revs/min of speed, is stirred reaction to 74 degrees Celsius
4.6 hours, filtering, it was neutral that filtrate, which is cleaned repeatedly with deionized water to filtrate,；
(3) product made from step (2) is put into 2% hydrogen peroxide of mass fraction, is uniformly mixed, merging 80 is Celsius
It in the water bath with thermostatic control of degree, handles 2.4 hours, filtering cleans filtrate 4 times repeatedly with deionized water；
(4) product made from step (3) is added in potassium hydroxide solution, after impregnating 12 hours, is put into 95 DEG C waters
Heating stirring 2 hours in bath, filtering, it is neutral that filtrate, which is cleaned repeatedly with deionized water to filtrate,；
(5) liquor natrii hypochloritis of mass fraction 1.5% is added in product made from step (4) and is uniformly mixed, is added
Glacial acetic acid is stirred reaction, until product surface, at white, filtering is cleaned repeatedly with filtrate to filtrate to solution pH value to 4-5
To neutrality to get coffee case fibre element；
(6) step (5) coffee case fibre element is added in superfine powder grinder, with 580 revs/min of speed, grinding 18
Hour, obtain coffee shell nano-cellulose；
(7) coffee shell nano-cellulose made from step (6) is weighed, being diluted with water to concentration is 0.2%, stirs 30 points
Clock keeps its evenly dispersed, and vacuum filtration removes moisture removal, obtains wet film；Wet film is taken out, is placed between two panels metal mesh, by metal
Net is placed between two pieces of glass plates after pressing, is placed in drying in baking oven and is taken out to get coffee shell nano fibrous membrane；
(8) coffee shell nano fibrous membrane is put into alcohol and is impregnated, to remove surface impurity, take out nanometer coir fibre film
It after air-drying, is placed in acrylic resin soln, after thin-film transparent, taking-up, which is placed in two blocks of sheet glass, to be flattened, by ultra-violet curing
Machine solidifies to get composite membrane.
The liquor natrii hypochloritis of mass fraction 1.5% in step (2) and the dosage mass ratio of coffee shell powder are 20:1.
In step (2) mass fraction 1.5% liquor natrii hypochloritis be added coffee shell in method be：By mass fraction
1.5% sodium hypochlorite is divided into 4 parts, and the liquor natrii hypochloritis of a mass fraction 1.5% was added at interval of one hour, and
Suitable glacial acetic acid, which is added, is adjusted to pH value to 4-5 simultaneously.
Processing 2.4 hours in step (3) are specially to be stirred under the power of 28KW with 450 revs/min of speed, ultrasound
Mixing 2.6 hours.
Potassium hydroxide solution is the potassium hydroxide solution of mass fraction 7% in step (4).
The dosage mass ratio of product made from the sodium hypochlorite of mass fraction 1.5% and step (4) is 10 in step (5):
1, liquor natrii hypochloritis's Adding Way of mass fraction 1.5% is：The liquor natrii hypochloritis of mass fraction 1.5% is divided into 2
Part, the liquor natrii hypochloritis of a mass fraction 1.5% was added at interval of one hour, and at the same time suitable glacial acetic acid tune is added
Section is to pH value to 4-5.
Drying in step (7) is specially to be dried in vacuo 48 hours under 87 degrees Celsius.
It is 4 minutes that step (8), which is placed in soaking time in alcohol,.
Uv curing machine irradiation intensity in step (8) is 8.5 watts/square centimeter, and irradiation time is 4 minutes.
Embodiment 4
(1) coffee shell is put into pulverizer summarizes and crush, cross 95 meshes to get coffee shell powder；
(2) coffee shell powder is added in the liquor natrii hypochloritis of mass fraction 1.5%, is uniformly mixed, appropriate ice is added
Acetic acid is adjusted to pH value to 4-5, is placed in water-bath that temperature control is to 72-78 degrees Celsius, with 550 revs/min of speed, is stirred anti-
It answers 4.4 hours, filters, it is neutral that filtrate, which is cleaned repeatedly with deionized water to filtrate,；
(3) product made from step (2) is put into 2% hydrogen peroxide of mass fraction, is uniformly mixed, merging 80 is Celsius
It in the water bath with thermostatic control of degree, handles 2.7 hours, filtering cleans filtrate 4 times repeatedly with deionized water；
(4) product made from step (3) is added in potassium hydroxide solution, after impregnating 12 hours, is put into 95 DEG C waters
Heating stirring 2 hours in bath, filtering, it is neutral that filtrate, which is cleaned repeatedly with deionized water to filtrate,；
(5) liquor natrii hypochloritis of mass fraction 1.5% is added in product made from step (4) and is uniformly mixed, is added
Glacial acetic acid is stirred reaction, until product surface, at white, filtering is cleaned repeatedly with filtrate to filtrate to solution pH value to 4-5
To neutrality to get coffee case fibre element；
(6) step (5) coffee case fibre element is added in superfine powder grinder, with 540 revs/min of speed, grinding 19
Hour, obtain coffee shell nano-cellulose；
(7) coffee shell nano-cellulose made from step (6) is weighed, being diluted with water to concentration is 0.2%, stirs 30 points
Clock keeps its evenly dispersed, and vacuum filtration removes moisture removal, obtains wet film；Wet film is taken out, is placed between two panels metal mesh, by metal
Net is placed between two pieces of glass plates after pressing, is placed in drying in baking oven and is taken out to get coffee shell nano fibrous membrane；
(8) coffee shell nano fibrous membrane is put into alcohol and is impregnated, to remove surface impurity, take out nanometer coir fibre film
It after air-drying, is placed in acrylic resin soln, after thin-film transparent, taking-up, which is placed in two blocks of sheet glass, to be flattened, by ultra-violet curing
Machine solidifies to get composite membrane.
The liquor natrii hypochloritis of mass fraction 1.5% in step (2) and the dosage mass ratio of coffee shell powder are 20:1.
In step (2) mass fraction 1.5% liquor natrii hypochloritis be added coffee shell in method be：By mass fraction
1.5% sodium hypochlorite is divided into 4 parts, and the liquor natrii hypochloritis of a mass fraction 1.5% was added at interval of one hour, and
Suitable glacial acetic acid, which is added, is adjusted to pH value to 4-5 simultaneously.
Processing 2.7 hours in step (3) are specially to be stirred under the power of 28KW with 420 revs/min of speed, ultrasound
Mixing 2.7 hours.
Potassium hydroxide solution is the potassium hydroxide solution of mass fraction 7% in step (4).
The dosage mass ratio of product made from the sodium hypochlorite of mass fraction 1.5% and step (4) is 10 in step (5):
1, liquor natrii hypochloritis's Adding Way of mass fraction 1.5% is：The liquor natrii hypochloritis of mass fraction 1.5% is divided into 2
Part, the liquor natrii hypochloritis of a mass fraction 1.5% was added at interval of one hour, and at the same time suitable glacial acetic acid tune is added
Section is to pH value to 4-5.
Drying in step (7) is specially to be dried in vacuo 48 hours under 86 degrees Celsius.
It is 4 minutes that step (8), which is placed in soaking time in alcohol,.
Uv curing machine irradiation intensity in step (8) is 7.8 watts/square centimeter, and irradiation time is 5 minutes.
Comparative example 1：Coffee shell nano-cellulose film, which is prepared, using the method and raw material proportioning of embodiment 1 (does not impregnate propylene
Acid resin)
Coffee shell nano-cellulose film is made with comparative example 1 in composite membrane made from embodiment 1-4 to be tested for the property, is tied
Fruit such as the following table 1；
Table 1：
In conclusion the present invention has the following advantages that：
(1) present invention is using coffee shell as raw material, after being impregnated using acidic oxidation and alkali, after activating coffee shell surface, and grinding
Coffee shell nano-cellulose is made, coffee case fibre element film is made after dilution filters and is impregnated in acrylic resin, is made multiple
Film is closed, there is good translucidus and toughness, can be applied to the wide range of areas such as Electronic Paper.
(2) the lignin difficulty in coffee shell removes, and after handling in the present invention using liquor natrii hypochloritis, successively uses dioxygen again
After water process, potassium hydroxide treatment, after being reprocessed again with liquor natrii hypochloritis, the content purity of obtained coffee case fibre
Height facilitates the surface homogeneity of composite membrane.
(3) for the present invention using acrylic resin soln dipping coffee case fibre element end, acrylic resin caking property is good, transparent
Degree is high, and the composite membrane after being impregnated using acrylic resin, stable structure, surface acrylic resin layer is not easily to fall off, has protection
The effect of coffee case fibre element film, while improving the light transmission rate of composite membrane.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, although referring to aforementioned reality
Applying example, invention is explained in detail, for those skilled in the art, still can be to aforementioned each implementation
Technical solution documented by example is modified or equivalent replacement of some of the technical features.It is all in essence of the invention
Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of method for preparing composite membrane using coffee shell, which is characterized in that include the following steps：
(1) coffee shell is put into pulverizer summarizes and crush, cross 80-100 mesh to get coffee shell powder；
(2) coffee shell powder is added in the liquor natrii hypochloritis of mass fraction 1.5%, is uniformly mixed, appropriate glacial acetic acid is added
PH value is adjusted to 4-5, is placed in water-bath that temperature control is to 72-78 degrees Celsius, with 400-600 revs/min of speed, is stirred anti-
It answers 4-5 hours, filters, it is neutral that filtrate, which is cleaned repeatedly with deionized water to filtrate,；
(3) product made from step (2) is put into 2% hydrogen peroxide of mass fraction, is uniformly mixed, 80 degrees Celsius of merging
It in water bath with thermostatic control, handles 2-3 hours, filtering cleans filtrate 3-5 times with deionized water repeatedly；
(4) product made from step (3) is added in potassium hydroxide solution, after impregnating 12 hours, is put into 95 DEG C water baths
Middle heating stirring 2 hours, filtering, it is neutral that filtrate, which is cleaned repeatedly with deionized water to filtrate,；
(5) liquor natrii hypochloritis of mass fraction 1.5% is added in product made from step (4) and is uniformly mixed, ice vinegar is added
Acid is stirred reaction, until product surface, at white, filtering is cleaned to filtrate with filtrate repeatedly into solution pH value to 4-5
Property to get coffee case fibre element；
(6) step (5) coffee case fibre element is added in superfine powder grinder, with 500-600 revs/min of speed, grinds 15-
20 hours, obtain coffee shell nano-cellulose；
(7) coffee shell nano-cellulose made from step (6) is weighed, being diluted with water to concentration is 0.2%, stirs 30 minutes, makes
Its is evenly dispersed, and vacuum filtration removes moisture removal, obtains wet film；Wet film is taken out, is placed between two panels metal mesh, metal mesh is set
After being flattened between two pieces of glass plates, it is placed in drying in baking oven and is taken out to get coffee shell nano fibrous membrane；
(8) coffee shell nano fibrous membrane is put into alcohol and is impregnated, to remove surface impurity, taken out nanometer coir fibre film and air-dry
Afterwards, it is placed in acrylic resin soln, after thin-film transparent, taking-up, which is placed in two blocks of sheet glass, to be flattened, and uv curing machine is consolidated
Change to get composite membrane.
2. the method according to claim 1 for preparing composite membrane using coffee shell, which is characterized in that in the step (2)
Mass fraction 1.5% liquor natrii hypochloritis and coffee shell powder dosage mass ratio be 20:1.
3. the method according to claim 2 for preparing composite membrane using coffee shell, which is characterized in that in the step (2)
The method that the liquor natrii hypochloritis of mass fraction 1.5% is added in coffee shell is：The sodium hypochlorite of mass fraction 1.5% is divided equally
It is 4 parts, the liquor natrii hypochloritis of a mass fraction 1.5% was added at interval of one hour, and at the same time suitable ice vinegar is added
Acid is adjusted to pH value to 4-5.
4. the method according to claim 1 for preparing composite membrane using coffee shell, which is characterized in that in the step (3)
Processing 2-3 hours are specially to be stirred under the power of 25-30KW with 300-500 revs/min of speed, and ultrasonic mixing 2-3 is small
When.
5. the method according to claim 1 for preparing composite membrane using coffee shell, which is characterized in that in the step (4)
Potassium hydroxide solution is the potassium hydroxide solution of mass fraction 5-8%.
6. the method according to claim 1 for preparing composite membrane using coffee shell, which is characterized in that in the step (5)
The dosage mass ratio of product made from the sodium hypochlorite and step (4) of mass fraction 1.5% is 10:1, mass fraction 1.5%
Liquor natrii hypochloritis's Adding Way is：The liquor natrii hypochloritis of mass fraction 1.5% is divided into 2 parts, was added at interval of one hour
Enter the liquor natrii hypochloritis of a mass fraction 1.5%, and at the same time suitable glacial acetic acid, which is added, is adjusted to pH value to 4-5.
7. the method according to claim 1 for preparing composite membrane using coffee shell, which is characterized in that in the step (7)
Drying be specially under 80-90 degrees Celsius, be dried in vacuo 48 hours.
8. the method according to claim 1 for preparing composite membrane using coffee shell, which is characterized in that the step (8) is set
Entering soaking time in alcohol is 2-5 minutes.
9. the method according to claim 1 for preparing composite membrane using coffee shell, which is characterized in that in the step (8)
Uv curing machine irradiation intensity be 7-9 watts/square centimeter, irradiation time be 3-7 minutes.
10. the method according to claim 9 for preparing composite membrane using coffee shell, which is characterized in that in the step (8)
Uv curing machine irradiation intensity be 7.8 watts/square centimeter, irradiation time be 5 minutes.
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