CN109537344A - The method for preparing transparency cellulose film with hydrogen peroxide bleaching fiber-rich cellulosic material - Google Patents
The method for preparing transparency cellulose film with hydrogen peroxide bleaching fiber-rich cellulosic material Download PDFInfo
- Publication number
- CN109537344A CN109537344A CN201811566846.6A CN201811566846A CN109537344A CN 109537344 A CN109537344 A CN 109537344A CN 201811566846 A CN201811566846 A CN 201811566846A CN 109537344 A CN109537344 A CN 109537344A
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- CN
- China
- Prior art keywords
- hydrogen peroxide
- cellulose film
- cellulosic material
- peroxide bleaching
- fiber
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08H—DERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS
- C08H6/00—Macromolecular compounds derived from lignin, e.g. tannins, humic acids
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
- D21C3/00—Pulping cellulose-containing materials
- D21C3/20—Pulping cellulose-containing materials with organic solvents or in solvent environment
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
- D21C9/00—After-treatment of cellulose pulp, e.g. of wood pulp, or cotton linters ; Treatment of dilute or dewatered pulp or process improvement taking place after obtaining the raw cellulosic material and not provided for elsewhere
- D21C9/001—Modification of pulp properties
- D21C9/007—Modification of pulp properties by mechanical or physical means
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
- D21C9/00—After-treatment of cellulose pulp, e.g. of wood pulp, or cotton linters ; Treatment of dilute or dewatered pulp or process improvement taking place after obtaining the raw cellulosic material and not provided for elsewhere
- D21C9/10—Bleaching ; Apparatus therefor
- D21C9/16—Bleaching ; Apparatus therefor with per compounds
- D21C9/163—Bleaching ; Apparatus therefor with per compounds with peroxides
Abstract
The present invention relates to synthetic fiber technologies, more particularly to a kind of method for preparing transparency cellulose film with hydrogen peroxide bleaching fiber-rich cellulosic material.The method for preparing transparency cellulose film with hydrogen peroxide bleaching fiber-rich cellulosic material, include the following steps: that (1) is crushed bagasse and poplar using micromill, and the mesh screen through 100 mesh screens out the raw material less than 100 mesh, is placed in oven and dried spare to over dry；(2) biomass Benzene-ethanol extraction and component separation process；(3) hydrogen peroxide bleaching fiber-rich element；(4) ultrasonic treatment prepares transparency cellulose film.Operation of the present invention method is simple, and applicability is wide, and manufactured transparency cellulose film has preferable light transmission through the invention.
Description
Technical field
The present invention relates to synthetic fiber technologies, more particularly to one kind with hydrogen peroxide bleaching fiber-rich cellulosic material system
The method of standby transparency cellulose film.
Background technique
With social progress and development, resource, energy consumption are more serious, and being faced with the earth, resource is exhausted and environment
Pollute two large problems.Biomass because have the advantages that rich reserves and it is reproducible due to be widely noticed, in recent years with biomass be original
The concept of the biorefining of material is come into being.Based on this concept, each component of biomass is separated first, later by
One is used, and prepares high-performance, the material of high added value, the energy, chemicals.In numerous biomass advanced materials, receive
Rice cellulose is concerned because haveing excellent performance.
Nano-cellulose refers to that the size at least one dimension space reaches the cellulose of Nano grade, and partial size is generally 30
100nm is in granular form or rodlike.Not only has the basic structure and function of cellulose from the nano-cellulose of biomass
Can, also there is the characteristics of nanoparticles for being different from cellulose, available transparent nano after nano-cellulose is formed a film and dried
Cellophane, resulting transparency cellulose film has many advantages, such as high-intensitive, high transparency and high gas-obstructing character, in flexibility
The fields such as device, optical material, energy storage have broad application prospects.
But the preparation of existing nano-cellulose is mostly after slurrying, bleaching process obtain paper pulp, through mechanical treatment or acid
Hydrolysis process obtains nano-cellulose, and existing technique mostly uses sulphite and chloro-containing reagent to carry out slurrying and bleaching, right
Environment is affected.
Summary of the invention
The present invention is directed in view of the above-mentioned problems, proposing that one kind prepares vitreous fibre with hydrogen peroxide bleaching fiber-rich cellulosic material
The method of plain film.
Technical program of the present invention lies in:
In the method that hydrogen peroxide bleaching fiber-rich cellulosic material prepares transparency cellulose film, include the following steps:
(1) bagasse and poplar are crushed using micromill, and the mesh screen through 100 mesh screens out the raw material less than 100 mesh,
It is placed in oven and dried spare to over dry；
(2) biomass Benzene-ethanol extraction and component separation process；
Soxhlet type 6h is carried out to above-mentioned biomass material with benzene alcoholic solution, wherein the volume ratio of benzene and dehydrated alcohol is 2:
1；Extracting uses washes of absolute alcohol after completing, until the benzene in raw material is eliminated, then wash with distilled water, to remove ethyl alcohol,
After to be put into oven drying spare；
Biomass material after extracting is in the mixed system that 1,2-PD and water and ionic-liquid catalyst form, temperature
30min is handled under the conditions of 200 DEG C, wherein biomass material is 4:1 in the volume ratio of 1,2-PD；After the completion of processing, very
Empty pump filters isolated CRM, wash with distilled water twice of rear drying for standby；It collects filtrate and excessive water sedimentation is added and isolates
Lignin；
(3) hydrogen peroxide bleaching fiber-rich element；
The hydrogen peroxide of 50g is weighed in conical flask, 0.1g epsom salt stabilizer is added, it is molten using 15% sodium hydroxide
It is 9 10 that liquid, which adjusts pH value,；0.5g fiber-rich cellulosic material is weighed, is poured into the conical flask for mixing up pH, puts and is heated into oil bath pan
Processing, and magnetic agitation is carried out simultaneously；Conical flask is taken out from oil bath pan after the reaction was completed, is cooled to room temperature, is used
Solution ph in bottle is adjusted to 67 by 0.5mol/L sulfuric acid, is then filtered, is placed in oven and dried after filter residue is cleaned standby
With；(4) ultrasonic treatment prepares transparency cellulose film；
It takes 0.5g bleaching CRM to be scattered in 100mL distilled water, is put into ultrasonic cell disruptor ultrasound 20 minutes；Ultrasound terminates
It takes out and stands afterwards, until isolating supernatant liquor, and filtered using organic filter membrane of 0.22 mm of aperture, on filter membrane
To transparency cellulose film.
The volume ratio of the biomass material and 1,2- propylene glycol is 4:1.
The filter membrane of the vacuum filtration, which is that nylon is organic, uses filter membrane, and aperture is 0.45 micron.
The concentration of the hydrogen peroxide is 15% or 30%.
The adjusting pH value be 9 10 when using 15% sodium hydroxide solution, adjust pH value be 67 when use
0.5mol/L sulfuric acid.
The power of the ultrasound is 1800w.
The technical effects of the invention are that:
Operation of the present invention method is simple, and applicability is wide, and manufactured transparency cellulose film has preferable light transmission through the invention.
Specific embodiment
Embodiment 1
In the method that hydrogen peroxide bleaching fiber-rich cellulosic material prepares transparency cellulose film, include the following steps:
(1) bagasse and poplar are crushed using micromill, and the mesh screen through 100 mesh screens out the raw material less than 100 mesh,
It is placed in oven and dried spare to over dry；
(2) biomass Benzene-ethanol extraction and component separation process；
Soxhlet type 6h is carried out to above-mentioned biomass material with benzene alcoholic solution, wherein the volume ratio of benzene and dehydrated alcohol is 2:
1；Extracting uses washes of absolute alcohol after completing, until the benzene in raw material is eliminated, then wash with distilled water, to remove ethyl alcohol,
After to be put into oven drying spare；
Biomass material after extracting is in the mixed system that 1,2-PD and water and ionic-liquid catalyst form, temperature
30min is handled under the conditions of 200 DEG C, wherein biomass material is 4:1 in the volume ratio of 1,2-PD；After the completion of processing, very
Empty pump filters isolated CRM, and filter membrane, which is that nylon is organic, uses filter membrane, and aperture is 0.45 micron；It does after twice wash with distilled water
It is dry spare；It collects filtrate and excessive water sedimentation is added and isolates lignin；
(3) hydrogen peroxide bleaching fiber-rich element；
The hydrogen peroxide of 50g is weighed in conical flask, wherein the concentration of hydrogen peroxide is 15%；It is steady that 0.1g epsom salt is added
Determine agent, the use of 15% sodium hydroxide solution adjustment pH value is 9 10；0.5g fiber-rich cellulosic material is weighed, the cone for mixing up pH is poured into
It in shape bottle, puts and heats into oil bath pan, and carry out magnetic agitation simultaneously；Conical flask is taken from oil bath pan after the reaction was completed
Out, it is cooled to room temperature, solution ph in bottle is adjusted to 67 using 0.5mol/L sulfuric acid, then filter, after filter residue is cleaned
It is placed in oven and dried spare, transparency cellulose film is made；
(4) ultrasonic treatment prepares transparency cellulose film；
It takes 0.5g bleaching CRM to be scattered in 100mL distilled water, is put into ultrasonic cell disruptor ultrasound 20 minutes, ultrasonic function
Rate is 1800w；Take out and stand after ultrasound, until isolate supernatant liquor, and using organic filter membrane of 0.22 mm of aperture into
Row filters, and transparency cellulose film is obtained on filter membrane.
Embodiment 2
In the method that hydrogen peroxide bleaching fiber-rich cellulosic material prepares transparency cellulose film, include the following steps:
(1) bagasse and poplar are crushed using micromill, and the mesh screen through 100 mesh screens out the raw material less than 100 mesh,
It is placed in oven and dried spare to over dry；
(2) biomass Benzene-ethanol extraction and component separation process；
Soxhlet type 6h is carried out to above-mentioned biomass material with benzene alcoholic solution, wherein the volume ratio of benzene and dehydrated alcohol is 2:
1；Extracting uses washes of absolute alcohol after completing, until the benzene in raw material is eliminated, then wash with distilled water, to remove ethyl alcohol,
After to be put into oven drying spare；
Biomass material after extracting is in the mixed system that 1,2-PD and water and ionic-liquid catalyst form, temperature
30min is handled under the conditions of 200 DEG C, wherein biomass material is 4:1 in the volume ratio of 1,2-PD；After the completion of processing, very
Empty pump filters isolated CRM, and filter membrane, which is that nylon is organic, uses filter membrane, and aperture is 0.45 micron；It does after twice wash with distilled water
It is dry spare；It collects filtrate and excessive water sedimentation is added and isolates lignin；
(3) hydrogen peroxide bleaching fiber-rich element；
The hydrogen peroxide of 50g is weighed in conical flask, wherein the concentration of hydrogen peroxide is 30%；It is steady that 0.1g epsom salt is added
Determine agent, the use of 15% sodium hydroxide solution adjustment pH value is 9 10；0.5g fiber-rich cellulosic material is weighed, the cone for mixing up pH is poured into
It in shape bottle, puts and heats into oil bath pan, and carry out magnetic agitation simultaneously；Conical flask is taken from oil bath pan after the reaction was completed
Out, it is cooled to room temperature, solution ph in bottle is adjusted to 67 using 0.5mol/L sulfuric acid, then filter, after filter residue is cleaned
It is placed in oven and dried spare, transparency cellulose film is made；
(4) ultrasonic treatment prepares transparency cellulose film；
It takes 0.5g bleaching CRM to be scattered in 100mL distilled water, is put into ultrasonic cell disruptor ultrasound 20 minutes, ultrasonic function
Rate is 1800w；Take out and stand after ultrasound, until isolate supernatant liquor, and using organic filter membrane of 0.22 mm of aperture into
Row filters, and transparency cellulose film is obtained on filter membrane.
Claims (6)
1. the method for preparing transparency cellulose film with hydrogen peroxide bleaching fiber-rich cellulosic material, it is characterised in that: including walking as follows
It is rapid:
(1) bagasse and poplar are crushed using micromill, and the mesh screen through 100 mesh screens out the raw material less than 100 mesh,
It is placed in oven and dried spare to over dry；
(2) biomass Benzene-ethanol extraction and component separation process；
Soxhlet type 6h is carried out to above-mentioned biomass material with benzene alcoholic solution, extracting uses washes of absolute alcohol after completing, until
Eliminate the benzene in raw material, then wash with distilled water, to remove ethyl alcohol, after to be put into oven drying spare；
Biomass material after extracting is in the mixed system that 1,2-PD and water and ionic-liquid catalyst form, temperature
30min is handled under the conditions of 200 DEG C；After the completion of processing, isolated CRM is filtered by vacuum, drying is standby after twice wash with distilled water
With；It collects filtrate and excessive water sedimentation is added and isolates lignin；
(3) hydrogen peroxide bleaching fiber-rich element；
The hydrogen peroxide of 50g is weighed in conical flask, 0.1g epsom salt stabilizer is added, adjustment pH value is 9 10；It weighs
0.5g fiber-rich cellulosic material, is poured into the conical flask for mixing up pH, is put and is heated into oil bath pan, and is carried out magnetic force simultaneously and stirred
It mixes；Conical flask is taken out from oil bath pan after the reaction was completed, is cooled to room temperature, solution ph in bottle is adjusted to 67, is then taken out
Filter, is placed in oven and dried spare after filter residue is cleaned；
(4) ultrasonic treatment prepares transparency cellulose film；
It takes 0.5g bleaching CRM to be scattered in 100mL distilled water, is put into ultrasonic cell disruptor ultrasound 20 minutes；Ultrasound terminates
It takes out and stands afterwards, until isolating supernatant liquor, and filtered using organic filter membrane of 0.22 mm of aperture, on filter membrane
To transparency cellulose film.
2. the method according to claim 1 that transparency cellulose film is prepared with hydrogen peroxide bleaching fiber-rich cellulosic material,
Be characterized in that: the volume ratio of the biomass material and 1,2- propylene glycol is 4:1.
3. the method according to claim 1 that transparency cellulose film is prepared with hydrogen peroxide bleaching fiber-rich cellulosic material,
Be characterized in that: the filter membrane of the vacuum filtration is the organic filter membrane of nylon, and aperture is 0.45 micron.
4. the method according to claim 1 that transparency cellulose film is prepared with hydrogen peroxide bleaching fiber-rich cellulosic material,
Be characterized in that: the concentration of the hydrogen peroxide is 15% or 30%.
5. the method according to claim 1 that transparency cellulose film is prepared with hydrogen peroxide bleaching fiber-rich cellulosic material,
Be characterized in that: the adjusting pH value be 9 10 when using 15% sodium hydroxide solution, adjust pH value be 67 when use
0.5mol/L sulfuric acid.
6. the method according to claim 1 that transparency cellulose film is prepared with hydrogen peroxide bleaching fiber-rich cellulosic material,
Be characterized in that: the power of the ultrasound is 1800w.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811566846.6A CN109537344A (en) | 2018-12-21 | 2018-12-21 | The method for preparing transparency cellulose film with hydrogen peroxide bleaching fiber-rich cellulosic material |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811566846.6A CN109537344A (en) | 2018-12-21 | 2018-12-21 | The method for preparing transparency cellulose film with hydrogen peroxide bleaching fiber-rich cellulosic material |
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| CN109537344A true CN109537344A (en) | 2019-03-29 |
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| CN201811566846.6A Pending CN109537344A (en) | 2018-12-21 | 2018-12-21 | The method for preparing transparency cellulose film with hydrogen peroxide bleaching fiber-rich cellulosic material |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110128555A (en) * | 2019-06-26 | 2019-08-16 | 广西大学 | The preparation method of Cellulose nanocrystal body |
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2018
- 2018-12-21 CN CN201811566846.6A patent/CN109537344A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110128555A (en) * | 2019-06-26 | 2019-08-16 | 广西大学 | The preparation method of Cellulose nanocrystal body |
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| PB01 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20190329 |
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| WD01 | Invention patent application deemed withdrawn after publication |