CN112940139A - Novel preparation method of microcrystalline cellulose - Google Patents
Novel preparation method of microcrystalline cellulose Download PDFInfo
- Publication number
- CN112940139A CN112940139A CN202110106622.2A CN202110106622A CN112940139A CN 112940139 A CN112940139 A CN 112940139A CN 202110106622 A CN202110106622 A CN 202110106622A CN 112940139 A CN112940139 A CN 112940139A
- Authority
- CN
- China
- Prior art keywords
- microcrystalline cellulose
- filtering
- minutes
- cellulose
- hot air
- 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.)
- Pending
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B15/00—Preparation of other cellulose derivatives or modified cellulose, e.g. complexes
- C08B15/02—Oxycellulose; Hydrocellulose; Cellulosehydrate, e.g. microcrystalline cellulose
Abstract
A preparation method of microcrystalline cellulose comprises the following steps: step 1, putting fiber waste into a container filled with sodium hydroxide, and treating in a water bath; step 2, performing water filtration on the product obtained in the step 1 for deep washing, and bleaching by using hydrogen peroxide; step 3, thoroughly washing the obtained cellulose with distilled water, filtering, and extruding the residual solution; drying in a hot air oven; the obtained N g of cellulose is put into a container and hydrolyzed by using a solution containing hydrogen chloride; step 4, pouring the obtained hot acid mixture into cold tap water, stirring by using a magnetic stirrer, and then standing; step 5, filtering and cleaning the obtained microcrystalline cellulose until the microcrystalline cellulose is neutral; then filtering, pressing and drying in a hot air oven to obtain the microcrystalline cellulose. Compared with the prior art, the microcrystalline cellulose prepared by the waste fibers has good thermal stability, high polymerization degree and reasonable crystallinity, and has good application value when being used for utilizing waste materials.
Description
Technical Field
The invention belongs to the field of chemical synthesis, and particularly relates to a method for recycling waste fibers and preparing the waste fibers into microcrystalline cellulose.
Background
Prior art document 1 (chemical institute of chinese academy of sciences, 2020-08-25, CN111575834A) discloses a method for preparing carbon nanofibers based on natural fibrilia raw materials, comprising the following steps: step 1, pretreating a natural fibrilia raw material by using a sodium hydroxide solution and anthraquinone-2-sodium sulfonate to obtain pretreated fibrilia; step 2, performing nanocrystallization treatment on the pretreated fibrilia by using a phosphoric acid solution to obtain nanocrystallized fibrilia; step 3, carrying out hydrothermal treatment on the nano fibrilia to obtain a hydrothermal treatment product; and 4, further carbonizing the hydrothermal treatment product to obtain the carbon nanofiber.
The production of natural fiber inevitably generates by-products or waste, that is, the prior art document 1 can produce only natural fiber, and the production process is complicated, and by-products or waste are generated. The prior art has the technical requirement of recycling, the waste fibers are recycled by using a proper method, the waste fibers have the advantages of waste utilization and resource recycling, and the recycling of the waste fibers is concerned more and more along with the climate change and the consumption of petroleum resources.
Disclosure of Invention
In order to solve the defects in the prior art, the invention aims to provide the preparation method of the microcrystalline cellulose, which is simple and feasible, is simple to operate, is used for recovering waste fibers and obtaining the microcrystalline cellulose with good thermal stability and high polymerization degree.
The invention adopts the following technical scheme. A preparation method of microcrystalline cellulose comprises the following steps:
step 1, putting fiber waste into a container filled with sodium hydroxide with set concentration, and treating in a water bath;
step 2, performing water filtration on the product obtained in the step 1 for deep washing, and bleaching by using hydrogen peroxide;
step 3, thoroughly washing the cellulose obtained in the step 2 with distilled water, filtering, and extruding the residual solution; drying in a hot air oven; the obtained N g of cellulose is put into a container and hydrolyzed by using a solution containing hydrogen chloride;
step 4, pouring the hot acid mixture obtained in the step 3 into cold tap water, stirring by using a magnetic stirrer, and then standing;
step 5, filtering and cleaning the microcrystalline cellulose obtained in the step 4 until the microcrystalline cellulose is neutral; then filtering, pressing and drying in a hot air oven to obtain the microcrystalline cellulose.
Preferably, in step 1, N grams of fiber waste is placed in a vessel containing 40N milliliters of 15% -25% strength sodium hydroxide and treated in a water bath at 60-100 ℃ for 40-80 minutes.
Further preferably, in step 1, N grams of the fiber waste is placed in a vessel containing 40N milliliters of 17% strength sodium hydroxide and treated in a water bath at 80 ℃ for 60 minutes.
Preferably, in step 2, the product of step 1 is subjected to water filtration for deep washing, and is bleached with 8% -12% hydrogen peroxide at 80 ℃ -120 ℃ for 20-40 minutes.
Further preferably, in step 2, the product of step 1 is subjected to water filtration for deep washing, and is bleached with 10% hydrogen peroxide at 95 ℃ for 30 minutes;
preferably, in step 3, the cellulose obtained in step 2 is thoroughly washed with distilled water, filtered, and the remaining solution is squeezed out manually or by a dehydrator; drying in a hot air oven at 50-100 deg.C for 30-120 min; the obtained N g of cellulose is put into a container, hydrolyzed by using 20N ml of solution containing 1 to 5 percent of hydrogen chloride and hydrolyzed for 20 to 30 minutes at the temperature of between 80 and 120 ℃.
Further preferably, in step 3, the cellulose obtained in step 2 is thoroughly washed with distilled water, filtered, and the remaining solution is extruded by a squeezer; drying in a hot air oven at 60 deg.C for 60 min; the resulting N g of cellulose was placed in a vessel, hydrolyzed using 20N ml of a solution containing 2.5% hydrogen chloride, and hydrolyzed at 105 ℃ for 15 minutes.
Preferably, in step 4, the hot acid mixture obtained in step 3 is poured into 200N ml of cold tap water, stirred at 400r/min or more by using a magnetic stirrer, and left for a set time.
Further preferably, in step 4, the hot acid mixture obtained in step 3 is poured into 200N ml of cold tap water, stirred at a speed of 600r/min or more by using a magnetic stirrer, and allowed to stand for 24 to 48 hours.
Preferably, in step 5, the microcrystalline cellulose obtained in step 4 is filtered and washed until the microcrystalline cellulose is neutral; then filtering, pressing and drying in a hot air oven at 80-120 ℃ for a set time to obtain the microcrystalline cellulose.
Further preferably, in step 5, the microcrystalline cellulose obtained in step 4 is filtered and washed until the microcrystalline cellulose is neutral; then, it was filtered again, pressed, and dried in a hot air oven at 105 ℃ for 30 minutes to obtain microcrystalline cellulose.
Compared with the prior art, the method has the beneficial effects that the waste fibers are used for preparing the microcrystalline cellulose, the prepared microcrystalline cellulose has good thermal stability, high polymerization degree and reasonable crystallinity, waste articles are utilized, and the method has good application value, is simple and easy to implement and is simple to operate.
Drawings
FIG. 1 is a flow chart of the preparation.
Detailed Description
The present application is further described below with reference to the accompanying drawings. The following examples are only for illustrating the technical solutions of the present invention more clearly, and the protection scope of the present application is not limited thereby.
Example 1:
embodiment 1 of the present invention discloses a method for preparing microcrystalline cellulose, comprising the steps of:
step 1, N g of fiber waste was placed in a vessel containing 40N ml of 15% strength sodium hydroxide and treated in a water bath at 60 ℃ for 40 minutes.
It is understood that N g is used to indicate the proportioning relationship between the fiber waste and various solutions in the process, and the amount of the fiber waste can be arbitrarily selected by those skilled in the art, so long as the proportion of the formula is kept consistent, and the invention falls into the technical scheme.
Step 2, performing water filtration on the product obtained in the step 1 for deep washing, and bleaching for 20 minutes at 80 ℃ by using 8% hydrogen peroxide;
step 3, thoroughly washing the cellulose obtained in the step 2 with distilled water, filtering, and manually extruding the residual solution; drying in a hot air oven at 50 deg.C for 30 min; the resulting N g of cellulose was placed in a vessel, hydrolyzed using 20N ml of a solution containing 1% hydrogen chloride, and hydrolyzed at 80 ℃ for 20 minutes.
And 4, pouring the hot acid mixture obtained in the step 3 into 200N ml of cold tap water, stirring the mixture by using a magnetic stirrer at a speed of over 400r/min, and standing the mixture for 36 hours.
Step 5, filtering and cleaning the microcrystalline cellulose obtained in the step 4 until the microcrystalline cellulose is neutral; then, the mixture was filtered again, pressed, and dried in a hot air oven at 80 ℃ for 45 minutes to obtain microcrystalline cellulose.
Example 2:
embodiment 2 of the present invention discloses a method for preparing microcrystalline cellulose, comprising the steps of:
step 1, N g of fiber waste was placed in a vessel containing 40N ml of 17% strength sodium hydroxide and treated in a water bath at 80 ℃ for 60 minutes.
It is understood that N g is used to indicate the proportioning relationship between the fiber waste and various solutions in the process, and the amount of the fiber waste can be arbitrarily selected by those skilled in the art, so long as the proportion of the formula is kept consistent, and the invention falls into the technical scheme.
Step 2, performing water filtration on the product obtained in the step 1 for deep washing, and bleaching for 30 minutes at 95 ℃ by using 10% hydrogen peroxide;
step 3, thoroughly washing the cellulose obtained in the step 2 with distilled water, filtering, and extruding the residual solution by a squeezer; drying in a hot air oven at 60 deg.C for 60 min; the resulting N g of cellulose was placed in a vessel, hydrolyzed using 20N ml of a solution containing 2.5% hydrogen chloride, and hydrolyzed at 105 ℃ for 15 minutes.
And 4, pouring the hot acid mixture obtained in the step 3 into 200N milliliters of cold tap water, stirring the mixture by using a magnetic stirrer at a speed of more than 600r/min, and standing the mixture for 24 hours.
Step 5, filtering and cleaning the microcrystalline cellulose obtained in the step 4 until the microcrystalline cellulose is neutral; then, the mixture was filtered again, pressed, and dried in a hot air oven at 105 ℃ for 30 minutes to obtain microcrystalline cellulose.
Example 3:
embodiment 3 of the present invention discloses a method for preparing microcrystalline cellulose, comprising the steps of:
step 1, N g of fiber waste was placed in a container containing 40N ml of 25% strength sodium hydroxide and treated in a water bath at 100 ℃ for 80 minutes.
It is understood that N g is used to indicate the proportioning relationship between the fiber waste and various solutions in the process, and the amount of the fiber waste can be arbitrarily selected by those skilled in the art, so long as the proportion of the formula is kept consistent, and the invention falls into the technical scheme.
Step 2, performing water filtration on the product obtained in the step 1 for deep washing, and bleaching for 40 minutes at 120 ℃ by using 12% hydrogen peroxide;
step 3, thoroughly washing the cellulose obtained in the step 2 with distilled water, filtering, and extruding the residual solution by a dehydrator; drying in a hot air oven at 100 deg.C for 120 min; the resulting N g of cellulose was placed in a vessel, hydrolyzed using 20N ml of a solution containing 5% hydrogen chloride, and hydrolyzed at 120 ℃ for 30 minutes.
And 4, pouring the hot acid mixture obtained in the step 3 into 200N milliliters of cold tap water, stirring the mixture by using a magnetic stirrer at the speed of more than 700r/min, and standing the mixture for 48 hours.
Step 5, filtering and cleaning the microcrystalline cellulose obtained in the step 4 until the microcrystalline cellulose is neutral; then filtering again, pressing and drying for 60 minutes in a hot air oven at 120 ℃ to obtain the microcrystalline cellulose.
Compared with the prior art, the method has the beneficial effects that the waste fibers are used for preparing the microcrystalline cellulose, the prepared microcrystalline cellulose has good thermal stability, high polymerization degree and reasonable crystallinity, waste articles are utilized, and the method has good application value, is simple and easy to implement and is simple to operate.
The present applicant has described and illustrated embodiments of the present invention in detail with reference to the accompanying drawings, but it should be understood by those skilled in the art that the above embodiments are merely preferred embodiments of the present invention, and the detailed description is only for the purpose of helping the reader to better understand the spirit of the present invention, and not for limiting the scope of the present invention, and on the contrary, any improvement or modification made based on the spirit of the present invention should fall within the scope of the present invention.
Claims (10)
1. A preparation method of microcrystalline cellulose is characterized by comprising the following steps:
step 1, putting fiber waste into a container filled with sodium hydroxide with set concentration, and treating in a water bath;
step 2, performing water filtration on the product obtained in the step 1 for deep washing, and bleaching by using hydrogen peroxide;
step 3, thoroughly washing the cellulose obtained in the step 2 with distilled water, filtering, and extruding the residual solution; drying in a hot air oven; the obtained N g of cellulose is put into a container and hydrolyzed by using a solution containing hydrogen chloride;
step 4, pouring the hot acid mixture obtained in the step 3 into cold tap water, stirring by using a magnetic stirrer, and then standing;
step 5, filtering and cleaning the microcrystalline cellulose obtained in the step 4 until the microcrystalline cellulose is neutral; then filtering, pressing and drying in a hot air oven to obtain the microcrystalline cellulose.
2. The method for producing microcrystalline cellulose according to claim 1, characterized in that:
in step 1, N g of fiber waste is put into a container filled with 40N ml of 15% -25% sodium hydroxide and treated in water bath at 60-100 ℃ for 40-80 minutes.
3. The method for producing microcrystalline cellulose according to claim 2, characterized in that:
in step 1, N g of the fiber waste was placed in a vessel containing 40N ml of 17% strength sodium hydroxide and treated in a water bath at 80 ℃ for 60 minutes.
4. The method for producing microcrystalline cellulose according to claim 1, characterized in that:
in step 2, the product of step 1 is subjected to water filtration for deep washing, and 8% -12% of hydrogen peroxide is used for bleaching for 20-40 minutes at 80-120 ℃.
5. The method for producing microcrystalline cellulose according to claim 4, characterized in that:
in step 2, the product of step 1 was subjected to water filtration for deep washing, and bleached with 10% hydrogen peroxide at 95 ℃ for 30 minutes.
6. The method for producing microcrystalline cellulose according to any one of claims 1, 2, or 4, characterized in that:
in step 3, thoroughly washing the cellulose obtained in step 2 with distilled water, filtering, and manually or by a dehydrator to extrude the residual solution; drying in a hot air oven at 50-100 deg.C for 30-120 min; the obtained N g of cellulose is put into a container, hydrolyzed by using 20N ml of solution containing 1 to 5 percent of hydrogen chloride and hydrolyzed for 20 to 30 minutes at the temperature of between 80 and 120 ℃.
7. The method for producing microcrystalline cellulose according to any one of claims 1, 2, or 4, characterized in that:
in step 3, thoroughly washing the cellulose obtained in step 2 with distilled water, filtering, and extruding the residual solution by a squeezer; drying in a hot air oven at 60 deg.C for 60 min; the resulting N g of cellulose was placed in a vessel, hydrolyzed using 20N ml of a solution containing 2.5% hydrogen chloride, and hydrolyzed at 105 ℃ for 15 minutes.
8. The method for producing microcrystalline cellulose according to any one of claims 1, 2, or 4, characterized in that:
in step 4, the hot acid mixture obtained in step 3 is poured into 200N ml of cold tap water, stirred by a magnetic stirrer at a speed of more than 400r/min, and kept stand for a set time.
Preferably, the hot acid mixture obtained in step 3 is poured into 200N ml of cold tap water, stirred by using a magnetic stirrer at a speed of more than 600r/min, and left for 24-48 hours.
9. The method for producing microcrystalline cellulose according to any one of claims 1 to 8, characterized in that:
in step 5, filtering and cleaning the microcrystalline cellulose obtained in step 4 until the microcrystalline cellulose is neutral; then filtering, pressing and drying in a hot air oven at 80-120 ℃ for a set time to obtain the microcrystalline cellulose.
10. The method for producing microcrystalline cellulose according to claim 9, characterized in that:
in step 5, filtering and cleaning the microcrystalline cellulose obtained in step 4 until the microcrystalline cellulose is neutral; then, it was filtered again, pressed, and dried in a hot air oven at 105 ℃ for 30 minutes to obtain microcrystalline cellulose.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110106622.2A CN112940139A (en) | 2021-01-26 | 2021-01-26 | Novel preparation method of microcrystalline cellulose |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110106622.2A CN112940139A (en) | 2021-01-26 | 2021-01-26 | Novel preparation method of microcrystalline cellulose |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112940139A true CN112940139A (en) | 2021-06-11 |
Family
ID=76237275
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110106622.2A Pending CN112940139A (en) | 2021-01-26 | 2021-01-26 | Novel preparation method of microcrystalline cellulose |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112940139A (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3954727A (en) * | 1973-08-02 | 1976-05-04 | DSO"Pharmachim" | Method of producing microcrystalline cellulose |
| US20030089465A1 (en) * | 2001-11-02 | 2003-05-15 | David Schaible | Process for producing microcrystalline cellulose |
| CN101649569A (en) * | 2009-09-01 | 2010-02-17 | 陕西科技大学 | Process for preparing low-pollution wheatgrass microcrystalline cellulose |
| CN106749686A (en) * | 2016-11-29 | 2017-05-31 | 陕西科技大学 | A kind of preparation method of microcrystalline cellulose |
| CN108410923A (en) * | 2018-02-07 | 2018-08-17 | 兰州理工大学 | A kind of method that broomcorn straw prepares microcrystalline cellulose |
| CN109162137A (en) * | 2018-09-25 | 2019-01-08 | 武汉轻工大学 | A kind of microcrystalline cellulose and the method for preparing microcrystalline cellulose using agricultural crop straw |
-
2021
- 2021-01-26 CN CN202110106622.2A patent/CN112940139A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3954727A (en) * | 1973-08-02 | 1976-05-04 | DSO"Pharmachim" | Method of producing microcrystalline cellulose |
| US20030089465A1 (en) * | 2001-11-02 | 2003-05-15 | David Schaible | Process for producing microcrystalline cellulose |
| CN101649569A (en) * | 2009-09-01 | 2010-02-17 | 陕西科技大学 | Process for preparing low-pollution wheatgrass microcrystalline cellulose |
| CN106749686A (en) * | 2016-11-29 | 2017-05-31 | 陕西科技大学 | A kind of preparation method of microcrystalline cellulose |
| CN108410923A (en) * | 2018-02-07 | 2018-08-17 | 兰州理工大学 | A kind of method that broomcorn straw prepares microcrystalline cellulose |
| CN109162137A (en) * | 2018-09-25 | 2019-01-08 | 武汉轻工大学 | A kind of microcrystalline cellulose and the method for preparing microcrystalline cellulose using agricultural crop straw |
Non-Patent Citations (1)
| Title |
|---|
| 李明皓等: "微晶纤维素的合成", 《广东化工》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102643357B (en) | Method for preparing sodium carboxymethylcellulose by abandoned cotton fabrics | |
| CN107629245B (en) | Recycling method of waste polyester-cotton blended fabric under hydrothermal condition | |
| CN103061174A (en) | Strong acid pretreatment assisted cellulose nano-filament preparation method | |
| CN103012605B (en) | Method for preparing high-retention environmental-friendly one-step double-modified starch | |
| CN101003577A (en) | Technique for producing polyanionic cellulose with high degree of substitution | |
| CN101994168A (en) | Method for preparing high-strength carrageenin fibers | |
| CN101161685A (en) | Method for preparing surface sizing fecula by synchronous etherification oxidation semi-dry process | |
| CN109485053A (en) | A method of white carbon black co-product soda ash and sodium metasilicate are prepared using carbon dioxide gas | |
| CN107915783A (en) | A kind of method that carboxymethyl cellulose is prepared using waste paper as raw material | |
| CN103554247A (en) | Method for preparing collagen microfiber by use of ionic liquid mixing solvent | |
| CN103804172A (en) | Method for improving organic acid product quality | |
| CN112940139A (en) | Novel preparation method of microcrystalline cellulose | |
| CN111101191A (en) | Method for preparing gypsum whisker by seed crystal method | |
| CN106866827A (en) | Modified nanometer cellulose containing various functional groups and preparation method thereof | |
| CN111019003A (en) | Waste fabric nanocellulose and preparation method thereof | |
| CN101412658B (en) | Method for saponification and acidolysis of hydrogenated castor oil by using high concentration acid and alkali | |
| CN109208118A (en) | A kind of production method producing disposable lanyard using soybean fiber | |
| CN107540749A (en) | A kind of preparation method of acetic acid octanoic acid cellulose esters | |
| CN109535486B (en) | Method for preparing high-viscosity nanofiber gel by using celery | |
| CN101440132A (en) | Preparation of technology level sodium carboxymethylcellulose | |
| CN107419355B (en) | A kind of processing method of useless acrylic fibres cloth | |
| CN111518227A (en) | Preparation method of agar glue solution | |
| CN101823786B (en) | Method for reducing production wastewater quantity of ramie fibre | |
| CN108708208A (en) | The method for preparing low polymerization degree low crystallinity cellulose using high-temperature heat treatment | |
| JPH0324497B2 (en) |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20210611 |
|
| RJ01 | Rejection of invention patent application after publication |