CN107541975A - A kind of activation method of carboxymetholcel - Google Patents
A kind of activation method of carboxymetholcel Download PDFInfo
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- CN107541975A CN107541975A CN201710546335.7A CN201710546335A CN107541975A CN 107541975 A CN107541975 A CN 107541975A CN 201710546335 A CN201710546335 A CN 201710546335A CN 107541975 A CN107541975 A CN 107541975A
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- carboxymetholcel
- wheat straw
- activation
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- 230000004913 activation Effects 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 title claims abstract description 14
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 38
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 12
- 239000012190 activator Substances 0.000 claims abstract description 9
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 6
- 239000011780 sodium chloride Substances 0.000 claims abstract description 6
- 241000209140 Triticum Species 0.000 claims description 28
- 235000021307 Triticum Nutrition 0.000 claims description 28
- 239000010902 straw Substances 0.000 claims description 27
- 239000002245 particle Substances 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 238000000498 ball milling Methods 0.000 claims description 6
- 239000004744 fabric Substances 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 230000008859 change Effects 0.000 claims description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims 1
- 229910052760 oxygen Inorganic materials 0.000 claims 1
- 239000001301 oxygen Substances 0.000 claims 1
- 229910052708 sodium Inorganic materials 0.000 claims 1
- 239000011734 sodium Substances 0.000 claims 1
- 229920002678 cellulose Polymers 0.000 abstract description 17
- 239000001913 cellulose Substances 0.000 abstract description 16
- 230000000694 effects Effects 0.000 abstract description 3
- 238000009835 boiling Methods 0.000 abstract description 2
- 238000001816 cooling Methods 0.000 abstract 1
- 235000010980 cellulose Nutrition 0.000 description 15
- 235000011121 sodium hydroxide Nutrition 0.000 description 11
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000009833 condensation Methods 0.000 description 3
- 230000005494 condensation Effects 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 229920002488 Hemicellulose Polymers 0.000 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- -1 decoration Substances 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 239000011591 potassium Substances 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- LNAZSHAWQACDHT-XIYTZBAFSA-N (2r,3r,4s,5r,6s)-4,5-dimethoxy-2-(methoxymethyl)-3-[(2s,3r,4s,5r,6r)-3,4,5-trimethoxy-6-(methoxymethyl)oxan-2-yl]oxy-6-[(2r,3r,4s,5r,6r)-4,5,6-trimethoxy-2-(methoxymethyl)oxan-3-yl]oxyoxane Chemical compound CO[C@@H]1[C@@H](OC)[C@H](OC)[C@@H](COC)O[C@H]1O[C@H]1[C@H](OC)[C@@H](OC)[C@H](O[C@H]2[C@@H]([C@@H](OC)[C@H](OC)O[C@@H]2COC)OC)O[C@@H]1COC LNAZSHAWQACDHT-XIYTZBAFSA-N 0.000 description 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- 229920002955 Art silk Polymers 0.000 description 1
- 244000025254 Cannabis sativa Species 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 1
- 229920000298 Cellophane Polymers 0.000 description 1
- 239000001856 Ethyl cellulose Substances 0.000 description 1
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000031709 bromination Effects 0.000 description 1
- 238000005893 bromination reaction Methods 0.000 description 1
- 125000001246 bromo group Chemical class Br* 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 239000001768 carboxy methyl cellulose Substances 0.000 description 1
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 1
- 239000008112 carboxymethyl-cellulose Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 235000019504 cigarettes Nutrition 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 238000005553 drilling Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 235000019325 ethyl cellulose Nutrition 0.000 description 1
- 229920001249 ethyl cellulose Polymers 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000000077 insect repellent Substances 0.000 description 1
- 229920005610 lignin Polymers 0.000 description 1
- 229920000609 methyl cellulose Polymers 0.000 description 1
- 239000001923 methylcellulose Substances 0.000 description 1
- 235000010981 methylcellulose Nutrition 0.000 description 1
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 description 1
- 239000001814 pectin Substances 0.000 description 1
- 235000010987 pectin Nutrition 0.000 description 1
- 229920001277 pectin Polymers 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229920000447 polyanionic polymer Polymers 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 1
- 229910001948 sodium oxide Inorganic materials 0.000 description 1
- KEAYESYHFKHZAL-IGMARMGPSA-N sodium-23 atom Chemical group [23Na] KEAYESYHFKHZAL-IGMARMGPSA-N 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
Landscapes
- Paper (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The present invention discloses a kind of activation method of carboxymetholcel, first pass through mechanical ball mill primary activation cellulose, then with the sodium hydroxide solution boiling that mass fraction is 3~5%, the mass fraction of sodium hydroxide is adjusted to 6~7% again after cooling and adds the activator being made up of the ammoniacal liquor that 3~7 parts of KBrs, 10~18 parts of sodium chloride and 20~25 parts of mass fractions are 25%, 3~5h is reacted under 600~1000W microwave conditions, is finally filtered and filter residue is washed till neutrality is obtained activated cellulose.The present invention has the characteristics of economic, efficient and activation effect is good.
Description
Technical field
The present invention relates to a kind of activation method of carboxymetholcel.
Background technology
Wheat Straw is the harvested accessory substance of northern China wheat, and annual production is huge, but only small part is used for papermaking
Industry, most Wheat Straw are incinerated or abandoned, and the gas of considerable damage environment can be given off when burning Wheat Straw, also simultaneously
Disaster hidden-trouble be present.The main component of Wheat Straw is cellulose, hemicellulose and lignin, and it is left to contain 40% for wherein cellulose
The right side, the content of cellulose are considerable.Cellulose of the whole world for papermaking of weaving, every year up to 8,000,000 tons.In addition, with separation
The cellulose of purifying does raw material, can manufacture artificial silk, the ester derivative such as cellophane and nitrate, acetate；Also can make
Into ether derivatives such as methylcellulose, ethyl cellulose, carboxymethyl cellulose, polyanion celluloses, for oil drilling,
Food, ceramic glaze, daily use chemicals, synthesis of detergent, graphite product, pencil manufacture, electronics, coating, building materials, decoration, mosquito-repellent incense, cigarette
Grass, papermaking, rubber, agricultural, adhesive, plastics, explosive, electrician and Scientific Research Equipments etc..Therefore, renewable resource will be used as
Wheat Straw in cellulose extract and activate be prepared activated fiber be one have major economic value problem, how
Efficiently, activated fiber is economically prepared then becomes the difficult point of research.
The content of the invention
The present invention provides a kind of activation method of carboxymetholcel, first passes through mechanical ball mill primary activation cellulose, then
Finally coordinate activator activated cellulose with alkali lye with alkaline process purification cellulose.
In order to solve the above technical problems, the present invention adopts the following technical scheme that：
A kind of activation method of carboxymetholcel, comprises the following steps：
S1. Wheat Straw is dried to constant weight at 40~60 DEG C, is then comminuted into particle, particle is crossed into the screen cloth of 60 mesh again
It is added in ball mill, pretreatment wheat straw is obtained with 500~800r/min 1.5~2.5h of rotating speed ball milling at 45~70 DEG C
Stalk；It is to weaken the toughness of Wheat Straw to dry Wheat Straw so that ball milling function more effectively destroys the crystal region of cellulose, real
The primary activation of existing cellulose；
S2. in terms of parts by weight, take the pretreatment Wheat Straw in 50 parts of S1, add equipped with 1000 parts of mass fractions be 3~
In the container of 5% sodium hydroxide solution, the container top is provided with condensing unit, and container stirs 1 under 90~95 DEG C of water-baths
~2h, mixing speed are 350~450r/min, stir and bath temperature is adjusted into room temperature after terminating, then continue to add into container
It is hydrogenated with sodium oxide molybdena so that the concentration of sodium hydroxide rises to 6~7% in solution, continues to add activator into container, then will hold
Device is placed in 3~5h of reaction in microwave environment；Wheat Straw uses sodium hydroxide solution boiling again after mechanical ball mill, removes wooden
While the impurity such as element, hemicellulose, pectin can also more effectively swollen Wheat Straw, finally reuse activator and coordinate microwave pair
Wheat Straw activates, and microwave energy weakens the influence of hydrogen bond in cellulose so that activator can more effectively activate Wheat Straw；
S3. the solution in container filters solution after S2 microwave reactions terminate, then with water by residue washing into
Property, then be placed in baking oven and be dried to constant weight with 45~50 DEG C, finally obtain activation carboxymetholcel.
The ammoniacal liquor that the activator is 25% by 3~7 parts of KBrs, 10~18 parts of sodium chloride and 20~25 parts of mass fractions
Composition.
The power of the microwave is 600~1000W.
Beneficial effects of the present invention：
The present invention prepares activated cellulose using Wheat Straw, and raw material sources are wide and cheap；It is fine that the present invention prepares activation
Dimension element combines physical method and chemical method, has and pollutes the advantages of small, activation effect is good, activity function is high；The present invention will
The sodium hydroxide of the purification of cellulose is used to coordinate activator to activate, and saves raw material, reduces operating cost；This law is simple to operate,
It can operate continuously, activation efficiency is high, is adapted to industrialized production.
Embodiment
Below with reference to specific embodiment, the present invention will be further described.
Embodiment 1
A kind of activation method of carboxymetholcel, comprises the following steps：
S1. Wheat Straw is dried to constant weight at 55 DEG C, is then comminuted into particle, the screen cloth that particle is crossed to 60 mesh adds
Into ball mill, pretreatment Wheat Straw is obtained with 800r/min rotating speed ball milling 1.5h at 45 DEG C；
S2. in terms of parts by weight, the pretreatment Wheat Straw in 50 parts of S1 is taken, it is 3% to add equipped with 1000 parts of mass fractions
Sodium hydroxide solution there-necked flask in, a side port of the there-necked flask side is provided with snakelike condensation, another side port plug
Close, be provided with agitator at the positive mouth of there-necked flask, there-necked flask stirs 1.5h under 95 DEG C of water-baths, mixing speed 400r/min, stirred
Mix and bath temperature is adjusted to room temperature after terminating, 30 parts of sodium hydroxides are then added into there-necked flask, continue to add 3 parts into container
The ammoniacal liquor that KBr, 14 parts of sodium chloride and 25 parts of mass fractions are 25% is formed, then container is placed in 700W microwave reactor
Middle reaction 3.5h；
S3. the solution in container filters solution after S2 microwave reactions terminate, then with water by residue washing into
Property, then be placed in baking oven and be dried to constant weight with 45 DEG C, finally obtain activation carboxymetholcel.
Embodiment 2
A kind of activation method of carboxymetholcel, comprises the following steps：
S1. Wheat Straw is dried to constant weight at 40 DEG C, is then comminuted into particle, the screen cloth that particle is crossed to 60 mesh adds
Into ball mill, pretreatment Wheat Straw is obtained with 600r/min rotating speed ball milling 2h at 70 DEG C；
S2. in terms of parts by weight, the pretreatment Wheat Straw in 50 parts of S1 is taken, it is 5% to add equipped with 1000 parts of mass fractions
Sodium hydroxide solution there-necked flask in, a side port of the there-necked flask side is provided with snakelike condensation, another side port plug
Close, agitator is provided with the positive mouth of there-necked flask, there-necked flask stirs 1h, mixing speed 3500r/min under 90 DEG C of water-baths, stirring
Bath temperature is adjusted to room temperature after end, 20 parts of sodium hydroxides are then added into there-necked flask, continues to add 7 parts of brominations into container
The ammoniacal liquor that potassium, 10 parts of sodium chloride and 20 parts of mass fractions are 25% is formed, then container is placed in 600W microwave reactor instead
Answer 5h；
S3. the solution in container filters solution after S2 microwave reactions terminate, then with water by residue washing into
Property, then be placed in baking oven and be dried to constant weight with 50 DEG C, finally obtain activation carboxymetholcel.
Embodiment 3
A kind of activation method of carboxymetholcel, comprises the following steps：
S1. Wheat Straw is dried to constant weight at 60 DEG C, is then comminuted into particle, the screen cloth that particle is crossed to 60 mesh adds
Into ball mill, pretreatment Wheat Straw is obtained with 500r/min rotating speed ball milling 2.5h at 55 DEG C；
S2. in terms of parts by weight, the pretreatment Wheat Straw in 50 parts of S1 is taken, it is 4% to add equipped with 1000 parts of mass fractions
Sodium hydroxide solution there-necked flask in, a side port of the there-necked flask side is provided with snakelike condensation, another side port plug
Close, agitator is provided with the positive mouth of there-necked flask, there-necked flask stirs 2h, mixing speed 450r/min under 93 DEG C of water-baths, stirring
Bath temperature is adjusted to room temperature after end, 25 parts of sodium hydroxides are then added into there-necked flask, continues to add 5 parts of bromines into container
Change the ammoniacal liquor that potassium, 16 parts of sodium chloride and 23 parts of mass fractions are 25% to form, then container is placed in 1000W microwave reactor
React 3h；
S3. the solution in container filters solution after S2 microwave reactions terminate, then with water by residue washing into
Property, then be placed in baking oven and be dried to constant weight with 48 DEG C, finally obtain activation carboxymetholcel.
Protection scope of the present invention is not limited merely to above-described embodiment, and all technical schemes for belonging under thinking of the present invention are equal
Belong to protection scope of the present invention.It should be pointed out that for those skilled in the art, the present invention is not being departed from
Some improvements and modifications under the premise of principle, these improvements and modifications also should be regarded as protection scope of the present invention.
Claims (3)
1. a kind of activation method of carboxymetholcel, it is characterised in that comprise the following steps：
S1. Wheat Straw is dried to constant weight at 40~60 DEG C, is then comminuted into particle, the screen cloth that particle is crossed to 60 mesh adds
Into ball mill, pretreatment Wheat Straw is obtained with 500~800r/min 1.5~2.5h of rotating speed ball milling at 45~70 DEG C；
S2. in terms of parts by weight, the pretreatment Wheat Straw in 50 parts of S1 is taken, it is 3~5% to add equipped with 1000 parts of mass fractions
In the container of sodium hydroxide solution, the container top is provided with condensing unit, and container stirs 1~2h under 90~95 DEG C of water-baths,
Mixing speed is 350~450r/min, stirs and bath temperature is adjusted into room temperature after terminating, and then continues to add hydrogen-oxygen into container
Change sodium so that the concentration of sodium hydroxide rises to 6~7% in solution, continues to add activator into container, then container is placed in
3~5h is reacted in microwave environment；
S3. the solution in container filters solution after S2 microwave reactions terminate, then with water by residue washing to neutrality, then
It is placed in baking oven and is dried to constant weight with 45~50 DEG C, finally obtains activation carboxymetholcel.
2. the activation method of a kind of carboxymetholcel according to claim 1, it is characterised in that the activator is by 3
The ammoniacal liquor that~7 parts of KBrs, 10~18 parts of sodium chloride and 20~25 parts of mass fractions are 25% forms.
A kind of 3. activation method of carboxymetholcel according to claim 1, it is characterised in that the power of the microwave
For 600~1000W.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710546335.7A CN107541975B (en) | 2017-07-06 | 2017-07-06 | A kind of activation method of carboxymetholcel |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710546335.7A CN107541975B (en) | 2017-07-06 | 2017-07-06 | A kind of activation method of carboxymetholcel |
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| Publication Number | Publication Date |
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| CN107541975A true CN107541975A (en) | 2018-01-05 |
| CN107541975B CN107541975B (en) | 2019-06-11 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109295719A (en) * | 2018-09-30 | 2019-02-01 | 安徽农业大学 | A kind of chitin modified oxidized fibre cellulose fabric of durable antibiotic and preparation method thereof |
| CN116000066A (en) * | 2022-12-05 | 2023-04-25 | 四川大学 | Method for treating woody plant garbage by microwave coupling alkali |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA2728689A1 (en) * | 2008-07-03 | 2010-01-07 | Novozymes A/S | Process for producing fermentation products |
| CN102266755A (en) * | 2011-07-04 | 2011-12-07 | 广西大学 | Method for preparing cellulose-based toxic gas adsorbing material |
| CN102776594A (en) * | 2012-07-10 | 2012-11-14 | 东华大学 | Cellulose fiber-supported nano silver antibacterial material and preparation method thereof |
| CN103243139A (en) * | 2013-05-21 | 2013-08-14 | 河南工业大学 | Method for efficiently degrading lignocelluloses raw material |
-
2017
- 2017-07-06 CN CN201710546335.7A patent/CN107541975B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA2728689A1 (en) * | 2008-07-03 | 2010-01-07 | Novozymes A/S | Process for producing fermentation products |
| CN102266755A (en) * | 2011-07-04 | 2011-12-07 | 广西大学 | Method for preparing cellulose-based toxic gas adsorbing material |
| CN102776594A (en) * | 2012-07-10 | 2012-11-14 | 东华大学 | Cellulose fiber-supported nano silver antibacterial material and preparation method thereof |
| CN103243139A (en) * | 2013-05-21 | 2013-08-14 | 河南工业大学 | Method for efficiently degrading lignocelluloses raw material |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109295719A (en) * | 2018-09-30 | 2019-02-01 | 安徽农业大学 | A kind of chitin modified oxidized fibre cellulose fabric of durable antibiotic and preparation method thereof |
| CN116000066A (en) * | 2022-12-05 | 2023-04-25 | 四川大学 | Method for treating woody plant garbage by microwave coupling alkali |
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| CN107541975B (en) | 2019-06-11 |
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