CN107541975B - A kind of activation method of carboxymetholcel - Google Patents
A kind of activation method of carboxymetholcel Download PDFInfo
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- CN107541975B CN107541975B CN201710546335.7A CN201710546335A CN107541975B CN 107541975 B CN107541975 B CN 107541975B CN 201710546335 A CN201710546335 A CN 201710546335A CN 107541975 B CN107541975 B CN 107541975B
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- carboxymetholcel
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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 44
- 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
- IOLCXVTUBQKXJR-UHFFFAOYSA-M potassium bromide Chemical compound [K+].[Br-] IOLCXVTUBQKXJR-UHFFFAOYSA-M 0.000 claims abstract description 8
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000000908 ammonium hydroxide Substances 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
- 238000001035 drying Methods 0.000 claims description 11
- 239000002245 particle Substances 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 238000000498 ball milling Methods 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 239000001257 hydrogen Substances 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 claims description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 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 12
- 238000002156 mixing Methods 0.000 description 5
- 238000009833 condensation Methods 0.000 description 3
- 230000005494 condensation Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000002994 raw material 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
- 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
- 239000000126 substance Substances 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
- 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
- 239000006227 byproduct 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
- 230000008859 change Effects 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
- 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
- 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
- 239000000203 mixture Substances 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
- 239000000047 product Substances 0.000 description 1
- 238000000926 separation method Methods 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
- Polysaccharides And Polysaccharide Derivatives (AREA)
- Paper (AREA)
Abstract
The present invention discloses a kind of activation method of carboxymetholcel, first pass through mechanical ball mill primary activation cellulose, then the sodium hydroxide solution boiling for being 3~5% with mass fraction, the mass fraction of sodium hydroxide is adjusted to 6~7% again after cooling and the activator being made of the ammonium hydroxide that 3~7 parts of potassium bromide, 10~18 parts of sodium chloride and 20~25 parts of mass fractions are 25% is added, 3~5h is reacted under 600~1000W microwave condition, finally filters and filter residue is washed till neutrality obtains activated cellulose.The present invention has the characteristics that economical, efficient and activation effect is good.
Description
Technical field
The present invention relates to a kind of activation methods of carboxymetholcel.
Background technique
Wheat Straw is the harvested by-product of northern China wheat, and annual output is huge, but only small part is used for papermaking
Industry, most Wheat Straw are incinerated or abandon, and the gas of considerable damage environment can be given off when burning Wheat Straw, simultaneously also
There are fire hazards.The main component of Wheat Straw is cellulose, hemicellulose and lignin, and wherein cellulose contains 40% left side
The content on the right side, cellulose is 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 derivatives such as cellophane and nitrate, acetate；It can also make
At 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 that activated fiber is prepared is the project with major economic value, how
Efficiently, activated fiber is economically prepared then becomes the difficult point of research.
Summary 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 cooperate activator activated cellulose with lye with alkaline process purification cellulose.
In order to solve the above technical problems, the present invention adopts the following technical scheme:
A kind of activation method of carboxymetholcel, comprising the following steps:
S1. by Wheat Straw, drying to constant weight at 40~60 DEG C, is then comminuted into particle, and particle is crossed the sieve of 60 mesh again
It is added in ball mill, 1.5~2.5h of revolving speed ball milling at 45~70 DEG C with 500~800r/min obtains pretreatment wheat straw
Stalk；Drying Wheat Straw is the toughness in order to weaken Wheat Straw, so that ball milling function more effectively destroys the crystal region of cellulose, it is real
The primary activation of existing cellulose；
S2. based on parts by weight, take the pretreatment Wheat Straw in 50 parts of S1, be added equipped with 1000 parts of mass fractions be 3~
In the container of 5% sodium hydroxide solution, the container top is equipped with condensing unit, and container stirs 1 under 90~95 DEG C of water-baths
~2h, mixing speed are 350~450r/min, and bath temperature is adjusted to room temperature after stirring, then continues to add into container
Adding sodium hydroxide so that the concentration of sodium hydroxide rises to 6~7% in solution continues that activator is added 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 cooperation microwave pair
Wheat Straw activation, microwave energy weaken the influence of hydrogen bond in cellulose, activator are enabled more effectively to activate Wheat Straw；
S3. the solution in container filters solution after S2 microwave reaction, then with water by residue washing into
Property, then it is placed in baking oven with 45~50 DEG C that drying to constant weight, finally obtain activation carboxymetholcel.
The ammonium hydroxide that the activator is 25% by 3~7 parts of potassium bromide, 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 the advantages that pollution is small, activation effect is good, activity function is high；The present invention will
The sodium hydroxide of the purification of cellulose saves raw material, reduces operating cost for cooperating activator to activate；This law is easy to operate,
It can operate continuously, activation efficiency is high, is suitble to industrialized production.
Specific embodiment
Below with reference to specific embodiment, the present invention will be further described.
Embodiment 1
A kind of activation method of carboxymetholcel, comprising the following steps:
S1. by Wheat Straw, drying to constant weight at 55 DEG C, is then comminuted into particle, and the sieve that particle crosses 60 mesh is added
Into ball mill, the revolving speed ball milling 1.5h at 45 DEG C with 800r/min obtains pretreatment Wheat Straw；
S2. based on parts by weight, the pretreatment Wheat Straw in 50 parts of S1 is taken, being added equipped with 1000 parts of mass fractions is 3%
Sodium hydroxide solution there-necked flask in, a side port of the there-necked flask side is equipped with snakelike condensation, another side port rubber plug
It closes, blender is equipped at the positive mouth of there-necked flask, there-necked flask stirs 1.5h under 95 DEG C of water-baths, and mixing speed 400r/min is stirred
Bath temperature is adjusted to room temperature after mixing, 30 parts of sodium hydroxides are then added into there-necked flask, continues that 3 parts are added into container
The ammonium hydroxide that potassium bromide, 14 parts of sodium chloride and 25 parts of mass fractions are 25% forms, then container is placed in the microwave reactor of 700W
Middle reaction 3.5h；
S3. the solution in container filters solution after S2 microwave reaction, then with water by residue washing into
Property, then it is placed in baking oven with 45 DEG C that drying to constant weight, finally obtain activation carboxymetholcel.
Embodiment 2
A kind of activation method of carboxymetholcel, comprising the following steps:
S1. by Wheat Straw, drying to constant weight at 40 DEG C, is then comminuted into particle, and the sieve that particle crosses 60 mesh is added
Into ball mill, the revolving speed ball milling 2h at 70 DEG C with 600r/min obtains pretreatment Wheat Straw；
S2. based on parts by weight, the pretreatment Wheat Straw in 50 parts of S1 is taken, being added equipped with 1000 parts of mass fractions is 5%
Sodium hydroxide solution there-necked flask in, a side port of the there-necked flask side is equipped with snakelike condensation, another side port rubber plug
It closes, blender is equipped at the positive mouth of there-necked flask, there-necked flask stirs 1h, mixing speed 3500r/min under 90 DEG C of water-baths, stirs
After bath temperature is adjusted to room temperature, 20 parts of sodium hydroxides are then added into there-necked flask, are continued into container plus 7 parts of brominations
The ammonium hydroxide that potassium, 10 parts of sodium chloride and 20 parts of mass fractions are 25% forms, then container is placed in the microwave reactor of 600W instead
Answer 5h；
S3. the solution in container filters solution after S2 microwave reaction, then with water by residue washing into
Property, then it is placed in baking oven with 50 DEG C that drying to constant weight, finally obtain activation carboxymetholcel.
Embodiment 3
A kind of activation method of carboxymetholcel, comprising the following steps:
S1. by Wheat Straw, drying to constant weight at 60 DEG C, is then comminuted into particle, and the sieve that particle crosses 60 mesh is added
Into ball mill, the revolving speed ball milling 2.5h at 55 DEG C with 500r/min obtains pretreatment Wheat Straw；
S2. based on parts by weight, the pretreatment Wheat Straw in 50 parts of S1 is taken, being added equipped with 1000 parts of mass fractions is 4%
Sodium hydroxide solution there-necked flask in, a side port of the there-necked flask side is equipped with snakelike condensation, another side port rubber plug
It closes, blender is equipped at the positive mouth of there-necked flask, there-necked flask stirs 2h, mixing speed 450r/min under 93 DEG C of water-baths, stirs
After bath temperature is adjusted to room temperature, 25 parts of sodium hydroxides are then added into there-necked flask, continue that 5 parts of bromines are added into container
Change the ammonium hydroxide that potassium, 16 parts of sodium chloride and 23 parts of mass fractions are 25% to form, then container is placed in the microwave reactor of 1000W
React 3h；
S3. the solution in container filters solution after S2 microwave reaction, then with water by residue washing into
Property, then it is placed in baking oven with 48 DEG C that drying to constant weight, finally obtain activation carboxymetholcel.
Protection scope of the present invention is not limited merely to above-described embodiment, and all technical solutions belonged under thinking of the present invention are equal
It belongs to the scope of protection of the present invention.It should be pointed out that for those skilled in the art, not departing from the present invention
Several improvements and modifications under the premise of principle, these modifications and embellishments should also be considered as the scope of protection of the present invention.
Claims (2)
1. a kind of activation method of carboxymetholcel, which comprises the following steps:
S1. by Wheat Straw, drying to constant weight at 40 ~ 60 DEG C, is then comminuted into particle, and the sieve that particle crosses 60 mesh is added
Into ball mill, 1.5 ~ 2.5h of revolving speed ball milling at 45 ~ 70 DEG C with 500 ~ 800r/min obtains pretreatment Wheat Straw；
S2. based on parts by weight, the pretreatment Wheat Straw in 50 parts of S1 is taken, the hydrogen for being 3 ~ 5% equipped with 1000 parts of mass fractions is added
In the container of sodium hydroxide solution, the container top is equipped with condensing unit, and container stirs 1 ~ 2h under 90 ~ 95 DEG C of water-baths, stirs
Speed is 350 ~ 450r/min, and bath temperature is adjusted to room temperature after stirring, then continues to add sodium hydroxide into container,
So that the concentration of sodium hydroxide rises to 6 ~ 7% in solution, continue that activator is added into container, then container is placed in microwave ring
3 ~ 5h is reacted in border；
S3. the solution in container filters solution after S2 microwave reaction, then with water by residue washing to neutrality, then
It is placed in baking oven with 45 ~ 50 DEG C that drying to constant weight, finally obtains activation carboxymetholcel；
The activator is made of the ammonium hydroxide that 3 ~ 7 parts of potassium bromide, 10 ~ 18 parts of sodium chloride and 20 ~ 25 parts of mass fractions are 25%.
2. a kind of activation method of carboxymetholcel according to claim 1, which is characterized in that the power of the microwave
For 600 ~ 1000W.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710546335.7A CN107541975B (en) | 2017-07-06 | 2017-07-06 | A kind of activation method of carboxymetholcel |
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| CN201710546335.7A CN107541975B (en) | 2017-07-06 | 2017-07-06 | A kind of activation method of carboxymetholcel |
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| CN107541975A CN107541975A (en) | 2018-01-05 |
| CN107541975B true CN107541975B (en) | 2019-06-11 |
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| 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 |
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 |
-
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 |
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