CN108003295A - A kind of preparation method of modified cellulose acetate - Google Patents
A kind of preparation method of modified cellulose acetate Download PDFInfo
- Publication number
- CN108003295A CN108003295A CN201711348995.0A CN201711348995A CN108003295A CN 108003295 A CN108003295 A CN 108003295A CN 201711348995 A CN201711348995 A CN 201711348995A CN 108003295 A CN108003295 A CN 108003295A
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- cellulose acetate
- preparation
- modified cellulose
- necked flask
- reaction
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F251/00—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof
- C08F251/02—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof on to cellulose or derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—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 a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/04—Acids; Metal salts or ammonium salts thereof
- C08F220/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The present invention proposes a kind of preparation method of modified cellulose acetate, comprises the following steps：(1) 10.0g cellulose acetates and 120mL deionized waters are placed in the three-necked flask of 250mL, load onto blender and condenser, be passed through N220~60min, O in abundant emptier2；(2) 1.5g nitric acid alms bowl hinge is dissolved in concentration to be added in 1.0mol/L salpeter solutions as initiator in reaction bulb, after 0.5h initiations are reacted at 60 DEG C, 2.0g acrylic monomers is slowly added dropwise in reaction vessel, 10~15h of isothermal reaction at 60 DEG C；(3) three-necked flask is taken out and stood, remove supernatant liquid, lower floor's powdery product is washed with absolute ethyl alcohol, is filtered under diminished pressure, repetitive operation 3~4 times, and modified cellulose acetate is made.The functional modification cellulose acetate that the present invention obtains, can apply the seperation film of the filter stick for having good selectivity retention harmful substances in flue gas with industrialized production and excellent membrane separating effect.
Description
Technical field
The present invention relates to cellulose acetate preparing technical field, and in particular to a kind of preparation side of modified cellulose acetate
Method.
Background technology
Cellulose acetate (CA) is to be matched somebody with somebody to acetify a kind of obtained thermoplastic resin by catalytic action with acid by cellulose, is
Utilize film raw material the most universal on the market now, have cheap, chemical stabilization, high mechanical strength, heat endurance it is good,
Filming technology is simple and material source extensively, the advantages that being easy to get, be widely used in manufacturing spectacle frame, coating, textile fabric, perfume (or spice)
Cigarette filter tip, plastics, film, seperation film etc..Meanwhile CA also has chemistry, heat endurance, hot-working character, poor mechanical property etc.
Shortcoming, and also there are other a large amount of problems in application process.In this regard, scientific worker has done substantial amounts of research work.For
Improve the spinnability of CA melt spinnings, plasticization and modification is carried out using additional plasticizer Dichlorodiphenyl Acetate cellulose, although improving
The spinnability of CA, but exudation and the resolution problem of plasticizer are also brought at the same time.In filter tip acetate fiber, loaded
Metallic catalyst is crossed, improve selective absorption effect of the filter tip material to oxynitrides etc., but due to loaded article in itself
The complexity of toxicity and loading process, limits the application of this method.In order to improve the separating effect of cellulose-acetafolic,
Carry out low-temperature oxygen plasma surface modification, the increase that water penetration can be at double.But this method equipment is relative complex, mechanism of modification
It is not very clearly, to be difficult to realize controllable modified.
The content of the invention
In view of the deficiencies of the prior art, the present invention proposes a kind of preparation method of modified cellulose acetate.
The technical proposal of the invention is realized in this way：A kind of preparation method of modified cellulose acetate, including following step
Suddenly：
(1) 10.0g cellulose acetates and 120mL deionized waters are placed in the three-necked flask of 250mL, load onto blender with
Condenser, is passed through N220~60min, O in abundant emptier2；
(2) 1.5g nitric acid alms bowl hinge is dissolved in concentration to be added to reaction bulb as initiator in 1.0mol/L salpeter solutions
It is interior, after 0.5h initiations are reacted at 60 DEG C, 2.0g acrylic monomers is slowly added dropwise in reaction vessel, it is permanent at 60 DEG C
10~15h of temperature reaction；
(3) three-necked flask is taken out and stood, remove supernatant liquid, lower floor's powdery product is washed with absolute ethyl alcohol, depressurized
Filtering, repetitive operation 3~4 times, is made modified cellulose acetate, and modified cellulose acetate then is put into 60 DEG C of vacuum drying chambers
Middle 20~36h of drying, finished product.
Further, it is passed through N in step (1)20 time is 30min.
Further, salpeter solution is 20mL in step (2).
Further, the isothermal reaction time is 12h in step (2).
Further, the time dry in step (5) is 20~36h.
Compared with prior art, the present invention has the following advantages：Present invention process is easy to operate, and reaction condition is gentle, fits
Mass produced for industrializing.The applicable most olefin monomer of the invention, and can by varying reaction condition,
To control graft polymers chain length.Linked in addition, modified cellulose acetate has both original vinegar acid cellulose matrix with branch
Branch polymer advantage, select the modification vinegar that different graft polymers can obtain difference in functionality fine.Therefore, it is of the invention to obtain
The functional modification cellulose acetate arrived, can apply has good selectivity retention harmful substances in flue gas with industrialized production
Filter stick and excellent membrane separating effect seperation film.
Embodiment
Below to technical scheme being clearly and completely described in conjunction with the embodiments, it is clear that described reality
It is only part of the embodiment of the present invention to apply example, instead of all the embodiments.Based on the embodiments of the present invention, this area is general
Logical technical staff all other embodiments obtained without creative efforts, belong to what the present invention protected
Scope.
A kind of preparation method of modified cellulose acetate, comprises the following steps：
(1) 10.0g cellulose acetates and 120mL deionized waters are placed in the three-necked flask of 250mL, load onto blender with
Condenser, is passed through N220~60min, O in abundant emptier2；
(2) 1.5g nitric acid alms bowl hinge is dissolved in concentration to be added to reaction bulb as initiator in 1.0mol/L salpeter solutions
It is interior, after 0.5h initiations are reacted at 60 DEG C, 2.0g acrylic monomers is slowly added dropwise in reaction vessel, it is permanent at 60 DEG C
10~15h of temperature reaction；
(3) three-necked flask is taken out and stood, remove supernatant liquid, lower floor's powdery product is washed with absolute ethyl alcohol, depressurized
Filtering, repetitive operation 3~4 times, is made modified cellulose acetate, and modified cellulose acetate then is put into 60 DEG C of vacuum drying chambers
Middle 20~36h of drying, finished product.
In above-described embodiment, step is passed through N in (1)20 time is 30min.
In above-described embodiment, salpeter solution is 20mL in step (2).
In above-described embodiment, the isothermal reaction time is 12h in step (2).
In above-described embodiment, the dry time is 20~36h in step (5).
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
With within principle, any modification, equivalent replacement, improvement and so on, should all be included in the protection scope of the present invention god.
Claims (5)
1. a kind of preparation method of modified cellulose acetate, it is characterised in that comprise the following steps：
(1) 10.0g cellulose acetates and 120mL deionized waters are placed in the three-necked flask of 250mL, load onto blender and condensation
Device, is passed through N220~60min, O in abundant emptier2；
(2) 1.5g nitric acid alms bowl hinge is dissolved in concentration to be added in 1.0mol/L salpeter solutions as initiator in reaction bulb,
After 0.5h initiations are reacted at 60 DEG C, 2.0g acrylic monomers is slowly added dropwise in reaction vessel, constant temperature is anti-at 60 DEG C
Answer 10~15h；
(3) three-necked flask being taken out and stood, remove supernatant liquid, lower floor's powdery product is washed with absolute ethyl alcohol, is filtered under diminished pressure,
Repetitive operation 3~4 times, is made modified cellulose acetate, and then modified cellulose acetate is put into 60 DEG C of vacuum drying chambers and is done
Dry 20~36h, finished product.
2. preparation method as claimed in claim 1, it is characterised in that step is passed through N in (1)20 time is 30min.
3. preparation method as claimed in claim 1, it is characterised in that salpeter solution is 20mL in step (2).
4. preparation method as claimed in claim 1, it is characterised in that the isothermal reaction time is 12h in step (2).
5. preparation method as claimed in claim 1, it is characterised in that the dry time is 20~36h in step (5).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711348995.0A CN108003295A (en) | 2017-12-15 | 2017-12-15 | A kind of preparation method of modified cellulose acetate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711348995.0A CN108003295A (en) | 2017-12-15 | 2017-12-15 | A kind of preparation method of modified cellulose acetate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108003295A true CN108003295A (en) | 2018-05-08 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
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| CN201711348995.0A Withdrawn CN108003295A (en) | 2017-12-15 | 2017-12-15 | A kind of preparation method of modified cellulose acetate |
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| Country | Link |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57174367A (en) * | 1981-04-20 | 1982-10-27 | Kazuo Saotome | Adhesive composition |
| CN103193938A (en) * | 2013-05-03 | 2013-07-10 | 云南烟草科学研究院 | Preparation method of modified cellulose acetate |
| CN104126870A (en) * | 2014-07-18 | 2014-11-05 | 云南中烟工业有限责任公司 | Manufacturing method and application of anionic polymer modified cellulose acetate |
| CN104130355A (en) * | 2014-07-18 | 2014-11-05 | 云南中烟工业有限责任公司 | Preparation method and use of hydrophobic polymer-modified cellulose acetate |
-
2017
- 2017-12-15 CN CN201711348995.0A patent/CN108003295A/en not_active Withdrawn
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57174367A (en) * | 1981-04-20 | 1982-10-27 | Kazuo Saotome | Adhesive composition |
| CN103193938A (en) * | 2013-05-03 | 2013-07-10 | 云南烟草科学研究院 | Preparation method of modified cellulose acetate |
| CN104126870A (en) * | 2014-07-18 | 2014-11-05 | 云南中烟工业有限责任公司 | Manufacturing method and application of anionic polymer modified cellulose acetate |
| CN104130355A (en) * | 2014-07-18 | 2014-11-05 | 云南中烟工业有限责任公司 | Preparation method and use of hydrophobic polymer-modified cellulose acetate |
Non-Patent Citations (1)
| Title |
|---|
| 许耀光等: "丙烯酸/醋酸纤维素超滤膜的改性及制备", 《林业工程学报》 * |
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Application publication date: 20180508 |