CN105906845B - A kind of cellulose acetate micelle and its manufacture method - Google Patents
A kind of cellulose acetate micelle and its manufacture method Download PDFInfo
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- CN105906845B CN105906845B CN201610274539.5A CN201610274539A CN105906845B CN 105906845 B CN105906845 B CN 105906845B CN 201610274539 A CN201610274539 A CN 201610274539A CN 105906845 B CN105906845 B CN 105906845B
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- cellulose acetate
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- plasticizer
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L1/00—Compositions of cellulose, modified cellulose or cellulose derivatives
- C08L1/08—Cellulose derivatives
- C08L1/10—Esters of organic acids, i.e. acylates
- C08L1/12—Cellulose acetate
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- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention belongs to acetate fiber to manufacture field, and in particular to a kind of cellulose acetate micelle and its manufacture method.The technical problems to be solved by the invention are to provide a kind of manufacture method of cellulose acetate micelle, comprise the following steps:Cellulose acetate is mixed with stabilizer, plasticizer, fully curing, extrusion, cooling, pelletizing produces cellulose acetate micelle;Prepare chemical cellulose in the raw cellulose of cellulose acetate and account for more than the 97% of cellulose gross weight;The addition of plasticizer accounts for cellulose acetate, stabilizer, the 17~25% of plasticizer three's gross weight.The inventive method prepare cellulose acetate micelle hardness is more preferable, toughness is more preferable, spectacles industry can be performed well in.
Description
Technical field
The invention belongs to acetate fiber to manufacture field, and in particular to a kind of cellulose acetate micelle and its manufacturer
Method.
Background technology
Cellulose acetate offset plate material picture frame have it is nonflammable, hardly changed colour by ultraviolet irradiation, glossiness
Preferably, it is durable, be easy to heating processing, style is more attractive in appearance, wear after the advantages that being unlikely to deform.
At present frequently with being that raw material produces cellulose acetate containing a certain amount of chemical cellulose, then by cellulose acetate powder
Plasticizer with being mixed with certain stabilizer is sufficiently mixed and cured, and fully the cellulose acetate after curing is squeezed using twin-screw
Go out machine to be produced as production equipment.Chemical cellulose content is 95~97% in the cellulosic material of this method;Under plasticizer is
At least one of row material, repefral, diethyl phthalate, tri-n-butyl citrate, citric acid three
Ethyl ester, triacetyl glycerine, plasticizer loading are 26~32%;It is steady that stabilizer includes but is not limited to antioxidant, heat stabilizer, light
Determine agent, processing aid.But the cellulose acetate that this method is prepared has the shortcomings that poor toughness, low intensity, so as to limit it
In the application of eye glass frame industry.
The content of the invention
The shortcomings of for existing cellulose acetate poor toughness, low intensity, the invention provides one kind to manufacture cellulose acetate
The new method of micelle.This method prepare cellulose acetate micelle hardness is more preferable, toughness is more preferable, so as to the picture frame prepared is thinner,
So as to which weight is lighter.
First technical problem to be solved by this invention is to provide a kind of manufacture method of cellulose acetate micelle.The party
Method comprises the following steps:Cellulose acetate and stabilizer, plasticizer are mixed, fully curing, extrusion, cooling, pelletizing produces vinegar
Acid cellulose micelle;Prepare chemical cellulose in the raw cellulose of cellulose acetate and account for more than the 97% of cellulose gross weight;Plasticising
The addition of agent accounts for the 17~25% of cellulose acetate, stabilizer and plasticizer three's gross weight.
Preferably, in the manufacture method of above-mentioned cellulose acetate micelle, it is fine to prepare α in the raw cellulose of cellulose acetate
Dimension element accounts for more than the 99% of cellulose gross weight.
Preferably, in the manufacture method of above-mentioned cellulose acetate micelle, described abundant curing is to place 12h at normal temperatures
More than.
Preferably, in the manufacture method of above-mentioned cellulose acetate micelle, the temperature of the extrusion is 150~250 DEG C.
Preferably, in the manufacture method of above-mentioned cellulose acetate micelle, described cellulose acetate is plastics level.
Specifically, in the manufacture method of above-mentioned cellulose acetate micelle, described plasticizer is that this area prepares acetic acid fibre
Tie up the Conventional plasticizers that plain micelle uses.
Specifically, in the manufacture method of above-mentioned cellulose acetate micelle, described stabilizer is that this area prepares acetic acid fibre
Tie up the conventional stabilizer that plain micelle uses;Including at least one of antioxidant, light stabilizer, processing aid.
Preferably, in the manufacture method of above-mentioned cellulose acetate micelle, the addition of the antioxidant account for cellulose acetate,
The 0.15~5% of stabilizer and plasticizer three's gross weight.
Preferably, in the manufacture method of above-mentioned cellulose acetate micelle, the addition of the processing aid accounts for acetate fiber
The 0.1~0.5% of plain, stabilizer and plasticizer three's gross weight.
Preferably, in the manufacture method of above-mentioned cellulose acetate micelle, the weight ratio of light stabilizer and plasticizer is 0.65
~0.75 ︰ 100.
Second technical problem to be solved by this invention is to provide the cellulose acetate micelle that the above method is prepared.
The present inventor has found reasonably to allocate the addition of plasticizer through overtesting, and accounts for more than 99% using chemical cellulose
Cellulose acetate micelle prepared by cellulose acetate powder stock that cellulose is prepared can overcome existing micelle poor toughness,
The shortcomings of low intensity.Good product performance prepared by this method, operating method are simple.
Embodiment
Inventor has found that the content control of plasticizer is prepared into cellulose acetate within a certain range to carry through overtesting
High fracture tensile strength, modulus of elasticity, Rockwell Hardness enhancing, but impact strength can be reduced again;In order to make up impact strength
Reduce, inventor has found through overtesting again, selection chemical cellulose weight account for more than 97% cellulose of whole cellulose for
Cellulose acetate prepared by raw material, then the cellulose acetate is used to preparing cellulose acetate micelle to can to make up above-mentioned impact strong
Spend the defects of low.Preferably, more than 99% is accounted for.
Cellulose acetate in the inventive method, in addition to chemical cellulose content in raw cellulose and existing method difference,
Other raw materials are the convenient sources that this area prepares cellulose acetate, recycle the conventional method of this area that this hair is prepared
Bright feed material plastics level cellulose acetate.
Plasticizer in the inventive method prepares the Conventional plasticizers that cellulose acetate micelle uses for this area, may be selected from
In repefral, diethyl phthalate, tri-n-butyl citrate, triethyl citrate or triacetyl glycerine
At least one, but be not limited to above-mentioned substance.
Stabilizer in the inventive method prepares the conventional stabilizer that cellulose acetate micelle uses for this area, may be selected from
At least one of antioxidant, light stabilizer, processing aid, but it is not limited to above-mentioned substance.
Further, the antioxidant may be selected from β-positive octadecanol ester of (3,5- di-tert-butyl-hydroxy phenyl) propionic acid,
Double (2,4- DI-tert-butylphenol compounds) pentaerythritol diphosphites, epoxy resin, β-(3,5- di-tert-butyl-hydroxy phenyls) third
Compound, the four [β-(3,5- di-t-butyl -4- hydroxyls of sour positive octadecanol ester and three [2.4- di-tert-butyl-phenyls] phosphite esters
Base phenyl) propionic acid] pentaerythritol ester, three [2.4- di-tert-butyl-phenyls] phosphite esters, a benzene didecyl, poly- (DPG) benzene
At least one of base ester, 3,5- di-tert-butyl-hydroxy phenyl propionic acid isooctanol esters, but it is not limited to above-mentioned substance.
Further, the processing aid may be selected from least one of ethanol, acetone, but be not limited to above-mentioned substance.
Further, the light stabilizer may be selected from BTA, N- (2- ethoxyl phenenyls)-N/- (4- ethylphenyls)-
At least one of oxalamide, but it is not limited to above-mentioned substance.
Embodiment 1
By weight, by 78 parts of cellulose acetate, 22 parts of additive (additive is stabilizer and plasticizer, wherein, increase
21.692 parts of agent is moulded, plasticizer is diethyl phthalate) it is added in high speed mixer, control temperature is in 80 DEG C of stirrings
1h, room temperature 12h in storage tank is put into after the completion of stirring, and material is fully cured standby;Squeezed using double screw extruder
Go out, extrusion temperature is 170 DEG C, and pelletizing is carried out through supercooling after extrusion, and particle dries 4h in 80 DEG C of baking ovens.
Cellulose acetate is that chemical cellulose accounts for 98% cellulose and is prepared according to a conventional method by raw material in the present embodiment.
Stabilizer in the present embodiment prepares the conventional stabilizer of cellulose acetate micelle, the present embodiment addition for this area
1076 0.11 part of (β-positive octadecanol ester of (3,5- di-tert-butyl-hydroxy phenyls) propionic acid), 626 (double (2,4- di-tert-butyls
Phenol) pentaerythritol diphosphites) 0.066 part, 0.132 part of 828 (epoxy resin).
Stabilizer and plasticizer are put into preparation tank in the present embodiment and stirred, temperature control is at 60~65 DEG C, stirring
Between 6~8h additive is prepared.
Embodiment 2
By weight, by 81 parts of cellulose acetate, stabilizer and plasticizer totally 19 parts (additive is stabilizer and plasticising
Agent, wherein, 18.62 parts of plasticizer, plasticizer is diethyl phthalate) it is added in high speed mixer, control temperature exists
75 DEG C of stirring 1h, room temperature 12h in storage tank is put into after the completion of stirring, and material is fully cured standby;Use double screw extruder
Extruded, extrusion temperature is 200 DEG C, and pelletizing is carried out through supercooling after extrusion, and particle dries 4h in 80 DEG C of baking ovens.
Cellulose acetate is that chemical cellulose accounts for 99.2% cellulose and is prepared into according to a conventional method by raw material in the present embodiment
Arrive.
Stabilizer in the present embodiment prepares the conventional stabilizer of cellulose acetate micelle, the present embodiment addition for this area
1076 0.076 part of (β-positive octadecanol ester of (3,5- di-tert-butyl-hydroxy phenyls) propionic acid), 626 (double (2,4- di-t-butyls
Phenol) pentaerythritol diphosphites) 0.057 part, 0.114 part of 828 (epoxy resin), N- (2- ethoxyl phenenyls)-N/-(4-
Ethylphenyl) 0.133 part of-oxalamide.
Stabilizer and plasticizer are put into preparation tank in the present embodiment and stirred, temperature control is at 60~65 DEG C, stirring
Between 6~8h additive is prepared.
Test example 1
Chemical cellulose content accounts for 96% in cellulosic material, and processing conditions is fixed, and stabilizer formula is fixed, plasticizer loading
Change, its proportion is analyzed also according to ASTM D792;Its tensile strength is tested according to ASTM D638;Divide according to ASTM D790
Analyse its modulus of elasticity;Its Rockwell Hardness is analyzed according to ASTM D785;Its impact strength, which is analyzed, according to ASTM D256 obtains each number
According to see the table below 1:
Table 1
As can be seen from Table 1, obtained by experiment, with the reduction of plasticizer loading, its hardness is significantly increased
Add, but at the same time, its impact strength then reduces with the reduction of diethyl phthalate content.
Test example 2
Processing conditions is fixed, and stabilizer formula is fixed, and diethyl phthalate content is fixed as 27%, and α is fine in raw material
Cellulose content change is tieed up, result is obtained and see the table below 2:
Table 2
As can be seen from Table 2, the impact strength of cellulose acetate in by raw material chemical cellulose content influenceed it is more bright
Aobvious, its impact strength is as the chemical cellulose content of cellulose acetate raw material improves and improves.
Test example 3
The cellulose acetate micelle performance comparison that cellulose acetate micelle prepared by the inventive method is prepared with existing method
Such as table 3 below:
Table 3
The inventive method reasonably have adjusted the content of plasticizer, the content of chemical cellulose, so as to be prepared for hardness it is more preferable,
The more preferable cellulose acetate micelle of toughness, improves processing characteristics, so as to which cellulose acetate picture frame is made into thinner, more
It is narrow, mitigate picture frame overall weight, reduce glasses production cost.
Claims (5)
1. a kind of manufacture method of cellulose acetate micelle, comprises the following steps:Cellulose acetate and stabilizer, plasticizer are mixed
Even, fully curing, extrusion, cooling, pelletizing produces cellulose acetate micelle;It is characterized in that:Prepare the raw material of cellulose acetate
Chemical cellulose accounts for more than the 97% of cellulose gross weight in cellulose;The addition of plasticizer accounts for cellulose acetate, stabilizer and increasing
Mould the 17~25% of agent three's gross weight;Described stabilizer is antioxidant, light stabilizer and processing aid, the processing aid
Addition account for the 0.1~0.5% of cellulose acetate, stabilizer and plasticizer three's gross weight, the processing aid is selected from second
At least one of alcohol, acetone;The temperature of the extrusion is 150~250 DEG C;
The addition of the antioxidant accounts for the 0.15~5% of cellulose acetate, stabilizer and plasticizer three's gross weight;Light is stable
The weight of agent and plasticizer ratio is 0.65~0.75 ︰ 100.
2. manufacture method according to claim 1, it is characterised in that:It is fine to prepare α in the raw cellulose of cellulose acetate
Dimension element accounts for more than the 99% of cellulose gross weight.
3. manufacture method according to claim 1 or 2, it is characterised in that:Described cellulose acetate is plastics level.
4. manufacture method according to claim 1 or 2, it is characterised in that:Described plasticizer is that this area prepares acetic acid
The Conventional plasticizers that cellulose micelle uses.
A kind of 5. cellulose acetate micelle, it is characterised in that:It is prepared into as the manufacture method described in any one of Claims 1 to 4
Arrive.
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CN107286375A (en) * | 2017-07-26 | 2017-10-24 | 深圳市集美新材料股份有限公司 | Glasses slab rubber and its manufacture method |
CN109369963A (en) * | 2018-09-17 | 2019-02-22 | 济南大自然新材料有限公司 | A kind of method that useless diacetate fiber prepares diacetate fiber micelle |
CN117417230A (en) * | 2022-11-11 | 2024-01-19 | 孟玄新材料有限公司 | Process for recovery of acetic acid and other valuable materials from cellulose acetate waste by pyrolysis |
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CN101346510A (en) * | 2006-01-13 | 2009-01-14 | 赛拉尼斯醋酸盐有限公司 | Manufacture of cellulose esters: recycle of caustic and/or acid from pre-treatment of pulp |
CN105504359A (en) * | 2016-01-12 | 2016-04-20 | 宜宾学院 | Cellulose acetate particles and preparing method thereof |
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CN101346510A (en) * | 2006-01-13 | 2009-01-14 | 赛拉尼斯醋酸盐有限公司 | Manufacture of cellulose esters: recycle of caustic and/or acid from pre-treatment of pulp |
CN105504359A (en) * | 2016-01-12 | 2016-04-20 | 宜宾学院 | Cellulose acetate particles and preparing method thereof |
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