CN106916341A - The manufacture method of acetate fiber promotor composition - Google Patents
The manufacture method of acetate fiber promotor composition Download PDFInfo
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- CN106916341A CN106916341A CN201610865255.3A CN201610865255A CN106916341A CN 106916341 A CN106916341 A CN 106916341A CN 201610865255 A CN201610865255 A CN 201610865255A CN 106916341 A CN106916341 A CN 106916341A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/10—Esters; Ether-esters
- C08K5/101—Esters; Ether-esters of monocarboxylic acids
- C08K5/103—Esters; Ether-esters of monocarboxylic acids with polyalcohols
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/10—Esters; Ether-esters
- C08K5/11—Esters; Ether-esters of acyclic polycarboxylic acids
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
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- Chemical Kinetics & Catalysis (AREA)
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Abstract
The present invention relates to the manufacture method of acetate fiber promotor composition, problem of the invention is the manufacture method of the acetate fiber promotor composition for providing the manufacture material for turning into the products formed that flexibility is high and impact resistance is good.Therefore, the manufacture method of acetate fiber promotor composition of the invention includes：Relative to the mass parts of (A) cellulose acetate 100, do not include more than aromatic ring and the mass parts of plasticizer 20 of 200~450g/mol of molecular weight and mixed in addition (B) molecule, wherein, the total capacity of (A) composition and (B) composition is more than 10L, and relative to (A) composition, whole additions of (B) composition are added mixing several times by described in.
Description
Technical field
Acetate fiber the present invention relates to turn into the manufacture material of the products formed with flexibility and with high-impact
The manufacture method of the manufacture method of promotor composition and above-mentioned products formed.
Background technology
Cellulose acetate is not enough due to thermoplasticity, therefore is used generally in the form of the composition comprising plasticizer.
In British Patent No. 2489491, describing can add water miscible increasing in acetate fiber promotor composition
Modeling agent preferably adds 25 mass % or 20 mass % (page 10) up to reaching 30 mass %.In embodiment, 10 matter are with the addition of
Measure the plasticizer of % or 20 mass %, but its actual usage amount (gross mass or total of cellulose acetate and glycerol triacetate
Capacity) it is unknown.
In the embodiment 1~2 of Japanese Unexamined Patent Publication 2002-060545 publications, describe the weight % of cellulose acetate 70
Supplied to double screw extruder with the weight % of glycerol triacetate 30 and pellet is carried out in 220 DEG C, and in embodiment 7~9
In, describe and be stirred in a in a henschel mixer with the ratio shown in table 3 by cellulose acetate and glycerol triacetate
Afterwards, using single screw extrusion machine come shaping membrane.However, its actual usage amount (cellulose acetate and glycerol triacetate
Gross mass or total capacity) it is unknown.
The content of the invention
Problem of the invention is to provide the manufacture material turned into flexibility and the products formed with high-impact
Acetate fiber promotor composition manufacture method and the manufacture method of above-mentioned products formed.
The present invention provides the manufacture method of acetate fiber promotor composition and the manufacture method of products formed, the cellulose acetate
The manufacture method of composition includes：Relative to the mass parts of (A) cellulose acetate 100, aromatic ring is not included in addition (B) molecule and is divided
More than the mass parts of plasticizer 20 of 200~450g/mol of son amount and mixed, wherein, above-mentioned (A) composition and above-mentioned (B) composition
Total capacity be more than 10L, and relative to above-mentioned (A) composition, whole additions of above-mentioned (B) composition are added several times
Plus mixing.
In addition, the present invention provides the manufacture method of acetate fiber promotor composition and the manufacture method of products formed, the acetic acid
The manufacture method of cellulose composition includes：Relative to the mass parts of (A) cellulose acetate 100, not comprising virtue in addition (B) molecule
More than the mass parts of plasticizer 20 of ring and 200~450g/mol of molecular weight and mixed, wherein, above-mentioned (A) composition and above-mentioned
(B) total capacity of composition is more than 10L, and the manufacture method has relative to above-mentioned (A) composition, by the whole of above-mentioned (B) composition
Addition adds the 1st operation mixed into mixer and the composition supply that will be obtained in above-mentioned 1st operation several times
The 2nd operation of extrusion molding is carried out to extruder, and in above-mentioned 1st operation, is had between multiple addition mixed processes
There is refrigerating work procedure.
Additionally, the present invention provides the manufacture method of acetate fiber promotor composition and the manufacture method of products formed, the acetic acid
The manufacture method of cellulose composition includes：Relative to the mass parts of (A) cellulose acetate 100, not comprising virtue in addition (B) molecule
More than the mass parts of plasticizer 20 of ring and 200~450g/mol of molecular weight and mixed, wherein, above-mentioned (A) composition and above-mentioned
(B) total capacity of composition is more than 10L, and the manufacture method has relative to above-mentioned (A) composition, by the whole of above-mentioned (B) composition
A part for addition 1 time adds the 1st operation mixed into mixer and will be in above-mentioned 1st operation several times
The composition for obtaining supplies to extruder the 2nd operation for carrying out extrusion molding, and in above-mentioned 1st operation, adds in multiple
Plus there is refrigerating work procedure between mixed processes, in above-mentioned 2nd operation, above-mentioned (B) composition of surplus is supplied to extruder.
Manufacturing method according to the invention, even if in the case of the addition for increasing plasticizer, it is also possible to obtain acetic acid
Cellulose and plasticizer have obtained the mobility composition high of homogeneous mixing, thus can make the composition based on extruder into
Type workability becomes good.
In addition it is possible to improve the physical property when the composition to being molded using extruder carries out injection moulding.
Specific embodiment
<The manufacture method of acetate fiber promotor composition>
The cellulose acetate of (A) composition used in manufacture method of the invention is known cellulose acetate, at this
In invention, preferably substitution value (substitution value of acetyl group) is less than 2.7 cellulose acetate, and more preferably substitution value is 2~2.7
Cellulose acetate.
Aromatic ring and 200~450g/ of molecular weight are not included in the molecule of (B) composition used in manufacture method of the invention
The plasticizer of mol is preferably selected from glycerol triacetate (triacetic acid glycerine) (molecular weight 218g/mol), triethyl citrate and (divides
Son amount 276g/mol), the composition of tributyl 2-acetylcitrate (molecular weight 402g/mol).
In manufacture method of the invention, relative to (A) composition, whole additions of (B) composition are carried out several times
Addition mixing.
In manufacture method of the invention, cellulose acetate group can be manufactured by the 1st manufacture method and the 2nd manufacture method
Compound.
(1) the 1st manufacture method
1st manufacture method is following methods：
It has：
Relative to (A) composition, whole additions of (B) composition are added the 1st work mixed into mixer several times
Sequence；With
The composition (intermediate composition) that will be obtained in above-mentioned 1st operation is supplied to extruder and carries out extrusion molding
2nd operation,
In above-mentioned 1st operation, there is refrigerating work procedure between multiple addition mixed processes.
In 1st operation, relative to (A) composition, whole additions of (B) composition are added several times and is mixed to mixer
In.
When carrying out adding mixing several times, preferably 2~4 times, more preferably 2 times or 3 times.
When adding (B) composition several times, the addition of 1 time is less than 20 mass preferably with respect to the mass parts of (A) composition 100
Below part, more preferably 18 mass parts, below more preferably 15 mass parts.
(B) when the addition number of times of composition is n times, preferably every time for 1/n measures degree.When addition number of times is 2 times, preferably divide 2
Secondary addition, every time 1/2 amount degree of addition, when addition number of times is 3 times, preferably divide 3 additions, every time 1/3 amount degree of addition, but respectively
Secondary addition can also be different.
Mixer has no specifically limited, usable rotary drum mixer, Henschel mixer, spiral ribbon mixer, kneader etc.
Mixer.
Mixer is preferably used can be with more than rotating speed 200r/min, preferably more than 400r/min, more preferably 500r/min
More than it is stirred the high-speed mixer of mixing.
In the 1st operation, (A) composition of whole amount and (B) composition of partial amount are added in mixer and is mixed
After conjunction, cooled down between the addition for carrying out subsequent (B) composition mixes.
When (B) composition is added in dividing 2 times to (A) composition, implement 1 cooling, the addition (B) in dividing 3 times to (A) composition
During composition, implement 2 coolings.
Cooling means can be used：Natural cooling (for example, being placed in the temperature atmosphere of 20~30 DEG C of room temperature), air-supply
Cooling, with state configuration condenser pipe contact around mixer and the side that makes circulation water in above-mentioned condenser pipe and cooled down
The cooling means such as method.
During using natural cooling as cooling means, mix and put by the stopping after mixing in 1~10 minute is carried out
20~50 minutes are put to be cooled down.
As adding proportion of (B) composition relative to (A) composition used in manufacture method of the invention, relative to
(A) mass parts of composition 100, (B) composition is more than 20 mass parts, is preferably 25~45 mass parts, more preferably 28~40 mass
Part, more preferably 30~40 mass parts.
In addition, the total capacity of (A) composition used in manufacture method of the invention and (B) composition be more than 10L, preferably
It is more than 50L, more preferably more than 100L.
(even if B) composition relative to (A) composition adding proportion in above range, in (A) composition and total appearance of (B) composition
In the case that amount is small (for example, in the case of below 1L), because total amount is a small amount of, therefore manufacture of the invention need not be used
Method, direct can be kneaded using such in the embodiment 1,2 of Japanese Unexamined Patent Publication 2002-060545 publications using extruder
Method, the embodiment 7~9 of same document in such entered using extruder after being mixed using Henschel mixer
The method of row mixing.
If however, the total capacity of (A) composition and (B) composition is in more than 10L, using Japanese Unexamined Patent Publication 2002-060545
During method as described in the embodiment of number publication, as shown in comparative example of the invention 1~3, it is difficult to produce with
Composition of the above-mentioned adding proportion comprising (A) composition and (B) composition.
In the 2nd operation, (A) composition and the composition (intermediate composition) of (B) composition that will be obtained in the 1st operation are supplied
To carrying out extrusion molding to extruder.
In the 2nd operation, can extrusion molding be carried out to be molded pellet, it is also possible to which extrusion molding is membranaceous, sheet, tubular
Etc. desired shape.
In the 1st operation or the 2nd operation, as needed, it is also possible to add in the range of problem of the invention can solve the problem that
Plus known resin additive.
As known resin additive, can enumerate：Packing material, fire retardant, flame retardant, stabilizer (antioxidant,
Ultra-violet absorber, heat stabilizer, photostabilizer etc.), colouring agent, antistatic additive, lubricant, antiblocking agent, dispersant, antiseptic
Deng.
(2) the 2nd manufacture methods
2nd manufacture method is following methods：
It has：
Relative to (A) composition, mixing is added the part 1 time in whole additions of (B) composition or several times
The 1st operation into mixer；With
Composition (intermediate composition) supply that will be obtained in the 1st operation is kneaded and is extruded into extruder
2nd operation of type,
In the 1st operation, there is refrigerating work procedure between multiple addition mixed processes,
In the 2nd operation, remaining above-mentioned (B) composition is supplied to extruder.
In 1st operation, relative to (A) composition, by the part 1 time in whole additions of (B) composition or several times
Ground addition mixes into mixer.
In the 1st operation, preferably add (B) composition whole additions 30~60% amounts, more preferably add 35~
50% amount.
In addition, whole additions of (B) composition of the 1st operation are less than 20 mass preferably with respect to the mass parts of (A) composition 100
Below part, more preferably 18 mass parts, below more preferably 15 mass parts.
When carrying out adding mixing several times, preferably 2 times, 1/2 amount degree is preferably added every time.
Mixer has no specifically limited, usable rotary drum mixer, Henschel mixer, spiral ribbon mixer, kneader etc.
Mixer.
Mixer is preferably used can be with more than rotating speed 200r/min, preferably more than 400r/min, more preferably 500r/min
More than it is stirred the high-speed mixer of mixing.
In the 1st operation, in mixer add whole amount (A) composition and partial amount (B) composition and mixed.
When mixing (B) composition is added in dividing 2 times to (A) composition, 1 cooling is implemented therebetween.
Cooling means can be used：Natural cooling (for example, being placed in the temperature atmosphere of 20~30 DEG C of room temperature), air-supply
Cooling, with state configuration condenser pipe contact around mixer and the side that makes circulation water in above-mentioned condenser pipe and cooled down
The cooling means such as method.
During using natural cooling as cooling means, mix and put by the stopping after mixing in 1~10 minute is carried out
20~50 minutes are put to be cooled down.
As adding proportion of (B) composition relative to (A) composition used in manufacture method of the invention, relative to
(A) mass parts of composition 100, (B) composition is more than 20 mass parts, is preferably 25~45 mass parts, more preferably 28~40 mass
Part, more preferably 30~40 mass parts.
In addition, the total capacity of (A) composition used in manufacture method of the invention and (B) composition be more than 10L, preferably
It is more than 50L, more preferably more than 100L.
(even if B) composition relative to (A) composition adding proportion in above range, in (A) composition and total appearance of (B) composition
In the case that amount is small (for example, in the case of below 1L), because total amount is a small amount of, therefore manufacture of the invention need not be used
Method, direct can be kneaded using such in the embodiment 1,2 of Japanese Unexamined Patent Publication 2002-060545 publications using extruder
Method, the embodiment 7~9 of same document in such entered using extruder after being mixed using Henschel mixer
The method of row mixing.
If however, the total capacity of (A) composition and (B) composition is in more than 10L, using Japanese Unexamined Patent Publication 2002-060545
During method as described in the embodiment of number publication, as shown in comparative example of the invention 1~3, it is difficult to produce with
Composition of the above-mentioned adding proportion comprising (A) composition and (B) composition.
In the 2nd operation, the composition (intermediate composition) of (A) composition that will be obtained in the 1st operation and (B) composition with
And the surplus of (B) composition is supplied to extruder and carries out extrusion molding.
(B) surplus of composition can also be with (A) composition and the composition (middle groups of (B) composition obtained in the 1st operation
Compound) supply together to extruder, but preferably added from the midway (near centre position) of extruder.
In the 2nd operation, can extrusion molding be carried out to be molded pellet, it is also possible to which extrusion molding is membranaceous, sheet, tubular
Etc. desired shape.
In the 1st operation or the 2nd operation, as needed, it is also possible to add in the range of problem of the invention can solve the problem that
Plus known resin additive.
As known resin additive, can enumerate：Packing material, fire retardant, flame retardant, stabilizer (antioxidant,
Ultra-violet absorber, heat stabilizer, photostabilizer etc.), colouring agent, antistatic additive, lubricant, antiblocking agent, dispersant, antiseptic
Deng.
(manufacture method of products formed)
The manufacture method of products formed of the invention is to manufacture second by the 1st above-mentioned manufacture method or the 2nd manufacture method
After acid cellulose composition, manufactured by above-mentioned composition using the known resin forming method such as injection moulding, compressing
The method of desired products formed.
Products formed is the products formed being selected from piece, film, plate, pipe, rod obtained from manufacture method of the invention.
The products formed obtained using manufacture method of the invention is strong due to impact resistance, therefore can be set as OA/ household electrical appliances
The houses such as field of transport vehicles, the furniture/building materials such as standby field, electrical/electronic field, domain of communication equipment, health field, automobile
The parts and outer cover in association area, groceries field etc. are used.
In addition, the flexibility of the products formed obtained using manufacture method of the invention is also high, thus be also applied for directly with
The purposes of people's contact.
Hereinafter, record is of the invention preferred embodiment.
<1>
The manufacture method of acetate fiber promotor composition, it includes：
Relative to the mass parts of (A) cellulose acetate 100, in addition (B) molecule not comprising aromatic ring and molecular weight 200~
More than the mass parts of plasticizer 20 of 450g/mol and mixed, wherein,
The total capacity of above-mentioned (A) composition and above-mentioned (B) composition is more than 10L,
Relative to above-mentioned (A) composition, whole additions of above-mentioned (B) composition are added mixing several times.
<2>
The manufacture method of acetate fiber promotor composition, it includes：
Relative to the mass parts of (A) cellulose acetate 100, in addition (B) molecule not comprising aromatic ring and molecular weight 200~
More than the mass parts of plasticizer 20 of 450g/mol and mixed, wherein,
The total capacity of above-mentioned (A) composition and above-mentioned (B) composition is more than 10L,
The manufacture method has：Relative to above-mentioned (A) composition, by whole additions of above-mentioned (B) composition several times
Addition mixes the 1st operation into mixer；Carried out with the composition obtained in above-mentioned 1st operation is supplied to extruder
2nd operation of extrusion molding,
In above-mentioned 1st operation, there is refrigerating work procedure between multiple addition mixed processes.
<3>
It is above-mentioned<1>Or<2>Manufacture method, wherein, be repeatedly 2~4 times, be preferably 2 times or 3 times.
<4>
It is above-mentioned<1>~<3>Any one of manufacture method, wherein, repeatedly in every 1 time relative to (A) composition 100
The addition of mass parts (B) composition is less than 20 mass parts, is preferably below 18 mass parts, is more preferably below 15 mass parts, and
The addition of each time can also be different.
<5>
It is above-mentioned<1>~<4>Any one of manufacture method, wherein, be repeatedly n times, and every 1 time (B) composition
Addition is that 1/n measures degree.
<6>
The manufacture method of acetate fiber promotor composition, it includes：
Relative to the mass parts of (A) cellulose acetate 100, in addition (B) molecule not comprising aromatic ring and molecular weight 200~
More than the mass parts of plasticizer 20 of 450g/mol and mixed, wherein,
The total capacity of above-mentioned (A) composition and above-mentioned (B) composition is more than 10L,
The manufacture method has：Relative to above-mentioned (A) composition, by a part 1 for whole additions of above-mentioned (B) composition
Secondary ground adds the 1st operation mixed into mixer several times；Supplied with the composition that will be obtained in above-mentioned 1st operation
The 2nd operation of extrusion molding is carried out to extruder,
In above-mentioned 1st operation, addition mixed processes for repeatedly in the case of, repeatedly between have refrigerating work procedure,
In above-mentioned 2nd operation, above-mentioned (B) composition of surplus is supplied to extruder.
<7>
It is above-mentioned<6>Manufacture method, wherein, in above-mentioned 1st operation, add (B) composition whole additions 30~
60% amount, the amount for being preferably 35~50%.
<8>
It is above-mentioned<6>Or<7>Manufacture method, wherein, whole additions of (B) composition of the 1st operation are relative to (A) composition
100 mass parts are less than below 20 mass parts, preferably 18 mass parts, below more preferably 15 mass parts.
<9>
It is above-mentioned<6>~<8>Manufacture method, wherein, (B) composition in above-mentioned 1st operation point is added mixing 2 times.
<10>
It is above-mentioned<6>~<9>Manufacture method, wherein, in the 2nd operation, obtained in the surplus of (B) composition and the 1st operation
(A) composition and (B) composition composition (intermediate composition) be supplied to together extruder or from the midway of extruder (in
Between near position) be added.
<11>
It is above-mentioned<1>~<10>Any one of manufacture method, wherein, cooling means is the temperature in 20~30 DEG C of room temperature
The natural cooling placed in degree atmosphere, cooling method of blowing configure condensation with the state contacted around mixer
The method managed and make to circulate in above-mentioned condenser pipe water and cooled down.
<12>
It is above-mentioned<11>Manufacture method, wherein, natural cooling be carry out 1~10 minute mixing after stop mixing simultaneously
Place the cooling means of 20~50 minutes.
<13>
It is above-mentioned<1>~<12>Any one of manufacture method, wherein, addition ratio of (B) composition relative to (A) composition
Example be：Relative to the mass parts of (A) composition 100, (B) composition is preferably 25~45 mass parts, more preferably 28~40 mass parts, enters
One step is preferably 30~40 mass parts.
<14>
It is above-mentioned<1>~<13>Any one of manufacture method, wherein, (A) composition is preferred with the total capacity of (B) composition
It is more than 50L, more preferably more than 100L.
<15>
It is above-mentioned<1>~<14>Any one of manufacture method, wherein, in the 1st operation or the 2nd operation, according to need
Want and add packing material, fire retardant, flame retardant, stabilizer (antioxidant, ultra-violet absorber, heat stabilizer, photostabilizer
Deng), colouring agent, antistatic additive, lubricant, antiblocking agent, dispersant, the resin additive such as antiseptic.
<16>
It is above-mentioned<1>~<15>Any one of manufacture method, wherein, above-mentioned mixer is can be with rotating speed 200r/
More than min, preferably more than 400r/min, the high-speed mixer that more preferably more than 500r/min is stirred and mixes.
<17>
It is above-mentioned<1>~<16>Any one of manufacture method, wherein, above-mentioned (B) composition be selected from glycerol triacetate,
Triethyl citrate, tributyl 2-acetylcitrate.
<18>
The manufacture method of products formed, it includes：Utilize<1>~<17>Any one of manufacture method manufacture acetic acid it is fine
Tie up promotor composition operation and
By the operation of above-mentioned cellulose acetate composition molding.
<19>
It is above-mentioned<18>The manufacture method of described products formed, wherein, above-mentioned products formed is selected from piece, film, plate, cylinder, rod.
Embodiment
<Use composition>
(A) cellulose acetate
L-50, substitution value 2.5, viscometric degree of polymerization 180, (strain) Daicel systems
(B) plasticizer
Trade name " Triacetin DRA150 " (liquid), molecular weight 218, (strain) Daicel systems
(other)
Stabilizer 1：Trade name " Irgafos 168 ", BASF Japan (strain) systems
Stabilizer 2：Trade name " Adekacizer O-130P ", (strain) ADEKA systems
Stabilizer 3：Citric anhydride, Kishida Chemical (strain) systems
Titanium oxide：" Ti-Pure R-103 ", DuPont systems
Embodiment 1
The acetate fiber promotor composition shown in table 1 is manufactured.
(the 1st operation：A1 operations)
In the high-speed mixer capacity 50L of tank diameter (the super mixer of Kawata systems " SWV-50 ") shown in addition table 1
The cellulose acetate of (A) composition, stabilizer 1 and stabilizer 3, with 510r/min stir within 1 minute.
Thereafter, while being stirred using high-speed mixer, using spray head, (B) composition of supply in 5 minutes is spent
Glycerol triacetate partial amount (15 mass parts) and stabilizer 2.It should be noted that the glycerol triacetate of (B) composition
The material being pre-mixed is used with stabilizer 2.
Thereafter, stop stirring, placed about 30 minutes for (20~25 DEG C) in room temperature.As a result, the temperature inside mixture reaches
To 40 DEG C~less than 35 DEG C.
Thereafter, carried out stirring for 15 seconds.
(the 1st operation：A2 operations)
Thereafter, while being stirred using high-speed mixer, the second of glycerine three of (B) composition is with the addition of using spray head
The surplus (15 mass parts) of acid esters.
(B) after the addition of the glycerol triacetate of composition terminates, further stirring 15 seconds, have obtained composition (middle
Composition).Above-mentioned composition (intermediate composition) is the material of dry and comfortable powdery, is also held from the taking-up operation of high-speed mixer
Easily.
It should be noted that (A) composition is 15L (about 6kg) with the total capacity of (B) composition.
(the 2nd operation)
Then, the composition taken out from high-speed mixer is supplied to the main feeder of extruder, be extruded as strand shape it
Afterwards, cooled down, cut, manufactured pellet (pellet of acetate fiber promotor composition).
(extrusion molding condition)
Extruder：TEX30 α (L/D=42) (totally 12 barrel)
Discharge-amount (Q)：15kg/h
Rotating speed (Ns)：200r/min
Barrel temperature：200-180℃
Die head temperature：250℃
Embodiment 2,3
The acetate fiber promotor composition shown in table 1 is manufactured.
(the 1st operation：A1 operations)
In the high-speed mixer capacity 50L of tank diameter (the super mixer of Kawata systems " SWV-50 ") shown in addition table 1
The cellulose acetate of (A) composition, stabilizer 1 and stabilizer 3, with 510r/min stir within 1 minute.
Thereafter, while being stirred using high-speed mixer, using spray head, (B) composition of supply in 5 minutes is spent
Glycerol triacetate partial amount (embodiment 2,3 is 15 mass parts) and stabilizer 2.It should be noted that (B) composition
Glycerol triacetate and stabilizer 2 use the material being pre-mixed.
Thereafter, stop stirring, placed about 30 minutes for (20~25 DEG C) in room temperature.As a result, the temperature inside mixture reaches
To 40 DEG C~less than 35 DEG C.
Thereafter, carried out stirring for 15 seconds.
(the 1st operation：A2 operations)
Thereafter, while being stirred using high-speed mixer, (B) composition is with the addition of within 5 minutes using spray head, cost
Glycerol triacetate surplus (embodiment 2 be 10 mass parts, embodiment 3 be 15 mass parts).
(the 1st operation：A3 operations)
Thereafter, while being stirred using high-speed mixer, (B) composition is with the addition of within 5 minutes using spray head, cost
Glycerol triacetate surplus (embodiment 2,3 is 10 mass parts).
(B) after the addition of the glycerol triacetate of composition terminates, further stirring 15 seconds, have obtained composition (middle
Composition).Above-mentioned composition (intermediate composition) is the material of dry and comfortable powdery, is also held from the taking-up operation of high-speed mixer
Easily.
(the 2nd operation)
Then, the composition taken out from high-speed mixer is supplied similarly to Example 1 to the hopper of extruder, extrusion
After for strand shape, cooled down, cut, manufactured pellet (pellet of acetate fiber promotor composition).
Comparative example 1,2
The acetate fiber promotor composition shown in table 1 is manufactured.
(the 1st operation：A1 operations)
In (A) composition shown in the interior addition table 1 of high-speed mixer (the super mixer of Kawata systems, " SWV-50 " 50L)
Cellulose acetate, stabilizer 1 and stabilizer 3, with 510r/min stir within 1 minute.
Thereafter, while being stirred using high-speed mixer, using spray head, (B) composition of supply in 5 minutes is spent
Glycerol triacetate whole amount and stabilizer 2.It should be noted that the glycerol triacetate and stabilizer 2 of (B) composition make
It is the material being pre-mixed.
Thereafter, stop stirring, placed about 30 minutes for (20~25 DEG C) in room temperature.As a result, the temperature inside mixture reaches
To 40 DEG C~less than 35 DEG C.
Thereafter, carry out stirring for 15 seconds, obtained the composition (intermediate composition) for comparing.Above-mentioned composition (middle groups
Compound) integrally become bulk.
In addition, desire supplies the composition taken out from high-speed mixer in the same manner as embodiment 1~3 to the hopper of extruder
(main feeder), but the solid of bulk hung on the hopper of extruder, in failing to put into extruder.
(fraction defective)
In embodiment 1~3, comparative example 1,2, intermediate composition will add obtained from high-speed mixer is stirred
Enter the sieve of mesh 4mm, vibration in 5 minutes is applied with to sieve with hand.Obtain to the last not yet by sieve intermediate composition it is residual
The ratio (quality %) of amount, as fraction defective.
[table 1]
The intermediate composition of embodiment 1~3 is dry and comfortable powdery state, therefore, the extrusion molding based on extruder thereafter
Also it is easy.
The intermediate composition of comparative example 1,2 is block, therefore, in order to carry out extrusion molding using extruder, it is necessary to be based on
The comminution process of pulverizer.Further, after being pulverized, become the mixture of various larger blocks, one part is carried out
Efflorescence.
Embodiment 4~7
(the 1st operation：A1 operations)
The 1st operation (a1 operations) is implemented in the same manner as embodiment 1~3 using the composition shown in table 2, is combined
Thing (intermediate composition).
In the 1st operation, the amount of less than half of whole additions of (B) composition is only with the addition of, therefore composition is (middle
Composition) be dry and comfortable powdery material, the taking-up operation from high-speed mixer is also easy.
(the 2nd operation)
The composition obtained in 1st operation is supplied to the main feeder of extruder, be extruded as after strand shape, carried out cold
But, cut, manufactured pellet (pellet of acetate fiber promotor composition).It should be noted that in the 2nd operation, from the 6th barrel
With the addition of (B) composition of surplus.
(extrusion molding condition)
Extruder：TEX30 α (L/D=42) (totally 12 barrel)
Discharge-amount (Q)：15kg/h
Rotating speed (Ns)：200r/min
Barrel temperature：200-180℃
Die head temperature：250℃
Comparative example 3
The whole compositions shown in hopper (main feeder) supply schedule 2 from direct extruder are attempted and have been extruded into
Type, but cellulose acetate fails equably to mix with plasticizer, and thermoplasticity is not enough, becomes bulk.Therefore, fail from extruder
Extrusion.
The pellet of the composition of embodiment 4~7 is supplied to injection moulding machine, ISO multipurpose test films are molded
After shaping, for each evaluation test.
(injection moulding condition)
Temperature cylinder：220℃
Mold temperature：50℃
(stretching norminal strain)
Stretching norminal strain (the tensile strength unit of test film based on ISO527, with the velocity determination of 50mm/min:
MPa, stretching norminal strain unit:%).
(modulus of elasticity in static bending)
(unit is determined based on ISO178:MPa).
(Charpy impact intensity)
Charpy impact intensity (kJ/m is determined based on ISO179/1eA2) (unit:KJ/m2)。
[table 2]
The intermediate composition of embodiment 4~7 is due to being dry and comfortable powdery state, thus being extruded into based on extruder thereafter
Type is also easy.Comparative example 3 fails to carry out extrusion molding.
In addition, the engineering properties of injection-molded article is also good, and plasticizer has measured increase, therefore flexibility
Height, such as when the material to being shaped to tubulose is contacted with finger, there is soft and comfortable thoughts and feelings.
Industrial applicibility
It is high, resistance to that the composition obtained using the manufacture method of acetate fiber promotor composition of the invention can obtain flexibility
The good products formed of impact.
Therefore, above-mentioned composition acts not only as OA/ home appliances field, electrical/electronic field, communication apparatus neck
The parts in the house association areas such as the field of transport vehicles such as domain, health field, automobile, furniture/building materials, groceries field etc. and outer
Cover to use, apply also for the purposes for directly being contacted with people.
Claims (8)
1. the manufacture method of acetate fiber promotor composition, it includes：
Relative to the mass parts of (A) cellulose acetate 100, aromatic ring and 200~450g/mol of molecular weight are not included in addition (B) molecule
The mass parts of plasticizer 20 more than, and mixed,
Wherein,
The total capacity of (A) composition and (B) composition is more than 10L,
Relative to (A) composition, whole additions of (B) composition are added mixing several times by described in.
2. the manufacture method of acetate fiber promotor composition, it includes：
Relative to the mass parts of (A) cellulose acetate 100, aromatic ring and 200~450g/mol of molecular weight are not included in addition (B) molecule
The mass parts of plasticizer 20 more than, and mixed,
Wherein,
The total capacity of (A) composition and (B) composition is more than 10L,
The manufacture method has：
Relative to (A) composition, whole additions of (B) composition by described in add mixed into mixer several times
1 operation and
The composition obtained in the 1st operation is supplied to extruder the 2nd operation for carrying out extrusion molding,
In the 1st operation, there is refrigerating work procedure between multiple addition mixed processes.
3. the manufacture method of acetate fiber promotor composition, it includes：
Relative to the mass parts of (A) cellulose acetate 100, aromatic ring and 200~450g/mol of molecular weight are not included in addition (B) molecule
The mass parts of plasticizer 20 more than, and mixed,
Wherein,
The total capacity of (A) composition and (B) composition is more than 10L,
The manufacture method has：
Relative to (A) composition, a part for whole additions of (B) composition 1 time or added several times mixed by described in
The 1st operation that is bonded in mixer and
The composition obtained in the 1st operation is supplied to extruder the 2nd operation for carrying out extrusion molding,
In the 1st operation, there is refrigerating work procedure between multiple addition mixed processes,
In the 2nd operation, (B) composition described in surplus is supplied to extruder.
4. the manufacture method of the acetate fiber promotor composition according to Claims 2 or 3, wherein, the mixer is can
With the high-speed mixer that more than rotating speed 200r/min is mixed.
5. the manufacture method of the acetate fiber promotor composition according to any one of Claims 1 to 4, wherein, (B) into
It is selected from：Glycerol triacetate, triethyl citrate, tributyl 2-acetylcitrate.
6. the manufacture method of the acetate fiber promotor composition according to any one of Claims 1 to 5, wherein, relative to institute
The addition for stating (B) composition of the mass parts of (A) composition 100 is 25~45 mass parts.
7. the manufacture method of products formed, it includes：
Manufactured using the manufacture method any one of claim 1~6 acetate fiber promotor composition operation and
By the operation of the cellulose acetate composition molding.
8. the manufacture method of products formed according to claim 7, wherein, the products formed is selected from：Piece, film, plate, cylinder, rod.
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| JP2015-198141 | 2015-10-06 | ||
| JP2015198141A JP6599197B2 (en) | 2015-10-06 | 2015-10-06 | Method for producing cellulose acetate composition |
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| JP7162366B1 (en) | 2021-07-26 | 2022-10-28 | 株式会社 ネクアス | Cellulose acetate composition and method for producing the same |
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| JP6599197B2 (en) | 2019-10-30 |
| JP2017071671A (en) | 2017-04-13 |
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