CN109593269A - Low melting point powder auxiliary agent master batch of high concentration and preparation method thereof - Google Patents
Low melting point powder auxiliary agent master batch of high concentration and preparation method thereof Download PDFInfo
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- CN109593269A CN109593269A CN201811396838.1A CN201811396838A CN109593269A CN 109593269 A CN109593269 A CN 109593269A CN 201811396838 A CN201811396838 A CN 201811396838A CN 109593269 A CN109593269 A CN 109593269A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
- C08J3/226—Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/10—Homopolymers or copolymers of propene
- C08J2323/12—Polypropene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2483/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2483/04—Polysiloxanes
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
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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
- C08K5/13—Phenols; Phenolates
- C08K5/132—Phenols containing keto groups, e.g. benzophenones
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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
- C08K5/36—Sulfur-, selenium-, or tellurium-containing compounds
- C08K5/37—Thiols
- C08K5/372—Sulfides, e.g. R-(S)x-R'
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- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)
Abstract
The invention discloses low melting point powder auxiliary agent master batches of a kind of high concentration and preparation method thereof, by adjusting factory formula, add silicone oil as dispersing agent in formula and powder stuffing talcum powder is uniformly adhered on acrylic resin surface；By adjusting production technology, so that powder auxiliary agent claims to carry out accurate discharge separately through weight-loss metering, avoiding it causes to melt during mixed at high speed because fusing point is lower in high-speed mixer, and then make material stick to each other together, it is unstable etc. to which main spout returning charge, vacuum returning charge and blanking occur, the auxiliary agent master batch of final obtained high concentration.It is demonstrated experimentally that high concentration auxiliary agent master batch stable production process prepared by the present invention is without exception, and for not only improving produced on-site operation when modified plastics production, reduce worker's amount of labour, while improving modified plastics stability of the production process.
Description
Technical field
The present invention relates to a kind of high concentration auxiliary agent master batch and preparation method thereof more particularly to a kind of low melting point powder of high concentration
Body auxiliary agent master batch and preparation method thereof belongs to high molecular material and its forming processing technology field.
Background technique
In modified plastic industry, often there is the case where a large amount of dust is flown upward in production scene, wherein causing dust from flying
Factor first is that because used raw material be powder mostly, especially be substantially powder shaped using auxiliary agent.For solution
Certainly above-mentioned technical problem has technical staff to propose powder auxiliary agent being first prepared into auxiliary agent master batch, is then then added to and needs to be modified
Plastics system in technical solution.The preparation of common auxiliary agent master batch be using resin as matrix, using powder shaped auxiliary agent as major ingredient,
Direct feeding shearing, is squeezed out to extruder, plasticizing heated by extruder after high-speed mixer mixes, and finally makes powder shaped
Auxiliary agent and resin sufficiently combine in physical aspect, thus manufactured nutty structure body.
However either directly powder auxiliary agent is added in resin system in the preparation process of auxiliary agent master batch and is made
It is standby, when the low melting point powder auxiliary agent that used powder auxiliary agent is fusing point lower (generally be lower than 100 DEG C), and the low melting point powder
When the content of body auxiliary agent is higher, according to conventional production technology, can generate following problems: (1) low melting point powder auxiliary agent is molten
It when building pressure after melting inside barrel, easily returns to be not easy to be transported away at feed opening, to cause the feelings of feed opening returning charge
Condition；(2) since the fusing point of powder auxiliary agent is lower, the auxiliary agent after melting will affect the plasticizing of thermoplastic resin, to cause
Vacuum returning charge；(3) low melting point auxiliary agent is easy agglomeration inside high-speed mixer, to will cause unstable in blanking process.
Summary of the invention
In order to solve the above technical problems, the present invention provides a kind of low melting point powder auxiliary agent master batch of high concentration and its preparations
Method, the preparation method simple process and production are stablized, and powder auxiliary agent content is higher in preparation gained auxiliary agent master batch, particularly suitable
In the production of low melting point powder auxiliary agent master batch.
The technical scheme is that
The invention discloses a kind of preparation methods of the low melting point powder auxiliary agent master batch of high concentration, under which includes
State step:
(1) start the high-speed mixer after putting into resin matrix in high-speed mixer to turn with the speed of 400-900r/min
It is dynamic, continue after then putting into silicone oil with speed mixed at high speed 5-25s；Then it is subsequent that powder stuffing is put into high-speed mixer
The continuous speed mixed at high speed 5-25s with 400-900r/min, obtains mixed material；
(2) claim feeding to the master of double screw extruder by the first weight-loss metering the mixed material in high-speed mixer
Spout is claimed by the second weight-loss metering by the side of the lateral feeding of low melting point powder auxiliary agent to double-screw extruding machine barrel middle section
At spout, the mixed material and low melting point powder auxiliary agent obtain height after double screw extruder carries out melt blending granulation
The low melting point powder auxiliary agent master batch of concentration.
In above-mentioned preparation method:
The dosage of the resin matrix is 30-100 parts by weight, preferably 40-100 parts by weight；The dosage of the powder stuffing
For 0-30 parts by weight, preferably 0-20 parts by weight；The dosage of the low melting point powder auxiliary agent is 40-60 parts by weight；The silicone oil
Dosage is the 0.01-2.0wt.%, preferably 0.1- of resin matrix, powder stuffing and low melting point powder auxiliary agent total weight
1.0wt.%.
Used resin matrix is the thermoplastic resin of this field routine, can according to the use environment of auxiliary agent master batch into
Row adjustment, if the auxiliary agent master batch needs to be added into acrylic resin system, then resin matrix can be selected as acrylic resin；Such as
The auxiliary agent master batch needs to be added into polycarbonate resin resin system, then polycarbonate resin can be selected in resin matrix, etc..The application
Middle resin matrix selects acrylic resin, and melt flow rate (MFR) of acrylic resin under the conditions of 230 DEG C/2.16kg is 1-
The acrylic resin that melt flow rate (MFR) under the conditions of 100g/10min, preferably 230 DEG C/2.16kg is 20-80g/10min.
Used silicone oil is methyl-silicone oil, ethyl silicon oil, phenyl silicone oil, Methyl Hydrogen Polysiloxane Fluid, methyl phenyl silicone oil, first
Base chlorphenyl silicone oil, MethylethoxylsiliconFluid Fluid, methyl trifluoro propyl silicone oil, methyl vinyl silicon oil, methylhydroxy silicone oil, ethyl
Containing hydrogen silicone oil, hydroxyl hydrogen silicone oil and at least one of containing nitrile silicone.Silicone oil is used as dispersing agent to exist in this application, adds
Being added in the resin system containing powder facilitates dispersing uniformity of the powder in resin.
Used powder stuffing can decide whether to carry out in auxiliary agent master batch according to the performance requirement of compound resin
Addition, can not add the powder stuffing when not needed.Powder stuffing used in general is powder stuffing commonly used in the art
Such as talcum powder, calcium carbonate, mica powder, titanium dioxide, barium sulfate, one of preferably talc powder and barium sulfate in the application.
Used low melting point powder auxiliary agent is the powder auxiliary agent that melting temperature is not higher than 100 DEG C, which needs
Meet fusing point not higher than 100 DEG C and in powder state two requirements, auxiliary agent type can be various powder commonly used in the art
Body auxiliary agent, such as antioxidant, light stabilizer, heat stabilizer, ultraviolet absorbing agent.Low melting point powder auxiliary agent includes molten in the application
One of antioxidant of the point temperature not higher than 100 DEG C and ultraviolet absorbing agent.
In above-mentioned preparation method:
The rate of feeding of first and second weight-loss metering is referred to as 400-1000kg/h, and first and second weight-loss metering
The ratio between rate of feeding be referred to as mixed material and low melting point powder auxiliary agent the ratio between dosage；Furthermore the first and second weight-loss type meter
The feeding dynamic accuracy of amount is referred to as 4-5 ‰, and preferably feeding dynamic accuracy is 5 ‰.First and second weight-loss metering described herein
Claim that Bradley sheet is selected to reach weighing balance.
In above-mentioned preparation method:
The side spout of the double screw extruder is opened at Section four, Section five or Section six of barrel, the application
In the preferably side spout be opened at Section five of barrel.
The draw ratio of the double screw extruder be (36-56): 1, preferably draw ratio be 40:1 double screw extruder, and
The screw speed of the double screw extruder is 300-1100rpm.
The invention also discloses a kind of low melting point powder auxiliary agent master batch of high concentration prepared by the preparation method,
The auxiliary agent master batch includes the following each components calculated by weight: resin matrix 30-100 parts by weight, preferably 40-100 parts by weight；
Powder stuffing 0-30 parts by weight, preferably 0-20 parts by weight；Low melting point powder auxiliary agent 40-60 parts by weight；Silicone oil is resin matrix, powder
0.01-2.0wt.%, the preferably 0.1-1.0wt.% of body filler and low melting point powder auxiliary agent total weight, wherein resin matrix, powder
The selection of body filler, low melting point powder auxiliary agent and silicone oil is as described in preceding preparation method.
The method have the benefit that: technical scheme adds silicon by adjusting factory formula in formula
Oil is uniformly adhered powder stuffing talcum powder on acrylic resin surface as dispersing agent；By adjusting production technology, make
It obtains powder auxiliary agent to claim to carry out accurate discharge separately through weight-loss metering, avoids it and led in high-speed mixer because fusing point is lower
Cause melts during mixed at high speed, and then makes material stick to each other together, so that main spout returning charge occurs, vacuum is returned
Material and blanking are unstable etc., the auxiliary agent master batch of final obtained high concentration.It is demonstrated experimentally that high concentration auxiliary agent prepared by the present invention is female
Grain stable production process is without exception, and for not only improving produced on-site operation when modified plastics production, reduces worker's labor
Momentum, while improving modified plastics stability of the production process.
Specific embodiment
In order to better understand the technical means of the present invention, it and can be implemented in accordance with the contents of the specification, below
In conjunction with specific embodiments, specific embodiments of the present invention will be described in further detail, and following embodiment is for illustrating this hair
It is bright, but be not intended to limit the scope of the invention.
Resin matrix selected by following specific embodiments and comparative example, powder stuffing, silicone oil and low melting point powder auxiliary agent
As described below, but it is merely to illustrate the present invention, is not intended to restrict the invention technical solution.
Resin matrix: melt flow rate (MFR) is the acrylic resin of 33g/10min under 230 DEG C/2.16kg.
Powder stuffing: talcum powder.
Silicone oil: methyl-silicone oil and MethylethoxylsiliconFluid Fluid are obtained by mixing according to mass ratio 1:1.
Powder auxiliary agent: antioxidant THANOX 412S, fusing point is 48-54 DEG C, white powdered；
Ultraviolet absorbent UV-531, fusing point are 48-49 DEG C, light yellow or white crystalline powder.
First and second weight-loss metering used in following specific embodiments claims to be that Bradley sheet reaches weighing balance, feeding
Speed is 400-1000kg/h, can choose the Bradley sheet that rate of feeding is 400-500kg/h and 800-1000kg/h and reaches metering
Claim, feeding dynamic accuracy is 5 ‰.Selected double screw extruder model TSE-75 is filled by Nanjing Rhea high polymer
Standby Co., Ltd produces, draw ratio 40:1, and screw speed is 300-1100rpm.
Carry out the preparation of specific embodiment and comparative example auxiliary agent master batch respectively according to formula and preparation method described in table 1:
Preparation method I:
(1) start the high-speed mixer after putting into resin matrix in high-speed mixer to turn with the speed of 400-900r/min
It is dynamic, continue after then putting into silicone oil with speed mixed at high speed 5-25s；Then it is subsequent that powder stuffing is put into high-speed mixer
The continuous speed mixed at high speed 5-25s with 400-900r/min, obtains mixed material；
(2) claim feeding to the master of double screw extruder by the first weight-loss metering the mixed material in high-speed mixer
Spout is claimed using the second weight-loss metering by the lateral feeding of low melting point powder auxiliary agent to Section of five barrel of double screw extruder
Place, the mixed material and low melting point powder auxiliary agent obtain high concentration after double screw extruder carries out melt blending granulation
Low melting point powder auxiliary agent master batch, wherein the ratio between the rate of feeding of the first and second weight-loss metering is referred to as mixed material and low melting point powder
The ratio between the dosage of body auxiliary agent.
Preparation method II:
(1) resin matrix is put into after high-speed mixer and starts the high-speed mixer with the speed of 400-900r/min turn
It is dynamic, continue after then putting into silicone oil with speed mixed at high speed 5-25s；Then it is subsequent that powder stuffing is put into high-speed mixer
The continuous speed mixed at high speed 5-25s with 400-900r/min；After finally putting into low melting point powder auxiliary agent into high-speed mixer again
Continue to obtain mixture with the speed mixed at high speed 5-25s of 400-900r/min.
(2) high-speed mixer is directly used to carry out feeding, warp to the main spout of double screw extruder the mixed material
Double screw extruder melt blending obtains low melting point powder auxiliary agent master batch after being granulated.
1 specific embodiment of table and comparative formulation composition (unit: parts by weight)
In the preparation process of above-mentioned specific embodiment and comparative example, to monitor whether stable blanking, powder auxiliary agent and tree
Whether the mixing between aliphatic radical body is stable, is measured using the method for monitoring master batch melt index, specific practice are as follows: every two is small
When sampling master batch and melt index determination is carried out to it and records measurement result, used test equipment is melt flow rate (MFR)
Tester, DMF-003, German Zwick/Roell group, and test condition are 230 DEG C/2.16kg.Measurement result is referring to 2 institute of table
Show.
Furthermore the phenomenon that whether will appear agglomeration in high-speed mixer is observed when carrying out mixed at high speed；Carry out blanking and
When melting extrusion, the case where whether double screw extruder will appear feed opening returning charge and vacuum returning charge is observed, result is recorded in
In table 2, it is recorded as "×" when there is above-mentioned unfavorable condition, " √ " is recorded as when not occurring above-mentioned unfavorable condition.
2 specific embodiment of table and comparative example the performance test results
Test result can be seen that technical scheme by adjusting factory formula from above-mentioned table 2, add in formula
Silicone oil is added as dispersing agent powder stuffing talcum powder to be uniformly adhered on acrylic resin surface；By adjusting production work
Skill so that powder auxiliary agent separately through weight-loss metering claim carry out accurate discharge and use lateral feeding manner, avoid its
High-speed mixer internal cause fusing point is lower to be caused to melt during mixed at high speed, and then makes material stick to each other together, from
And occur that main spout returning charge, vacuum returning charge and blanking are unstable etc., the auxiliary agent master batch of final obtained high concentration.Experiment card
Bright, high concentration auxiliary agent master batch stable production process prepared by the present invention is without exception, and for not only improving when modified plastics production
Produced on-site operation, reduces worker's amount of labour, while improving modified plastics stability of the production process.
The above is only a preferred embodiment of the present invention, it is not intended to restrict the invention, it is noted that for this skill
For the those of ordinary skill in art field, without departing from the technical principles of the invention, can also make it is several improvement and
Modification, these improvements and modifications also should be regarded as protection scope of the present invention.
Claims (10)
1. a kind of preparation method of the low melting point powder auxiliary agent master batch of high concentration, it is characterised in that: include the following steps:
(1) start the high-speed mixer after putting into resin matrix in high-speed mixer to rotate with the speed of 400-900r/min,
Then continue after putting into silicone oil with speed mixed at high speed 5-25s；Then continue after putting into powder stuffing into high-speed mixer
With the speed mixed at high speed 5-25s of 400-900r/min, mixed material is obtained；
(2) claim feeding to the main feeding of double screw extruder by the first weight-loss metering the mixed material in high-speed mixer
Mouthful, claimed by the second weight-loss metering by the side feed material of the lateral feeding of low melting point powder auxiliary agent to double-screw extruding machine barrel middle section
At mouthful, the mixed material and low melting point powder auxiliary agent obtain high concentration after double screw extruder carries out melt blending granulation
Low melting point powder auxiliary agent master batch；
Wherein
The low melting point powder auxiliary agent is the powder auxiliary agent that melting temperature is not higher than 100 DEG C；
The dosage of the resin matrix is 30-100 parts by weight, and the dosage of the powder stuffing is 0-30 parts by weight, the eutectic
The dosage of point powder auxiliary agent is 40-60 parts by weight, and the dosage of the silicone oil is resin matrix, powder stuffing and low melting point powder
The 0.01-2.0wt.% of auxiliary agent total weight.
2. the preparation method of auxiliary agent master batch according to claim 1, it is characterised in that: first and second weight-loss metering claims
Rate of feeding be 400-1000kg/h, and the ratio between the rate of feeding of first and second weight-loss metering is referred to as mixed material and low
The ratio between the dosage of fusing point powder auxiliary agent.
3. the preparation method of high concentration master batch according to claim 1, it is characterised in that: first and second weight-loss metering
Feeding dynamic accuracy be referred to as 4-5 ‰.
4. the preparation method of high concentration master batch according to claim 1, it is characterised in that: the side feed of the double screw extruder
Material mouth is opened at Section four, Section five or Section six of barrel.
5. the preparation method of high concentration master batch according to claim 1, it is characterised in that: the resin matrix is polypropylene tree
Rouge, and melt flow rate (MFR) of acrylic resin under the conditions of 230 DEG C/2.16kg is 1-100g/10min.
6. the preparation method of high concentration master batch according to claim 1, it is characterised in that: the silicone oil is methyl-silicone oil, second
Base silicone oil, phenyl silicone oil, Methyl Hydrogen Polysiloxane Fluid, methyl phenyl silicone oil, methylchlorophenyl silicone oil, MethylethoxylsiliconFluid Fluid, methyl
Trifluoro propyl silicone oil, methyl vinyl silicon oil, methylhydroxy silicone oil, ethyl containing hydrogen silicone oil, hydroxyl hydrogen silicone oil and contain nitrile silicone
At least one of.
7. the preparation method of high concentration master batch according to claim 1, it is characterised in that: the powder stuffing be talcum powder and
One of barium sulfate.
8. the preparation method of high concentration master batch according to claim 1, it is characterised in that: the low melting point powder auxiliary agent includes
One of antioxidant of the melting temperature not higher than 100 DEG C and ultraviolet absorbing agent.
9. the preparation method of high concentration master batch according to claim 1, it is characterised in that: the major diameter of the double screw extruder
Than for (36-56): 1, and the screw speed of the double screw extruder is 300-1100rpm.
10. a kind of low melting point powder for the high concentration that the preparation method as described in any claim in claim 1 to 9 is prepared
Body auxiliary agent master batch.
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| CN111251494A (en) * | 2020-01-21 | 2020-06-09 | 天津利安隆新材料股份有限公司 | Preparation method of low-melting-point weather-resistant auxiliary agent master batch |
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Application publication date: 20190409 |