CN110054847A - A method of improving PVC thermostabilization and flame retardant property - Google Patents
A method of improving PVC thermostabilization and flame retardant property Download PDFInfo
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- CN110054847A CN110054847A CN201910334012.0A CN201910334012A CN110054847A CN 110054847 A CN110054847 A CN 110054847A CN 201910334012 A CN201910334012 A CN 201910334012A CN 110054847 A CN110054847 A CN 110054847A
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- pvc
- flame retardant
- thermostabilization
- retardant property
- lignin
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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
- C08L27/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
- C08L27/02—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L27/04—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
- C08L27/06—Homopolymers or copolymers of vinyl chloride
-
- 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
- C08K3/38—Boron-containing compounds
- C08K2003/387—Borates
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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
- C08K2201/011—Nanostructured additives
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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
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
Abstract
The invention discloses a kind of methods for improving PVC thermostabilization and flame retardant property with nano boric acid magnesium/lignin composite material, this method comprises the following steps: (1) being that plasticiser carries out hydrophobically modified to nano boric acid magnesium/lignin composite material with dioctyl phthalate (Dioctyl phthalate, abbreviation DOP)；(2) nano boric acid magnesium/lignin composite material of hydrophobically modified is uniformly mixed with PVC powder, carries out plasticizing modification；(3) the modified mixed material mixing in mixer of plasticizing；(4) mixed material obtained mixing is hot-forming, obtains PVC moulding material.For the present invention using nano boric acid magnesium/lignin composite material of fabricated in situ as reinforcing agent, DOP is plasticiser, is remarkably improved the thermal stability and flame retardant property of PVC moulding material.
Description
Technical field
The invention belongs to PVC technical fields, and in particular to a method of improve PVC thermostabilization and flame retardant property.
Background technique
Antifungin nano material has good physical and chemical properties, such as lightweight, high-ductility, wear-resisting, resistance to highly basic, antioxygen
The features such as change, corrosion-resistant, high temperature resistant, good insulating, after carrying out surface modification treatment to it, it can be used as reinforcing agent, antiwear additive etc.
Applied in the functional materials such as magnesium alloy, ceramic matric composite, plastics and oil product.Using antifungin nano material as thermoplastic
The enhancing group timesharing of property high molecular material, can improve the performances such as the mechanical strength, weatherability, fire-retardant, anti-corrosion of basis material.
Lignin is one of big main component of lignified plant three, and content accounts for 15-35%, is only second to cellulose, is certainly
The renewable aryl compound that right boundary uniquely can provide, have can bio-regeneration and degradation, non-toxic resistant, with it is from a wealth of sources,
The various features such as active group is abundant, anti-oxidant, antibiont erosion, thermoplasticity, glass transition.Lignin can be used as macromolecule
Filler, fire retardant, stabilizer for plastics of polymer etc..Lignin is added in thermoplastic resin PVC to its thermal stability and machine
Tool performance has an important influence.
There is presently no relevant documents to be added in PVC nano boric acid magnesium/lignin composite material to enhance its property
The relevant report of energy.This will be the Efficient Development of Liginon Resource using theoretical foundation is provided, and be that lignin and antifungin are one-dimensional
Application of the nano material in terms of PVC material provides reference.
Summary of the invention
The object of the present invention is to provide a kind of methods for improving PVC thermostabilization and flame retardant property, are dredged by the way that plasticiser is added
The modified nano boric acid magnesium/lignin composite material of water is simultaneously plasticized to improve the thermal stability of PVC moulding material and fire-retardant
Performance.
The purpose of the present invention is what is be achieved through the following technical solutions:
A method of improving PVC thermostabilization and flame retardant property, this method comprises the following steps,
(1) hydrophobic, plasticizing is modified: being taken dry reinforcement materials to be added in plasticiser and is carried out hydrophobically modified, then mixes with PVC
After carry out plastication, obtain being plasticized modified mixture；
(2) mixing: the modified mixture of plasticizing being added in mixer and carries out mixing, obtains sheet output, after crushing
To pulverulent mixture material；
(3) hot-forming: pulverulent mixture material being put into vulcanizing press and carries out hot pressing, can be obtained after cooling with excellent
The PVC moulding material of good thermostabilization and anti-flammability.
As a preferred option of the technical scheme, the static heat-stable time of the PVC moulding material be 260-700s, it is maximum weightless
Rate temperature is 300-330 DEG C, oxygen index (OI) 34-41.
As a preferred option of the technical scheme, the reinforcement materials are nano boric acid magnesium/lignin composite wood of fabricated in situ
Material.
As a preferred option of the technical scheme, the lignin is log quality or activation lignin.Log quality be without
Cross the lignin of processing；Activation lignin activates to obtain by different time machinery solid phase reaction, passes through churned mechanically mode
The strand of lignin is interrupted, lignin is activated with this.
As a preferred option of the technical scheme, antifungin and lignin quality in the nano boric acid magnesium/lignin composite material
Than for 1:0.2-1.5.
As a preferred option of the technical scheme, the plasticiser is DOP (i.e. dioctyl phthalate), two fourth of phthalic acid
Any one of ester, stearic acid.
As a preferred option of the technical scheme, the additional amount of reinforcement materials is PVC and reinforcing agent gross mass in the step (1)
5-20%, the additional amount of plasticiser is the 10-30% of PVC and reinforcing agent gross mass.
As a preferred option of the technical scheme, the temperature of the hydrophobically modified is 90-120 DEG C, time 1-3h.
As a preferred option of the technical scheme, the temperature of the plastication is 60-100 DEG C, time 1-3h.
As a preferred option of the technical scheme, the temperature of mixing is 160-190 DEG C in the step (2).
As a preferred option of the technical scheme, 160-200 DEG C of temperature of pressing plate vulcanizer in the step (3), the pressing plate time is
10-30 minutes, pressure 5-10MPa.
Nano boric acid magnesium/lignin composite material mentioned in the present invention can be prepared as follows to obtain:
A kind of preparation method of nano boric acid magnesium/lignin composite material, the preparation method with inorganic magnesium salt, borate,
Log quality or activation lignin are raw material, and antifungin is pressed first in inorganic magnesium salt solution and lignin quality ratio is 1:0.2-
1.5 addition lignin are uniformly mixed, and alkaline solution control pH value is slowly added dropwise, it is coprecipitated that borate solution progress is then added dropwise
Reaction of forming sediment is prepared presoma feed liquid, inorganic magnesium salt, borate molar ratio be n (Mg)/n (B)=0.7-1.2, finally will
Presoma feed liquid, which is put into autoclave, carries out hydro-thermal reaction, can fabricated in situ nano boric acid magnesium/lignin composite material.
It is under certain condition, by design of alloy, to close that in-situ synthesis reaction, which prepares metal-base composites,
Chemical reaction occurs in golden system and generates one or more of high rigidity, the ceramics of high elastic modulus or intermetallic compound enhancing
Body, and reach the process of enhancing matrix purpose.
The invention has the following advantages:
1, of the invention by being added in PVC material using nano boric acid magnesium/lignin composite material as reinforcing agent, with
DOP is plasticiser, improves the thermal stability and flame retardant property of PVC material.
2, lignin captures free radical by the effect of phenolic hydroxyl group and forms the free radical that stable quinone structure prevents high polymer
Reaction makes lignin have inoxidizability and light, thermal stability；Lignin is added in PVC, in a large amount of hydroxyl and PVC
Cl is crosslinked, and in addition to enhancing polymer thermostable, also has fire retardation.
3, activation lignin can be used in the present invention, and lignin passes through the mechanical activation modification of certain time, can have
Effect improves the content of phenolic hydroxyl groups and reactivity of lignin, improves its own thermal stability and its compatibility with PVC.
4, the present invention can form collaboration between the two and make simultaneously using lignin and antifungin nano material as enhancing component
With effect, the performances such as the mechanical strength, heat resistance, fire-retardant, anti-corrosion of PVC matrix material are significantly improved.
Detailed description of the invention
Congo red method heat stability testing equipment in Fig. 1 material properties test of the present invention.
Appended drawing reference: 1 plug, 2 glass tubes, 3 test tubes, 4 Congored test papers, 5 heat insulation layers, 6 oil baths, 7 samples.
Specific embodiment
In order to make those skilled in the art better understand the technical solution in the application, come below in conjunction with embodiment
Technical solution of the present invention is clearly and completely described, it is clear that described embodiment is only a part of the application
Embodiment, based on the embodiment in the application, those of ordinary skill in the art are obtained without making creative work
The every other embodiment obtained, shall fall within the protection scope of the present application.
Embodiment 1
A method of improving PVC thermostabilization and flame retardant property, this method comprises the following steps,
(1) hydrophobic, plasticizing is modified: taking dry nano boric acid magnesium/lignin composite material (antifungin and protolignin's quality
For amount than being 1:0.5, activation lignin machinery solid phase reaction activation time is 0.5h) it is used as reinforcement materials, reinforcing agent additive amount
Be the 20% of PVC and reinforcing agent gross mass, 20% DOP of PVC and reinforcing agent gross mass be added, in 100 DEG C of baking oven into
Row hydrophobically modified 2h, then progress plastication 2h in 60 DEG C of baking oven is mixed in PVC, it obtains being plasticized modified mixture；
(2) mixing: mixer temperature setting is 165 DEG C, will be plasticized modified mixture and is added in mixer, in 10rpm
Revolving speed under mixing 10min, obtain sheet output, pulverulent mixture material obtained after crushing using high speed disintegrator；
(3) hot-forming: cleaning template pours into pulverulent mixture material in mold, is put into compression molding after pre- thermal softening
Machine, hot pressing temperature are 180 DEG C, and hot pressing time is 15 minutes, pressure 7MPa, carry out pressing plate, take out after cooling, tool can be obtained
There is the PVC moulding material of excellent thermostabilization and anti-flammability.
Embodiment 2
A method of improving PVC thermostabilization and flame retardant property, this method comprises the following steps,
(1) hydrophobic, plasticizing is modified: taking dry nano boric acid magnesium/lignin composite material (antifungin and activation quality matter
For amount than being 1:0.2, activation lignin machinery solid phase reaction activation time is 1.0h) it is used as reinforcement materials, reinforcing agent additive amount
Be the 5% of PVC and reinforcing agent gross mass, 10% stearic acid of PVC and reinforcing agent gross mass be added, in 90 DEG C of baking oven into
Row hydrophobically modified 1.h, then progress plastication 1h in 100 DEG C of baking oven is mixed in PVC, it obtains being plasticized modified mixture；
(2) mixing: mixer temperature setting is 160 DEG C, will be plasticized modified mixture and is added in mixer, in 10rpm
Revolving speed under mixing 10min, obtain sheet output, pulverulent mixture material obtained after crushing using high speed disintegrator；
(3) hot-forming: cleaning template pours into pulverulent mixture material in mold, is put into compression molding after pre- thermal softening
Machine, hot pressing temperature are 160 DEG C, and hot pressing time is 10 minutes, pressure 5MPa, carry out pressing plate, take out after cooling, tool can be obtained
There is the PVC moulding material of excellent thermostabilization and anti-flammability.
Embodiment 3
A method of improving PVC thermostabilization and flame retardant property, this method comprises the following steps,
(1) hydrophobic, plasticizing is modified: taking dry nano boric acid magnesium/lignin composite material (antifungin and activation quality matter
For amount than being 1:1.5, activation lignin machinery solid phase reaction activation time is 1.5h) it is used as reinforcement materials, reinforcing agent additive amount
It is the 10% of PVC and reinforcing agent gross mass, the 30% neck dibatyl phithalate of PVC and reinforcing agent gross mass is added, in 90-
Hydrophobically modified 3.h is carried out in 120 DEG C of baking oven, then is mixed in progress plastication 3h in 90 DEG C of baking oven with PVC, is plasticized
Modified mixture；
(2) mixing: mixer temperature setting is 190 DEG C, will be plasticized modified mixture and is added in mixer, in 10rpm
Revolving speed under mixing 10min, obtain sheet output, pulverulent mixture material obtained after crushing using high speed disintegrator；
(3) hot-forming: cleaning template pours into pulverulent mixture material in mold, is put into compression molding after pre- thermal softening
Machine, hot pressing temperature are 200 DEG C, and hot pressing time is 30 minutes, pressure 10MPa, carry out pressing plate, take out, can be obtained after cooling
PVC moulding material with excellent thermostabilization and anti-flammability.
Embodiment 4
A method of improving PVC thermostabilization and flame retardant property, this method comprises the following steps,
(1) hydrophobic, plasticizing is modified: taking dry nano boric acid magnesium/lignin composite material (antifungin and activation lignin
Mass ratio is 1:1.2, and activation lignin machinery solid phase reaction activation time is 2.5h) it is used as reinforcement materials, reinforcing agent addition
Amount is the 15% of PVC and reinforcing agent gross mass, 25% DOP of PVC and reinforcing agent gross mass is added, in 90-120 DEG C of baking oven
Middle progress hydrophobically modified 1.5.h, then progress plastication 1.5h in 80 DEG C of baking oven is mixed in PVC, it is modified mixed to obtain plasticizing
Close material；
(2) mixing: mixer temperature setting is 175 DEG C, will be plasticized modified mixture and is added in mixer, in 10rpm
Revolving speed under mixing 10min, obtain sheet output, pulverulent mixture material obtained after crushing using high speed disintegrator；
(3) hot-forming: cleaning template pours into pulverulent mixture material in mold, is put into compression molding after pre- thermal softening
Machine, hot pressing temperature are 190 DEG C, and hot pressing time is 25 minutes, pressure 9MPa, carry out pressing plate, take out after cooling, tool can be obtained
There is the PVC moulding material of excellent thermostabilization and anti-flammability.
Comparative example
The preparation method of the present embodiment and the difference of embodiment 1 are: not adding reinforcing agent and plasticiser, be prepared pure
PVC moulding material.
The thermal stability and flame retardant property index test of PVC material of the present invention.
Heat stability testing method:
(1) static heat stability is measured using congo red method.Test process is executed referring to GB/T 2917.1-2002, i.e. sample
Product heat releasing hydrogen chloride at a certain temperature and Congored test paper are made to become blue, and record is put into sample, and to making, test paper change is blue to be taken
Between, the time is longer, and thermal stability is better.10 mesh (2.0mm) and 14 mesh (1.4mm) are smashed it through with pulverizer before sample test
Sieve, takes intermediate trapped substance to be measured.Test equipment is as shown in Figure 1,180 DEG C of measuring temperature.
(2) dynamic thermal stability analysis uses thermogravimetry.14 mesh are taken to carry out TG measurement with lower plate broken material 5-10mg.
Measuring temperature range is 30-600 DEG C, 10 DEG C/min of heating rate, nitrogen protection.By TG-DTG curve observation sample weightlessness and
Weight-loss ratio process, weightless slower, maximum weight-loss ratio temperature is higher, then thermal stability is better.
(3) flame retardant property test method: oxygen index (OI) (OI) test, GB/T2406-1993 is executed according to national standards, preparation
Sample batten having a size of 80.0 × 10.0 × 4.0mm is tested, and oxygen index (OI) more high flame resistance is better.Smoke density test,
By observing the smog release conditions of sample combustion process, smog is better more bright flame retardant effect of saving your breath.
Table 1
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Comparative example | |
| Static heat-stable time/s | 700 | 260 | 468 | 667 | 147 |
| Maximum weight-loss ratio temperature/DEG C | 330 | 300 | 315 | 320 | 289 |
| Oxygen index (OI) | 41 | 34 | 38 | 40 | 30 |
Upper table is the contrast table that the material that each embodiment is prepared carries out thermal stability and anti-flammability test, can by upper table
Know: thermal stability result: pure PVC moulding material, static heat-stable time is 147 seconds, maximum weight-loss ratio temperature is 289 DEG C, is added
The static heat-stable time for entering PVC moulding material after nano boric acid magnesium/lignin composite material reinforcing agent is 260-700s, maximum
Weight-loss ratio temperature is 300-330 DEG C.
Flame resistance effect: pure PVC moulding material, oxygen index (OI) 30, smog burst size is big, addition nano boric acid magnesium/wooden
The oxygen index (OI) of PVC moulding material is 34-41 after plain composite reinforcement, and smog burst size substantially reduces.
The present invention is pungent with two by being added in PVC material using nano boric acid magnesium/lignin composite material as reinforcing agent
Rouge DOP is plasticiser, can significantly improve the thermal stability and flame retardant property of PVC material.
Claims (10)
1. a kind of method for improving PVC thermostabilization and flame retardant property, it is characterised in that: this method comprises the following steps,
(1) hydrophobic, plasticizing is modified: being taken dry reinforcement materials to be added in plasticiser and is carried out hydrophobically modified, then after mixing with PVC
Plastication is carried out, obtains being plasticized modified mixture；
(2) mixing: the modified mixture of plasticizing is added in mixer and carries out mixing, sheet output is obtained, obtains powder after crushing
Shape mixed material；
(3) hot-forming: pulverulent mixture material being put into vulcanizing press and carries out hot pressing, can be obtained after cooling with thermostabilization
With the PVC moulding material of anti-flammability.
2. the method according to claim 1 for improving PVC thermostabilization and flame retardant property, it is characterised in that: the PVC molding
The static heat-stable time of material is 260-700s, maximum weight-loss ratio temperature is 300-330 DEG C, oxygen index (OI) 34-41.
3. the method according to claim 1 for improving PVC thermostabilization and flame retardant property, it is characterised in that: the reinforcing agent
Material is nano boric acid magnesium/lignin composite material of fabricated in situ；The lignin is log quality or activation lignin.
4. the method according to claim 3 for improving PVC thermostabilization and flame retardant property, it is characterised in that: nano boric acid magnesium/
Nano boric acid magnesium and lignin quality ratio are 1:0.2-1.5 in lignin composite material.
5. the method according to claim 1 for improving PVC thermostabilization and flame retardant property, it is characterised in that: the plasticiser
For any one of dioctyl phthalate, dibutyl phthalate, stearic acid.
6. the method for -5 any improvement the PVC thermostabilizations and flame retardant property according to claim 1, it is characterised in that: described
The additional amount of reinforcement materials is the 5-20% of PVC and reinforcing agent gross mass in step (1), the additional amount of plasticiser be PVC and
The 10-30% of reinforcing agent gross mass.
7. the method according to claim 6 for improving PVC thermostabilization and flame retardant property, it is characterised in that: described hydrophobic to change
Property temperature be 90-120 DEG C, time 1-3h.
8. the method according to claim 6 for improving PVC thermostabilization and flame retardant property, it is characterised in that: the plasticizing is anti-
The temperature answered is 60-100 DEG C, time 1-3h.
9. the method according to claim 1 for improving PVC thermostabilization and flame retardant property, it is characterised in that: the step (2)
The temperature of middle mixing is 160-190 DEG C.
10. the method according to claim 1 for improving PVC thermostabilization and flame retardant property, it is characterised in that: the step
(3) 160-200 DEG C of the temperature of pressing plate vulcanizer in, pressing plate time are 10-30 minutes, and pressure is 5-10 MPa.
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