CN107226981A - A kind of preparation method of polyvinyl chloride composite materials - Google Patents
A kind of preparation method of polyvinyl chloride composite materials Download PDFInfo
- Publication number
- CN107226981A CN107226981A CN201710557624.7A CN201710557624A CN107226981A CN 107226981 A CN107226981 A CN 107226981A CN 201710557624 A CN201710557624 A CN 201710557624A CN 107226981 A CN107226981 A CN 107226981A
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- China
- Prior art keywords
- polyvinyl chloride
- stalk
- preparation
- composite materials
- coupling agent
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Classifications
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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
- 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
- C08L2201/22—Halogen free composition
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
- C08L2205/16—Fibres; Fibrils
Abstract
The invention provides a kind of preparation method of polyvinyl chloride, it is first to carry out nano modification with stalk；Nano modification stalk is subjected to coupling agent surface treatment again, is then added to as fire-retardant filler in the preparation of polyvinyl chloride.The present invention instead of poisonous and hazardous halogenated flame retardant using the nano modification stalk of coupling agent treatment.Because the nano modification stalk of coupling agent treatment is to be dispersed in nano particle state in PVC base system; it can generate oxide and vapor when heat is decomposed; vapor, which waters down, dilutes imflammable gas; and the generation of oxide helps to make flameout; serve the effect for suppressing burning; generate protective layer and be covered in polymer body surface (use of coupling agent makes covering more firm); so as to isolate burning things which may cause a fire disaster and oxygen, therefore composite is set to be provided with good fire resistance.The present invention is effectively utilized agricultural wastes straw simultaneously, it is turned waste into wealth, creates new application value.
Description
Technical field
The invention belongs to technical field of composite materials, more particularly to a kind of preparation method of polyvinyl chloride composite materials.
Background technology
Polyvinyl chloride (PVC) was once the general-purpose plastics of yield maximum in the world, using widely.In construction material, work
Industry product, commodity, flooring laminate, floor tile, artificial leather, tubing, electric wire, packaging film, bottle, expanded material, encapsulant,
It is widely used in terms of fiber.Polyvinyl chloride can discharge hydrogen chloride and other toxic gases in combustion, for example
Dioxin.The burning of polyvinyl chloride is divided into two steps.First go out hydrogen chloride gas and containing double bond in 240 DEG C of -340 DEG C of combustion decompositions
Alkadienes, then occurs the burning of carbon at 400-470 DEG C.Conventional fire retardant is halogenated flame retardant at present, because its is efficient
Flame retardant effect, be widely used in flame-retardant polymer it is material modified in.But, the based flame retardant can discharge substantial amounts of in burning
Poisonous and hazardous gas, the gas such as hydrogen halides, bioxin causes secondary pollution, seriously endangers life security and environment peace
Entirely.
The content of the invention
It is an object of the invention to provide a kind of polyvinyl chloride for not using halogenated flame retardant and having good fire resistance
The preparation method of composite.
The purpose of the present invention can be achieved through the following technical solutions：
A kind of preparation method of polyvinyl chloride composite materials of the present invention, comprises the following steps：
(1) dry stalk is crushed and adds mass fraction in 5-6% sodium hydroxide solution, to soak at 50-60 DEG C
Filtering drying after 10-15h；
(2) stalk after drying is placed in vacuum impregnation in the aluminum salt solution that concentration is 1.0-3.0molL-1, then will
Stalk after vacuum impregnation is at 120-150 DEG C, and the constant temperature 5-10h in hydrothermal reaction kettle is cooled to room temperature, takes out washing, very
Empty drying and crushing obtains a nanometer stalk；
(3) take a nanometer stalk to be placed in alcoholic solvent, add titanate coupling agent, stir 20-30min, filtration drying is obtained
Coupling agent modified nanometer stalk；
(4) 100 parts of polyvinyl chloride, 12-15 parts of lubricants, 10-20 parts of coupling agent modified stalks, 40-50 parts of increasings are weighed
Agent, 1-3 parts of light stabilizers, 1-2 parts of antioxidant are moulded, height in high mixer is added to and mixes 5-6 minutes, take out standby；
(5) step (6) resulting material is added in double screw extruder, in 120-140 DEG C of extruding pelletization.
The preparation method of polyvinyl chloride composite materials described above, wherein step (1) described stalk be maize straw or
Wheat stalk.
The preparation method of polyvinyl chloride composite materials described above, wherein step (2) described aluminum salt solution is aluminum sulfate
Solution, aluminum nitrate solution or liquor alumini chloridi.
The preparation method of polyvinyl chloride composite materials described above, wherein step (2) the vacuum impregnation processing time
For 5-8h, vacuum 0.1MPa.
The preparation method of polyvinyl chloride composite materials described above, step (3) described alcoholic solvent be isopropanol, ethanol or
Methanol.
The preparation method of polyvinyl chloride composite materials described above, the consumption of step (3) described titanate coupling agent is
The 2-5% of nanometer stalk quality.
The preparation method of polyvinyl chloride composite materials described above, the temperature of step (4) described high mixer is 40 DEG C -50
DEG C, rotating speed be 500-800r/min.
The preparation method of polyvinyl chloride composite materials described above, step (4) described lubricant is selected from zinc stearate, second
Support the one or more in bis-stearamides, erucyl amide, polypropylene wax, Tissuemat E, oleamide.
The preparation method of polyvinyl chloride composite materials described above, step (4) described plasticizer is phthalic acid ester
Class；The light stabilizer is hindered amine light stabilizer ZX-70.
The preparation method of polyvinyl chloride composite materials described above, step (4) described antioxidant be antioxidant 1010 with
Irgasfos 168 in mass ratio 1:1 it is compound.
The present invention instead of poisonous and hazardous halogenated flame retardant using by coupling agent modified nanometer stalk, be made fire-retardant
Polyvinyl chloride composite materials, wherein nano modification stalk are to be modified to obtain three by coupling agent coupling again by nano-aluminum hydroxide
The stalk structure of network structure is tieed up, because the nano modification stalk of coupling agent treatment is to be dispersed in polychlorostyrene second with nano particle state
In alkenyl body, it can generate oxide and vapor when heat is decomposed, and vapor, which waters down, dilutes imflammable gas, and aoxidizes
The generation of thing helps to make flameout, serves the effect for suppressing burning, generates protective layer and be covered in polymer body table
Face (use of coupling agent makes covering more firm), so that isolated burning things which may cause a fire disaster and oxygen, therefore it is good to be provided with composite
Fire resistance, according to GB/T2406 standard testings oxygen index (OI) more than 35, fire resistance is good.The present invention is effectively utilized simultaneously
Agricultural wastes straw, makes it turn waste into wealth, and creates new application value.
Embodiment
With reference to specific embodiment, the present invention is described in detail.Following examples agents useful for same is only for example
Protection domain that is bright, being not intended to limit the invention, other embodiments of the invention still elect to all in right
Optional reagent.Unless otherwise instructed, the number is mass parts.
Embodiment 1
(1) dry wheat stalk is crushed and adds mass fraction in 5% sodium hydroxide solution, to soak at 55 DEG C
Filtering drying after 10h；
(2) stalk after drying is placed in vacuum impregnation in the aluminum sulfate solution that concentration is 2.0molL-1 and handles 5h, very
Reciprocal of duty cycle 0.1MPa；Then by the stalk after vacuum impregnation at 150 DEG C, the constant temperature 5h in hydrothermal reaction kettle is cooled to room temperature, taken
Go out washing, nanometer stalk is crushed to obtain in vacuum drying；
(3) take a nanometer stalk to be placed in isopropanol, add titanate coupling agent KR-TTS, stir 30min, cross and be filtered dry
It is dry, obtain coupling agent modified nanometer stalk；The consumption of titanate coupling agent is the 2% of nanometer stalk quality；
(4) 100 parts of polyvinyl chloride, 12 parts of lubricants, 10 parts of coupling agent modified stalks, 50 parts of plasticizer, 1 part of light are weighed
Stabilizer, 1 part of antioxidant, are added to height in high mixer and mix 5-6 minutes, take out standby；
(5) step (6) resulting material is added in double screw extruder, in 120-140 DEG C of extruding pelletization.According to GB/
T2406 standard testings oxygen index (OI) 36, fire resistance is good.
Embodiment 2
(1) dry wheat stalk is crushed and adds mass fraction in 5% sodium hydroxide solution, to soak at 55 DEG C
Filtering drying after 12h；
(2) stalk after drying is placed in vacuum impregnation in the aluminum sulfate solution that concentration is 2.0molL-1 and handles 5h, very
Reciprocal of duty cycle 0.1MPa；Then by the stalk after vacuum impregnation at 150 DEG C, the constant temperature 5h in hydrothermal reaction kettle is cooled to room temperature, taken
Go out washing, nanometer stalk is crushed to obtain in vacuum drying；
(3) take a nanometer stalk to be placed in isopropanol, add titanate coupling agent KR-TTS, stir 30min, cross and be filtered dry
It is dry, obtain coupling agent modified nanometer stalk；The consumption of titanate coupling agent is the 2% of nanometer stalk quality；
(4) 100 parts of polyvinyl chloride, 12 parts of lubricants, 20 parts of coupling agent modified stalks, 50 parts of plasticizer, 1 part of light are weighed
Stabilizer, 1 part of antioxidant, are added to height in high mixer and mix 5-6 minutes, take out standby；
(5) step (6) resulting material is added in double screw extruder, in 120-140 DEG C of extruding pelletization.According to GB/
T2406 standard testings oxygen index (OI) 38, fire resistance is good.
Embodiment 3
(1) dry corn straw smashing is added mass fraction in 5% sodium hydroxide solution, to soak at 55 DEG C
Filtering drying after 15h；
(2) stalk after drying is placed in vacuum impregnation in the aluminum nitrate solution that concentration is 2.0molL-1 and handles 5h, very
Reciprocal of duty cycle 0.1MPa；Then by the stalk after vacuum impregnation at 130 DEG C, the constant temperature 10h in hydrothermal reaction kettle is cooled to room temperature,
Washing is taken out, nanometer stalk is crushed to obtain in vacuum drying；
(3) take a nanometer stalk to be placed in ethanol, add titanate coupling agent KR-TTS, stir 30min, filtration drying,
Obtain coupling agent modified nanometer stalk；The consumption of titanate coupling agent is the 3% of nanometer stalk quality；
(4) 100 parts of polyvinyl chloride, 15 parts of lubricants, 20 parts of coupling agent modified stalks, 50 parts of plasticizer, 3 parts of light are weighed
Stabilizer, 1 part of antioxidant, are added to height in high mixer and mix 5-6 minutes, take out standby；
(5) step (6) resulting material is added in double screw extruder, in 120-140 DEG C of extruding pelletization.According to GB/
T2406 standard testings oxygen index (OI) 39, fire resistance is good.
Embodiment 4
(1) dry wheat stalk is crushed and adds mass fraction in 5% sodium hydroxide solution, to soak at 55 DEG C
Filtering drying after 10h；
(2) stalk after drying is placed in vacuum impregnation in the aluminum sulfate solution that concentration is 2.0molL-1 and handles 8h, very
Reciprocal of duty cycle 0.1MPa；Then by the stalk after vacuum impregnation at 130 DEG C, the constant temperature 8h in hydrothermal reaction kettle is cooled to room temperature, taken
Go out washing, nanometer stalk is crushed to obtain in vacuum drying；
(3) take a nanometer stalk to be placed in isopropanol, add titanate coupling agent KR-TTS, stir 30min, cross and be filtered dry
It is dry, obtain coupling agent modified nanometer stalk；The consumption of titanate coupling agent is the 5% of nanometer stalk quality；
(4) 100 parts of polyvinyl chloride, 15 parts of lubricants, 10 parts of coupling agent modified stalks, 50 parts of plasticizer, 3 parts of light are weighed
Stabilizer, 1 part of antioxidant, are added to height in high mixer and mix 5-6 minutes, take out standby；
(5) step (6) resulting material is added in double screw extruder, in 120-140 DEG C of extruding pelletization.According to GB/
T2406 standard testings oxygen index (OI) 37, fire resistance is good.
Claims (10)
1. a kind of preparation method of polyvinyl chloride composite materials, it is characterised in that comprise the following steps：
(1) dry stalk is crushed and adds mass fraction in 5-6% sodium hydroxide solution, 10- is soaked at 50-60 DEG C
Filtering drying after 15h；
(2) stalk after drying is placed in vacuum impregnation in the aluminum salt solution that concentration is 1.0-3.0molL-1, then by vacuum
Stalk after impregnating is at 120-150 DEG C, and the constant temperature 5-10h in hydrothermal reaction kettle is cooled to room temperature, takes out washing, and vacuum is done
It is dry to crush to obtain nanometer stalk；
(3) take a nanometer stalk to be placed in alcoholic solvent, add titanate coupling agent, stir 20-30min, filtration drying must be coupled
The nanometer stalk that agent is modified；
(4) weigh 100 parts of polyvinyl chloride, 12-15 parts of lubricants, 10-20 parts of coupling agent modified stalks, 40-50 parts of plasticizer,
1-3 parts of light stabilizers, 1-2 parts of antioxidant, are added to height in high mixer and mix 5-6 minutes, take out standby；
(5) step (4) resulting material is added in double screw extruder, in 120-140 DEG C of extruding pelletization.
2. the preparation method of polyvinyl chloride composite materials as claimed in claim 1, it is characterised in that step (1) described stalk
For maize straw or wheat stalk.
3. the preparation method of polyvinyl chloride composite materials as claimed in claim 1, it is characterised in that step (2) described aluminium salt
Solution is aluminum sulfate solution, aluminum nitrate solution or liquor alumini chloridi.
4. the preparation method of polyvinyl chloride composite materials as claimed in claim 1, it is characterised in that step (2) described vacuum
The Immersion treatment time is 5-8h, vacuum 0.1MPa.
5. the preparation method of polyvinyl chloride composite materials as claimed in claim 1, it is characterised in that step (3) described alcohol is molten
Agent is isopropanol, ethanol or methanol.
6. the preparation method of polyvinyl chloride composite materials as claimed in claim 1, it is characterised in that step (3) described metatitanic acid
The consumption of ester coupling agent is the 2-5% of nanometer stalk quality.
7. the preparation method of polyvinyl chloride composite materials as claimed in claim 1, it is characterised in that step (4) is described high mixed
The temperature of machine is 40 DEG C -50 DEG C, rotating speed is 500-800r/min.
8. the preparation method of polyvinyl chloride composite materials as claimed in claim 1, it is characterised in that step (4) lubrication
The one kind or several of agent in zinc stearate, ethylene bis stearamide, erucyl amide, polypropylene wax, Tissuemat E, oleamide
Kind.
9. the preparation method of polyvinyl chloride composite materials as claimed in claim 1, it is characterised in that step (4) plasticising
Agent is phthalate；The light stabilizer is hindered amine light stabilizer.
10. the preparation method of polyvinyl chloride composite materials as claimed in claim 1, it is characterised in that step (4) described antioxygen
Agent is antioxidant 1010 and irgasfos 168 in mass ratio 1:1 it is compound.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710557624.7A CN107226981A (en) | 2017-07-10 | 2017-07-10 | A kind of preparation method of polyvinyl chloride composite materials |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710557624.7A CN107226981A (en) | 2017-07-10 | 2017-07-10 | A kind of preparation method of polyvinyl chloride composite materials |
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| Publication Number | Publication Date |
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| CN107226981A true CN107226981A (en) | 2017-10-03 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710557624.7A Pending CN107226981A (en) | 2017-07-10 | 2017-07-10 | A kind of preparation method of polyvinyl chloride composite materials |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108250783A (en) * | 2017-12-28 | 2018-07-06 | 武汉华丽环保科技有限公司 | A kind of full biomass cellulose composite plastic and preparation method thereof |
| CN111761848A (en) * | 2020-05-19 | 2020-10-13 | 界首市鑫豪塑胶有限公司 | Method for preparing light-weight plastic flooring base material by using crop straws |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102873724A (en) * | 2012-10-15 | 2013-01-16 | 安徽农业大学 | Nanometer hydroxide wood composite material and preparation method thereof |
| CN104672707A (en) * | 2015-02-13 | 2015-06-03 | 丹东渤海节水灌溉设备有限公司 | Hard corn stalk pipe for agricultural irrigation and water supply and processing process of hard corn stalk pipe |
-
2017
- 2017-07-10 CN CN201710557624.7A patent/CN107226981A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102873724A (en) * | 2012-10-15 | 2013-01-16 | 安徽农业大学 | Nanometer hydroxide wood composite material and preparation method thereof |
| CN104672707A (en) * | 2015-02-13 | 2015-06-03 | 丹东渤海节水灌溉设备有限公司 | Hard corn stalk pipe for agricultural irrigation and water supply and processing process of hard corn stalk pipe |
Non-Patent Citations (1)
| Title |
|---|
| 焦富强: ""秸秆/PVC复合材料的制备与性能研究"", 《化工时刊》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108250783A (en) * | 2017-12-28 | 2018-07-06 | 武汉华丽环保科技有限公司 | A kind of full biomass cellulose composite plastic and preparation method thereof |
| CN111761848A (en) * | 2020-05-19 | 2020-10-13 | 界首市鑫豪塑胶有限公司 | Method for preparing light-weight plastic flooring base material by using crop straws |
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Application publication date: 20171003 |
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