CN109206784A - A kind of aqueous polyurethane toughening polyvinyl chloride tubing preparation method - Google Patents
A kind of aqueous polyurethane toughening polyvinyl chloride tubing preparation method Download PDFInfo
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- CN109206784A CN109206784A CN201810979275.2A CN201810979275A CN109206784A CN 109206784 A CN109206784 A CN 109206784A CN 201810979275 A CN201810979275 A CN 201810979275A CN 109206784 A CN109206784 A CN 109206784A
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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
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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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
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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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/267—Magnesium carbonate
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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
- C08L2203/00—Applications
- C08L2203/18—Applications used for pipes
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/06—Polymer mixtures characterised by other features having improved processability or containing aids for moulding methods
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Abstract
The invention discloses a kind of aqueous polyurethane toughening polyvinyl chloride tubing preparation methods, the polychloroethylene pipes tensile strength with higher and elongation at break of the method preparation provided through the invention, its TIR is 0-1% simultaneously, has excellent toughness and shock resistance, creep resistance, easy processing；It is handled using special calcine by steps, so that close by silicate sturcture prepared by calcium carbonate, barium carbonate, magnesium carbonate and silica, and layering is obvious, mobile performance between layers is preferable, so that silicate is had biggish specific surface area, while enhancing the interface cohesion of itself and polychloroethylene pipes substrate, make to be coextruded material with excellent tensile resistance and shock resistance, mechanical property is preferable, while reducing the viscosity of tubing melt, easy processing.
Description
Technical field
The invention belongs to tubing preparation technical field, especially a kind of aqueous polyurethane toughening polyvinyl chloride tubing preparation side
Method.
Background technique
China polychloroethylene pipes market is in ascent stage, huge market capacity and lower access threshold, makes
Polychloroethylene pipes are always the Hot events of domestic each side's investment in the past few years.Polychloroethylene pipes have weight
Gently, the advantages that corrosion resistance and good, electrical insulation capability are good, frictional resistance is small, thermal coefficient is small is important in plastic tube product
Kind all has apparent advantage in many aspects.
But in the preparation process of polychloroethylene pipes, that there is also brittleness is larger, toughness is lower, easily rupturable, weather-proof
Not the problems such as property is not good enough.
Summary of the invention
In view of the above-mentioned problems, the present invention is intended to provide a kind of toughness is preferable, is not easily broken, and weather resistance is superior aqueous
Polyurethane toughened polychloroethylene pipes preparation method.
The invention is realized by the following technical scheme:
A kind of aqueous polyurethane toughening polyvinyl chloride tubing preparation method, which is characterized in that preparation method includes the following steps:
(1) 3-5 part calcium carbonate, 2-4 parts of barium carbonates, 1-2 parts of magnesium carbonate and 5-15 parts of silica in parts by weight are put into
In ball grinder, after ball milling mixing 1-2h, 5-10 parts of dehydrated alcohols, 3-5 parts of castor oil are added, continue ball milling 3-5h, then by institute
It obtains object to be put into vacuum oven, at 150-155 DEG C after dry 20-24h, be transferred in tube furnace, with the rate of 2-4 DEG C/min
It is warming up to 360-380 DEG C, 1-2h is calcined, then be cooled to 280-300 DEG C with the rate of 4-5 DEG C/min, calcines 30-40min, then
It is warming up to 590-600 DEG C with the rate of 2-4 DEG C/min, after calcining 50-60min, 500- is cooled to the rate of 4-5 DEG C/min
510 DEG C, calcine 40-50min, be finally warming up to 820-830 DEG C with the rate of 2-4 DEG C/min, calcine 80-85min, with 4-5 DEG C/
After the rate of min is cooled to 700-705 DEG C of calcining 90-100min, room temperature is down to the rate of 6-8 DEG C/min.
(2) step (1) gains are added in the polyester polyol solution of 5-10 times of its volume, in 40-45 DEG C, 700-
2-3h is stirred under 900rpm, after then placing 2-3h at -0.08~-0.1MPa, 80-85 DEG C, then in 70-75 DEG C, 400-
1-2h is stirred under 500rpm, is down to room temperature, and filter, is freeze-dried；
(3) step (2) gains are added in the Waterborne Polyurethane Prepolymer of 5-10 times of its volume, and three second of 2-3 part is added
5-8 part distilled water are added after stirring 20-30min under 300-400rpm in amine, the stirring and emulsifying dispersion 50- at 700-800rpm
Then 90min is added 10-12 parts of chain extenders, continues after being stirred to react 2-3h, 4-5h, filtering are stood, and wash, at 50-60 DEG C
Lower drying；
(4) 80-120 parts of polyvinyl chloride, step (3) gains, 3-5 parts of rice bran oil fatty acid esters, 1-3 parts of antioxidant are put into mixed
In conjunction machine, 12-16min is stirred at 100-108 DEG C, 1200-1500rpm, then at 55-60 DEG C, 600-650rpm
It is stirred 20-30min, gains are then transferred to extrusion molding in extruder, cooling cutting.
Further, step (2) polyester polyol is polyadipate -1,4-butanediol ester or polycarbonate.
Further, step (3) chain extender is 1,4-butanediol diformazan alkyl sulfonate.
Further, step (4) extrusion temperature is 190-198 DEG C.
Further, step (3) Waterborne Polyurethane Prepolymer passes through carbon fiber modifying, specific method of modifying are as follows: will
Carbon fiber is added in mixing machine together with titanate coupling agent, is stirred to react 10- at 60-70 DEG C, 1000-1300rpm
15min is added in Waterborne Polyurethane Prepolymer after being washed out drying, ultrasonic disperse 30-40min, the ultrasound item
Part is 100-110Hz.
Beneficial effects of the present invention: the polychloroethylene pipes stretching with higher of the method preparation provided through the invention
Intensity and elongation at break, while its TIR is 0-1%, has excellent toughness and shock resistance, creep resistance, easy processing；Benefit
It is handled with special calcine by steps, so that tight by silicate sturcture prepared by calcium carbonate, barium carbonate, magnesium carbonate and silica
It is close, and be layered obviously, mobile performance between layers is preferable, so that silicate is had biggish specific surface area, enhances simultaneously
The interface cohesion of itself and polychloroethylene pipes substrate makes coextrusion material have excellent tensile resistance and shock resistance,
Mechanical property is preferable, while reducing the viscosity of tubing melt, easy processing；The presence of castor oil improves the toughness of tubing, makes
It is with good mechanical property and lower temperature resistance；Silicate is handled using polyester polyol, enhance silicate with
The compatibility and interface interaction of Waterborne Polyurethane Prepolymer, participate in it in preparation of aqueous polyurethane, are subsequent aqueous
Uniform package of the polyurethane on its surface creates condition, to further enhance the toughness of tubing；Changed using carbon fiber
Property Waterborne Polyurethane Prepolymer, then generate modified polyurethane after silicate is modified, one side silicate promotes water
Dispersion of the property polyurethane in polyvinyl chloride, so that toughening effect is obvious, while modified aqueous polyurethane also promotes silicate
Dispersion in polyvinyl chloride enhances its interface binding power with substrate, enhances the toughness of tubing, meanwhile, also largely
Improve the shock resistance of tubing.
Specific embodiment
Illustrate the present invention with specific embodiment below, but is not limitation of the present invention.
Embodiment 1
A kind of aqueous polyurethane toughening polyvinyl chloride tubing preparation method, which is characterized in that preparation method includes the following steps:
(1) 3 parts of calcium carbonate, 2 parts of barium carbonates, 1 part of magnesium carbonate and 5 parts of silica in parts by weight are put into ball grinder,
After ball milling mixing 1h, 5 parts of dehydrated alcohols, 3 parts of castor oil are added, continues ball milling 3h, gains is then put into vacuum oven
In, it at 150 DEG C after dry 20h, is transferred in tube furnace, is warming up to 360 DEG C with the rate of 2 DEG C/min, calcines 1-2h, then with 4
DEG C/rate of min is cooled to 280 DEG C, and 30min is calcined, is then warming up to 590 DEG C with the rate of 2 DEG C/min, after calcining 50min,
500 DEG C are cooled to the rate of 4 DEG C/min, calcines 40min, is finally warming up to 820 DEG C with the rate of 2 DEG C/min, calcining
80min is down to room temperature after being cooled to 700 DEG C of calcining 90min with the rate of 4 DEG C/min with the rate of 6 DEG C/min.
(2) step (1) gains are added in the polyester polyol solution of 5 times of its volume, are stirred at 40 DEG C, 700rpm
2h is mixed, after then placing 2h at -0.08MPa, 80 DEG C, then 1h is stirred at 70 DEG C, 400rpm, is down to room temperature, and filter,
Freeze-drying；
(3) step (2) gains are added in the Waterborne Polyurethane Prepolymer of 5 times of its volume, and 2 parts of triethylamines are added,
5 parts of distilled water are added after stirring 20min under 300rpm, stirring and emulsifying disperses 50min at 700rpm, and 10 parts of chain extensions are then added
Agent continues after being stirred to react 2h, stands 4h, filtering, and wash, dry at 50 DEG C；
(4) 80 parts of polyvinyl chloride, step (3) gains, 3 parts of rice bran oil fatty acid esters, 1 part of antioxidant are put into mixing machine,
It is stirred 12min at 100 DEG C, 1200rpm, 20min is then stirred at 55 DEG C, 600rpm, then by gains
It is transferred to extrusion molding in extruder, cooling cutting.
Further, step (2) polyester polyol is polyadipate -1,4-butanediol ester or polycarbonate.
Further, step (3) chain extender is 1,4-butanediol diformazan alkyl sulfonate.
Further, step (4) extrusion temperature is 190 DEG C.
Further, step (3) Waterborne Polyurethane Prepolymer passes through carbon fiber modifying, specific method of modifying are as follows: will
Carbon fiber is added in mixing machine together with titanate coupling agent, is stirred to react 10min at 60 DEG C, 1000rpm, is washed out
It is added in Waterborne Polyurethane Prepolymer after drying, ultrasonic disperse 30min, the ultrasound condition is 100Hz.
Embodiment 2
A kind of aqueous polyurethane toughening polyvinyl chloride tubing preparation method, which is characterized in that preparation method includes the following steps:
(1) 4 parts of calcium carbonate, 3 parts of barium carbonates, 2 parts of magnesium carbonate and 10 parts of silica in parts by weight are put into ball grinder
In, after ball milling mixing 2h, 8 parts of dehydrated alcohols, 4 parts of castor oil are added, continues ball milling 4h, gains is then put into vacuum drying
It in case, at 152 DEG C after dry 22h, is transferred in tube furnace, is warming up to 370 DEG C with the rate of 3 DEG C/min, calcines 2h, then with 5
DEG C/rate of min is cooled to 290 DEG C, and 35min is calcined, is then warming up to 595 DEG C with the rate of 3 DEG C/min, after calcining 55min,
505 DEG C are cooled to the rate of 5 DEG C/min, calcines 45min, is finally warming up to 825 DEG C with the rate of 3 DEG C/min, calcining
82min is down to room temperature after being cooled to 702 DEG C of calcining 95min with the rate of 5 DEG C/min with the rate of 7 DEG C/min.
(2) step (1) gains are added in the polyester polyol solution of 8 times of its volume, are stirred at 42 DEG C, 800rpm
3h is mixed, after then placing 3h at -0.09MPa, 82 DEG C, then 2h is stirred at 72 DEG C, 450rpm, is down to room temperature, and filter,
Freeze-drying；
(3) step (2) gains are added in the Waterborne Polyurethane Prepolymer of 7 times of its volume, and 3 parts of triethylamines are added,
7 parts of distilled water are added after stirring 25min under 350rpm, stirring and emulsifying disperses 70min at 750rpm, and 11 parts of chain extensions are then added
Agent continues after being stirred to react 3h, stands 5h, filtering, and wash, dry at 55 DEG C；
(4) 100 parts of polyvinyl chloride, step (3) gains, 4 parts of rice bran oil fatty acid esters, 2 parts of antioxidant are put into mixing machine,
It is stirred 15min at 105 DEG C, 1300rpm, 25min is then stirred at 58 DEG C, 620rpm, then by gains
It is transferred to extrusion molding in extruder, cooling cutting.
Further, step (2) polyester polyol is polyadipate -1,4-butanediol ester or polycarbonate.
Further, step (3) chain extender is 1,4-butanediol diformazan alkyl sulfonate.
Further, step (4) extrusion temperature is 195 DEG C.
Further, step (3) Waterborne Polyurethane Prepolymer passes through carbon fiber modifying, specific method of modifying are as follows: will
Carbon fiber is added in mixing machine together with titanate coupling agent, is stirred to react 12min at 65 DEG C, 1200rpm, is washed out
It is added in Waterborne Polyurethane Prepolymer after drying, ultrasonic disperse 35min, the ultrasound condition is 105Hz.
Embodiment 3
A kind of aqueous polyurethane toughening polyvinyl chloride tubing preparation method, which is characterized in that preparation method includes the following steps:
(1) 5 parts of calcium carbonate, 4 parts of barium carbonates, 2 parts of magnesium carbonate and 15 parts of silica in parts by weight are put into ball grinder
In, after ball milling mixing 2h, 10 parts of dehydrated alcohols, 5 parts of castor oil are added, continues ball milling 5h, gains is then put into vacuum and are done
In dry case, at 155 DEG C it is dry for 24 hours after, be transferred in tube furnace, be warming up to 380 DEG C with the rate of 4 DEG C/min, calcine 2h, then with
The rate of 5 DEG C/min is cooled to 300 DEG C, calcines 40min, is then warming up to 600 DEG C with the rate of 4 DEG C/min, calcines 60min
Afterwards, 510 DEG C are cooled to the rate of 5 DEG C/min, calcine 50min, be finally warming up to 830 DEG C with the rate of 4 DEG C/min, calcining
85min is down to room temperature after being cooled to 705 DEG C of calcining 100min with the rate of 5 DEG C/min with the rate of 8 DEG C/min.
(2) step (1) gains are added in the polyester polyol solution of 10 times of its volume, at 45 DEG C, 900rpm
3h is stirred, after then placing 3h at -0.1MPa, 85 DEG C, then 2h is stirred at 75 DEG C, 500rpm, is down to room temperature, and mistake
Filter, freeze-drying；
(3) step (2) gains are added in the Waterborne Polyurethane Prepolymer of 10 times of its volume, and 3 parts of triethylamines are added,
8 parts of distilled water are added after stirring 30min under 400rpm, stirring and emulsifying disperses 90min at 800 rpm, and 12 parts of chain extensions are then added
Agent continues after being stirred to react 3h, stands 5h, filtering, and wash, dry at 60 DEG C；
(4) 120 parts of polyvinyl chloride, step (3) gains, 5 parts of rice bran oil fatty acid esters, 3 parts of antioxidant are put into mixing machine,
It is stirred 16min at 108 DEG C, 1500rpm, 30min is then stirred at 60 DEG C, 650rpm, then by gains
It is transferred to extrusion molding in extruder, cooling cutting.
Further, step (2) polyester polyol is polyadipate -1,4-butanediol ester or polycarbonate.
Further, step (3) chain extender is 1,4-butanediol diformazan alkyl sulfonate.
Further, step (4) extrusion temperature is 198 DEG C.
Further, step (3) Waterborne Polyurethane Prepolymer passes through carbon fiber modifying, specific method of modifying are as follows: will
Carbon fiber is added in mixing machine together with titanate coupling agent, is stirred to react 15min at 70 DEG C, 1300rpm, is washed out
It is added in Waterborne Polyurethane Prepolymer after drying, ultrasonic disperse 40min, the ultrasound condition is 110Hz.
Comparative example 1
This comparative example will be directly placed into pipe after calcium carbonate, barium carbonate, magnesium carbonate, silica drying compared to embodiment 2
3h is calcined in formula furnace at 825 DEG C, method and step in addition to this is all the same.
Comparative example 2
The addition of castor oil is omitted compared to embodiment 2 in this comparative example, and method and step in addition to this is all the same.
Comparative example 3
The processing of step (2) is omitted compared to embodiment 2 in this comparative example, and method and step in addition to this is all the same.
Comparative example 4
The modification of Waterborne Polyurethane Prepolymer, method in addition to this is omitted compared to embodiment 2 in this comparative example
Step is all the same.
Tensile strength, the impact property of sample obtained by each embodiment and comparative example are tested for the property, wherein resisting
Impact property is tested using drop impact, its impact property TIR, test result such as 1 institute of table are tested under the conditions of 20 DEG C, 2Kg, 2M
Show:
Table 1
As can be seen from Table 1, polychloroethylene pipes prepared by the present invention tensile strength with higher and elongation at break, simultaneously
Its TIR is 0-1%, has excellent toughness and shock resistance.
Claims (5)
1. a kind of aqueous polyurethane toughening polyvinyl chloride tubing preparation method, which is characterized in that preparation method includes following step
It is rapid:
(1) 3-5 part calcium carbonate, 2-4 parts of barium carbonates, 1-2 parts of magnesium carbonate and 5-15 parts of silica in parts by weight are put into
In ball grinder, after ball milling mixing 1-2h, 5-10 parts of dehydrated alcohols, 3-5 parts of castor oil are added, continue ball milling 3-5h, then by institute
It obtains object to be put into vacuum oven, at 150-155 DEG C after dry 20-24h, be transferred in tube furnace, with the rate of 2-4 DEG C/min
It is warming up to 360-380 DEG C, 1-2h is calcined, then be cooled to 280-300 DEG C with the rate of 4-5 DEG C/min, calcines 30-40min, then
It is warming up to 590-600 DEG C with the rate of 2-4 DEG C/min, after calcining 50-60min, 500- is cooled to the rate of 4-5 DEG C/min
510 DEG C, calcine 40-50min, be finally warming up to 820-830 DEG C with the rate of 2-4 DEG C/min, calcine 80-85min, with 4-5 DEG C/
After the rate of min is cooled to 700-705 DEG C of calcining 90-100min, room temperature is down to the rate of 6-8 DEG C/min.
(2) step (1) gains are added in the polyester polyol solution of 5-10 times of its volume, in 40-45 DEG C, 700-
2-3h is stirred under 900rpm, after then placing 2-3h at -0.08~-0.1MPa, 80-85 DEG C, then in 70-75 DEG C, 400-
1-2h is stirred under 500rpm, is down to room temperature, and filter, is freeze-dried；
(3) step (2) gains are added in the Waterborne Polyurethane Prepolymer of 5-10 times of its volume, and three second of 2-3 part is added
5-8 part distilled water are added after stirring 20-30min under 300-400rpm in amine, the stirring and emulsifying dispersion 50- at 700-800rpm
Then 90min is added 10-12 parts of chain extenders, continues after being stirred to react 2-3h, 4-5h, filtering are stood, and wash, at 50-60 DEG C
Lower drying；
(4) 80-120 parts of polyvinyl chloride, step (3) gains, 3-5 parts of rice bran oil fatty acid esters, 1-3 parts of antioxidant are put into mixed
In conjunction machine, 12-16min is stirred at 100-108 DEG C, 1200-1500rpm, then at 55-60 DEG C, 600-650rpm
It is stirred 20-30min, gains are then transferred to extrusion molding in extruder, cooling cutting.
2. a kind of aqueous polyurethane toughening polyvinyl chloride tubing preparation method according to claim 1, which is characterized in that step
Suddenly (2) described polyester polyol is polyadipate -1,4-butanediol ester or polycarbonate.
3. a kind of aqueous polyurethane toughening polyvinyl chloride tubing preparation method according to claim 1, which is characterized in that step
Suddenly (3) described chain extender is 1,4-butanediol diformazan alkyl sulfonate.
4. a kind of aqueous polyurethane toughening polyvinyl chloride tubing preparation method according to claim 1, which is characterized in that step
Suddenly (4) described extrusion temperature is 190-198 DEG C.
5. a kind of aqueous polyurethane toughening polyvinyl chloride tubing preparation method according to claim 1, which is characterized in that step
Suddenly (3) described Waterborne Polyurethane Prepolymer passes through carbon fiber modifying, specific method of modifying are as follows: by carbon fiber and titanate coupling agent
It is added in mixing machine together, is stirred to react 10-15min at 60-70 DEG C, 1000-1300rpm, add after being washed out drying
Enter into Waterborne Polyurethane Prepolymer, ultrasonic disperse 30-40min, the ultrasound condition is 100-110Hz.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110358284A (en) * | 2019-08-20 | 2019-10-22 | 南通华能新材料有限公司 | A kind of environment-friendly type PVC material |
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| CN110358284A (en) * | 2019-08-20 | 2019-10-22 | 南通华能新材料有限公司 | A kind of environment-friendly type PVC material |
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Application publication date: 20190115 |