CN108329629A - A kind of polyvinyl chloride-based wear resistant filler and preparation method thereof - Google Patents
A kind of polyvinyl chloride-based wear resistant filler and preparation method thereof Download PDFInfo
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- CN108329629A CN108329629A CN201810158061.9A CN201810158061A CN108329629A CN 108329629 A CN108329629 A CN 108329629A CN 201810158061 A CN201810158061 A CN 201810158061A CN 108329629 A CN108329629 A CN 108329629A
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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
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
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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
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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
- C08K3/28—Nitrogen-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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-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
- C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
- C08K5/098—Metal salts of carboxylic acids
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- 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
- C08K3/32—Phosphorus-containing compounds
- C08K2003/321—Phosphates
- C08K2003/322—Ammonium phosphate
Abstract
The invention is related to a kind of polyvinyl chloride-based wear resistant filler, including following raw material components：Modified polyvinyl chloride, modified calcium carbonate, modified calcium oxalate, modified polyvinyl chloride is by hydroxyacetic acid modified polyvinyl chloride, ammonium oxalate, ammonium carbonate and ammonium phosphate reaction are made, hydroxyacetic acid modified polyvinyl chloride is by polyvinyl chloride, hydroxyacetic acid, lactic acid, sodium ethoxide, sodium hydrate aqueous solution, the concentrated sulfuric acid and phosphorus pentoxide reaction are made, modified calcium carbonate is by calcium chloride, 1 decyl 2, 3 methylimidazole toluenesulfonates, ammonium hydrogen carbonate and ammonium oleate reaction are made, modified calcium oxalate is by oxalic acid, calcium stearate, ethyl alcohol, water and the reaction of 1 butyl, 3 methylimidazole dodecane sulfonate are made.The invention has excellent wearability.
Description
Technical field
The invention is related to a kind of polyvinyl chloride-based wear resistant filler and preparation method thereof.
Background technology
Polyvinyl chloride has the advantages such as excellent mechanical strength, processing performance, high oxygen index (OI), wearability, polyvinyl chloride quilt
It is widely used in the fields such as plastic plate, plastic package material, shopping bag, plastic label material, plastic pipe.
Currently, pvc material needs further to be promoted in wearability.The invention is using modified polyvinyl chloride, carbonic acid
Calcium, calcium oxalate are prepared for polyvinyl chloride-based wear resistant filler, and polyvinyl chloride-based wear resistant filler prepared by this method has excellent resistance to
Mill property.
Invention content
The invention is designed to provide a kind of preparation method of polyvinyl chloride-based wear resistant filler, and this method is anti-by changing
Answer raw material and technology mode, the material of preparation that there is excellent wearability.
To achieve the goals above, the technical solution of the invention is as follows.
A kind of polyvinyl chloride-based wear resistant filler and preparation method thereof, specifically includes following steps：(1), by oxalic acid, stearic acid
Calcium, ethyl alcohol, water and 1- butyl -3- methylimidazoles dodecane sulfonate are 10 according to quality parts ratio：63~71：137~
151：35~46：95~116 are added in hydrothermal reaction kettle, react 35min under the conditions of 32~45 DEG C of maintenance system temperature, production
Object through 78 DEG C of 1L benzene wash 3 times, 65 DEG C of 500mL ethyl alcohol wash 2 times, be dried in vacuo 20min, powder in 53 DEG C, -0.09MPa
It is broken, obtain modified calcium oxalate；(2), by calcium chloride, 1- decyl -2,3- methylimidazoles toluenesulfonate, ammonium hydrogen carbonate and
Ammonium oleate is 70 according to quality parts ratio：120~134：112~126：9~15 are added in reaction kettle, mixing speed be 88~
97r/min reacts 1~3h under the conditions of 93~115 DEG C of maintenance system temperature, and product is through 1L ethyl alcohol concussion washing 3 times, in 65
DEG C, -0.07MPa be dried in vacuo 11min, crush, obtain modified calcium carbonate；(3), by polyvinyl chloride and sodium ethoxide according to mass parts
Number ratio 83：45~53 are added in hydrothermal reaction kettle, maintain 35 DEG C of hydro-thermal reaction 8min, the hydrogen for being 39~44 by quality parts ratio
Aqueous solution of sodium oxide is added in hydrothermal reaction kettle, maintain 39 DEG C of hydro-thermal reaction 5min, product through filtering, water washing to neutrality,
It is dried in vacuo 14min in 65 DEG C, -0.06MPa, is 35~41 by product and quality parts ratio：5~8：3~5：9~14 hydroxyl
Acetic acid, lactic acid, the concentrated sulfuric acid and phosphorus pentoxide are added in reaction kettle, and mixing speed is 83~95r/min, maintenance system temperature
118~131 DEG C, 2~4h is reacted under the conditions of -0.07MPa, product is through filtering, water washing to neutrality, 67 DEG C, -0.07MPa vacuum
Dry 10min is to get to hydroxyacetic acid modified polyvinyl chloride；(4), by hydroxyacetic acid modified polyvinyl chloride, ammonium oxalate, ammonium carbonate
With ammonium phosphate according to quality parts ratio 88：17~23：12~18：8~12 are added in high-speed mixer, are existed with high-speed mixer
173~176 DEG C of 1~4min of hybrid reaction of temperature, with extruder in 174~177 DEG C of extruding pelletizations of temperature to get to modified polychlorostyrene
Ethylene；(5), by modified polyvinyl chloride, modified calcium carbonate, modified calcium oxalate according to quality parts ratio 82：35~44：45~51 add
Enter into high-speed mixer, with high-speed mixer in 178~185 DEG C of 1~4min of hybrid reaction of temperature, with extruder in temperature
178~187 DEG C of extruding pelletizations are to get to polyvinyl chloride-based wear resistant filler.
The preparation method of polyvinyl chloride-based wear resistant filler described in the invention, includes the following steps：
(1), by oxalic acid, calcium stearate, ethyl alcohol, water and 1- butyl -3- methylimidazole dodecane sulfonates according to mass fraction
Than being 10：63~71：137~151：35~46：95~116 are added in hydrothermal reaction kettle, 32~45 DEG C of maintenance system temperature
Under the conditions of react 35min, product through 78 DEG C of 1L benzene wash 3 times, 65 DEG C of 500mL ethyl alcohol wash 2 times, in 53 DEG C, -0.09MPa
It is dried in vacuo 20min, is crushed, modified calcium oxalate is obtained；The purpose of the 1- butyl -3- methylimidazole dodecane sulfonates
For the thermal coefficient as reaction medium and raising reaction system and product.
(2), by calcium chloride, 1- decyl -2,3- methylimidazoles toluenesulfonate, ammonium hydrogen carbonate and ammonium oleate according to
Quality parts ratio is 70：120~134：112~126：9~15 are added in reaction kettle, and mixing speed is 88~97r/min, dimension
Hold and react 1~3h under the conditions of 93~115 DEG C of system temperature, product through 1L ethyl alcohol concussion washing 3 times, in 65 DEG C, -0.07MPa it is true
The dry 11min of sky, crushes, obtains modified calcium carbonate；The mesh of the 1- decyl -2,3- methylimidazole toluenesulfonates
In order to improve the thermal coefficient of modified calcium carbonate.
(3), by polyvinyl chloride and sodium ethoxide according to quality parts ratio 83：45~53 are added in hydrothermal reaction kettle, maintain
The sodium hydrate aqueous solution that quality parts ratio is 39~44 is added in hydrothermal reaction kettle by 35 DEG C of hydro-thermal reaction 8min, is maintained
39 DEG C of hydro-thermal reaction 5min, product is dried in vacuo 14min through filtering, water washing to neutrality, in 65 DEG C, -0.06MPa, by product
It is 35~41 with quality parts ratio：5~8：3~5：9~14 hydroxyacetic acid, lactic acid, the concentrated sulfuric acid and phosphorus pentoxide is added to
In reaction kettle, mixing speed is 83~95r/min, reaction 2 under the conditions of 118~131 DEG C of maintenance system temperature, -0.07MPa~
4h, product through filtering, water washing to neutrality, 67 DEG C, -0.07MPa vacuum drying 10min to get to hydroxyacetic acid be modified polychlorostyrene
Ethylene；The purpose of the hydroxyacetic acid and lactic acid is in order to be modified polyvinyl chloride.
(4), by hydroxyacetic acid modified polyvinyl chloride, ammonium oxalate, ammonium carbonate and ammonium phosphate according to quality parts ratio 88：17~
23：12~18：8~12 are added in high-speed mixer, with high-speed mixer 173~176 DEG C of hybrid reactions 1 of temperature~
4min, with extruder in 174~177 DEG C of extruding pelletizations of temperature to get to modified polyvinyl chloride；The ammonium oxalate, ammonium carbonate
Purpose with ammonium phosphate is in order to as pore creating material, improve the porosity of polyvinyl chloride.
(5), by modified polyvinyl chloride, modified calcium carbonate, modified calcium oxalate according to quality parts ratio 82：35~44：45~
51 are added in high-speed mixer, with high-speed mixer in 178~185 DEG C of 1~4min of hybrid reaction of temperature, with extruder in temperature
178~187 DEG C of extruding pelletizations are spent to get to polyvinyl chloride-based wear resistant filler；The modified polyvinyl chloride, modified calcium carbonate and
While being modified thermal coefficient of the purpose of calcium oxalate in order to improve polyvinyl chloride-based wear resistant filler, improve polyvinyl chloride-based wear-resisting
The wearability of filler.
Invention has the beneficial effects that：
Polyvinyl chloride-based wear resistant filler prepared by the present invention has excellent wearability, thermal coefficient, particle uniformity and storage
Stability can significantly improve the wearability of material.
Specific implementation mode
The specific implementation mode of the invention is described with reference to embodiment, to be better understood from the invention.
Embodiment 1
A kind of polyvinyl chloride-based wear resistant filler, preparation method includes the following steps：
(1), 10 parts of oxalic acid, 67 parts of calcium stearates, 145 parts of ethyl alcohol, 41 parts of water and 103 parts of 1- butyl -3- methylimidazoles ten are weighed
Dialkyl group sulfonate is added in hydrothermal reaction kettle, 35min is reacted under the conditions of 35 DEG C of maintenance system temperature, product is through 78 DEG C of 1L
Benzene wash 3 times, 65 DEG C of 500mL ethyl alcohol wash 2 times, be dried in vacuo 20min in 53 DEG C, -0.09MPa, crush, obtain modified grass
Sour calcium；
(2), 70 parts of calcium chloride, 128 parts of 1- decyl -2,3- methylimidazoles toluenesulfonates, 119 parts of ammonium hydrogen carbonate are weighed
It is added in reaction kettle with 13 parts of ammonium oleates, mixing speed 92r/min, reacts 2h under the conditions of 105 DEG C of maintenance system temperature,
Product is dried in vacuo 11min through 1L ethyl alcohol concussion washing 3 times, in 65 DEG C, -0.07MPa, crushes, obtains modified calcium carbonate；
(3), 83 parts of polyvinyl chloride are weighed and 45 parts of sodium ethoxides are added in hydrothermal reaction kettle, maintain 35 DEG C of hydro-thermal reaction 8min,
40 parts of sodium hydrate aqueous solutions are added in hydrothermal reaction kettle, maintain 39 DEG C of hydro-thermal reaction 5min, product is through filtering, water washing
To neutrality, it is dried in vacuo 14min in 65 DEG C, -0.06MPa, by product and 38 parts of hydroxyacetic acids, 6.5 parts of lactic acid, 3.5 parts of dense sulphur
Acid and 10 parts of phosphorus pentoxides are added in reaction kettle, mixing speed 85r/min, 128 DEG C of maintenance system temperature ,-
React 3h under the conditions of 0.07MPa, product through filtering, water washing to neutrality, 67 DEG C, -0.07MPa vacuum drying 10min to get to
Hydroxyacetic acid modified polyvinyl chloride；
(4), 88 parts of hydroxyacetic acid modified polyvinyl chlorides, 21 parts of ammonium oxalate, 16 parts of ammonium carbonates and 9 parts of ammonium phosphate are weighed and are added to height
In fast mixing machine, with high-speed mixer in 173 DEG C of hybrid reaction 3min of temperature, with extruder in 176 DEG C of extruding pelletizations of temperature, i.e.,
Obtain modified polyvinyl chloride；
(5), 82 parts of modified polyvinyl chlorides, 39 parts of modified calcium carbonates, 49 parts of modified calcium oxalates are weighed to be added in high-speed mixer,
With high-speed mixer in 179 DEG C of hybrid reaction 3min of temperature, with extruder in 12 DEG C of extruding pelletizations of temperature to get to polyvinyl chloride
Base wear resistant filler.
Embodiment 2
A kind of polyvinyl chloride-based wear resistant filler, preparation method includes the following steps：
(1), 10 parts of oxalic acid, 63 parts of calcium stearates, 137 parts of ethyl alcohol, 35 parts of water and 95 parts of 1- butyl -3- methylimidazoles 12 are weighed
Alkylsulfonate is added in hydrothermal reaction kettle, 35min is reacted under the conditions of 32 DEG C of maintenance system temperature, product is through 78 DEG C of 1L
Benzene wash 3 times, 65 DEG C of 500mL ethyl alcohol wash 2 times, be dried in vacuo 20min in 53 DEG C, -0.09MPa, crush, obtain modified grass
Sour calcium；
(2), 70 parts of calcium chloride, 120 parts of 1- decyl -2,3- methylimidazoles toluenesulfonates, 112 parts of ammonium hydrogen carbonate are weighed
It is added in reaction kettle with 9 parts of ammonium oleates, mixing speed 88r/min, reacts 3h under the conditions of 93 DEG C of maintenance system temperature, produced
Object is dried in vacuo 11min through 1L ethyl alcohol concussion washing 3 times, in 65 DEG C, -0.07MPa, crushes, obtains modified calcium carbonate；
(3), 83 parts of polyvinyl chloride are weighed and 45 parts of sodium ethoxides are added in hydrothermal reaction kettle, maintain 35 DEG C of hydro-thermal reaction 8min,
39 parts of sodium hydrate aqueous solutions are added in hydrothermal reaction kettle, maintain 39 DEG C of hydro-thermal reaction 5min, product is through filtering, water washing
To neutrality, it is dried in vacuo 14min in 65 DEG C, -0.06MPa, by product and 35 parts of hydroxyacetic acids, 5 parts of lactic acid, 3 parts of concentrated sulfuric acids and 9
Part phosphorus pentoxide is added in reaction kettle, mixing speed 83r/min, 118 DEG C of maintenance system temperature, -0.07MPa conditions
Lower reaction 4h, product through filtering, water washing to neutrality, 67 DEG C, -0.07MPa vacuum drying 10min change to get to hydroxyacetic acid
Property polyvinyl chloride；
(4), 88 parts of hydroxyacetic acid modified polyvinyl chlorides, 17 parts of ammonium oxalate, 12 parts of ammonium carbonates and 8 parts of ammonium phosphate are weighed and are added to height
In fast mixing machine, with high-speed mixer in 173 DEG C of hybrid reaction 4min of temperature, with extruder in 174 DEG C of extruding pelletizations of temperature, i.e.,
Obtain modified polyvinyl chloride；
(5), 82 parts of modified polyvinyl chlorides, 35 parts of modified calcium carbonates, 45 parts of modified calcium oxalates are weighed to be added in high-speed mixer,
With high-speed mixer in 178 DEG C of hybrid reaction 4min of temperature, with extruder in 178 DEG C of extruding pelletizations of temperature to get to polychlorostyrene second
Alkenyl wear resistant filler.
Embodiment 3
A kind of polyvinyl chloride-based wear resistant filler, preparation method includes the following steps：
(1), 10 parts of oxalic acid, 71 parts of calcium stearates, 151 parts of ethyl alcohol, 46 parts of water and 116 parts of 1- butyl -3- methylimidazoles ten are weighed
Dialkyl group sulfonate is added in hydrothermal reaction kettle, 35min is reacted under the conditions of 45 DEG C of maintenance system temperature, product is through 78 DEG C of 1L
Benzene wash 3 times, 65 DEG C of 500mL ethyl alcohol wash 2 times, be dried in vacuo 20min in 53 DEG C, -0.09MPa, crush, obtain modified grass
Sour calcium；
(2), 70 parts of calcium chloride, 134 parts of 1- decyl -2,3- methylimidazoles toluenesulfonates, 126 parts of ammonium hydrogen carbonate are weighed
It is added in reaction kettle with 15 parts of ammonium oleates, mixing speed 97r/min, reacts 1h under the conditions of 115 DEG C of maintenance system temperature,
Product is dried in vacuo 11min through 1L ethyl alcohol concussion washing 3 times, in 65 DEG C, -0.07MPa, crushes, obtains modified calcium carbonate；
(3), 83 parts of polyvinyl chloride are weighed and 53 parts of sodium ethoxides are added in hydrothermal reaction kettle, maintain 35 DEG C of hydro-thermal reaction 8min,
44 parts of sodium hydrate aqueous solutions are added in hydrothermal reaction kettle, maintain 39 DEG C of hydro-thermal reaction 5min, product is through filtering, water washing
To neutrality, 14min is dried in vacuo in 65 DEG C, -0.06MPa, by product and 41 parts of hydroxyacetic acids, 8 parts of lactic acid, 5 parts of concentrated sulfuric acids and
14 parts of phosphorus pentoxides are added in reaction kettle, mixing speed 95r/min, 131 DEG C of maintenance system temperature, -0.07MPa items
React 2h under part, product is through filtering, water washing to neutrality, 67 DEG C, -0.07MPa vacuum drying 10min are to get to hydroxyacetic acid
Modified polyvinyl chloride；
(4), 88 parts of hydroxyacetic acid modified polyvinyl chlorides, 23 parts of ammonium oxalate, 18 parts of ammonium carbonates and 12 parts of ammonium phosphate are weighed to be added to
In high-speed mixer, with high-speed mixer in 176 DEG C of hybrid reaction 1min of temperature, with extruder in 177 DEG C of extruding pelletizations of temperature,
Obtain modified polyvinyl chloride；
(5), 82 parts of modified polyvinyl chlorides, 44 parts of modified calcium carbonates, 51 parts of modified calcium oxalates are weighed to be added in high-speed mixer,
With high-speed mixer in 185 DEG C of hybrid reaction 1min of temperature, with extruder in 187 DEG C of extruding pelletizations of temperature to get to polychlorostyrene second
Alkenyl wear resistant filler.
Embodiment 4
A kind of polyvinyl chloride-based wear resistant filler, preparation method includes the following steps：
(1), 10 parts of oxalic acid, 65 parts of calcium stearates, 140 parts of ethyl alcohol, 40 parts of water and 105 parts of 1- butyl -3- methylimidazoles ten are weighed
Dialkyl group sulfonate is added in hydrothermal reaction kettle, 35min is reacted under the conditions of 35 DEG C of maintenance system temperature, product is through 78 DEG C of 1L
Benzene wash 3 times, 65 DEG C of 500mL ethyl alcohol wash 2 times, be dried in vacuo 20min in 53 DEG C, -0.09MPa, crush, obtain modified grass
Sour calcium；
(2), 70 parts of calcium chloride, 125 parts of 1- decyl -2,3- methylimidazoles toluenesulfonates, 120 parts of ammonium hydrogen carbonate are weighed
It is added in reaction kettle with 10 parts of ammonium oleates, mixing speed 90r/min, reacts 2h under the conditions of 95 DEG C of maintenance system temperature, produced
Object is dried in vacuo 11min through 1L ethyl alcohol concussion washing 3 times, in 65 DEG C, -0.07MPa, crushes, obtains modified calcium carbonate；
(3), 83 parts of polyvinyl chloride are weighed and 50 parts of sodium ethoxides are added in hydrothermal reaction kettle, maintain 35 DEG C of hydro-thermal reaction 8min,
40 parts of sodium hydrate aqueous solutions are added in hydrothermal reaction kettle, maintain 39 DEG C of hydro-thermal reaction 5min, product is through filtering, water washing
To neutrality, 14min is dried in vacuo in 65 DEG C, -0.06MPa, by product and 40 parts of hydroxyacetic acids, 6 parts of lactic acid, 4 parts of concentrated sulfuric acids and
10 parts of phosphorus pentoxides are added in reaction kettle, mixing speed 90r/min, 125 DEG C of maintenance system temperature, -0.07MPa items
React 3h under part, product is through filtering, water washing to neutrality, 67 DEG C, -0.07MPa vacuum drying 10min are to get to hydroxyacetic acid
Modified polyvinyl chloride；
(4), 88 parts of hydroxyacetic acid modified polyvinyl chlorides, 20 parts of ammonium oxalate, 15 parts of ammonium carbonates and 10 parts of ammonium phosphate are weighed to be added to
In high-speed mixer, with high-speed mixer in 175 DEG C of hybrid reaction 3min of temperature, with extruder in 175 DEG C of extruding pelletizations of temperature,
Obtain modified polyvinyl chloride；
(5), 82 parts of modified polyvinyl chlorides, 40 parts of modified calcium carbonates, 50 parts of modified calcium oxalates are weighed to be added in high-speed mixer,
With high-speed mixer in 180 DEG C of hybrid reaction 2min of temperature, with extruder in 185 DEG C of extruding pelletizations of temperature to get to polychlorostyrene second
Alkenyl wear resistant filler.
Embodiment 5
A kind of polyvinyl chloride-based wear resistant filler, preparation method includes the following steps：
(1), 10 parts of oxalic acid, 66 parts of calcium stearates, 139 parts of ethyl alcohol, 37 parts of water and 99 parts of 1- butyl -3- methylimidazoles 12 are weighed
Alkylsulfonate is added in hydrothermal reaction kettle, 35min is reacted under the conditions of 33 DEG C of maintenance system temperature, product is through 78 DEG C of 1L
Benzene wash 3 times, 65 DEG C of 500mL ethyl alcohol wash 2 times, be dried in vacuo 20min in 53 DEG C, -0.09MPa, crush, obtain modified grass
Sour calcium；
(2), 70 parts of calcium chloride, 128 parts of 1- decyl -2,3- methylimidazoles toluenesulfonates, 119 parts of ammonium hydrogen carbonate are weighed
It is added in reaction kettle with 11 parts of ammonium oleates, mixing speed 89r/min, reacts 1.5h under the conditions of 98 DEG C of maintenance system temperature,
Product is dried in vacuo 11min through 1L ethyl alcohol concussion washing 3 times, in 65 DEG C, -0.07MPa, crushes, obtains modified calcium carbonate；
(3), 83 parts of polyvinyl chloride are weighed and 49 parts of sodium ethoxides are added in hydrothermal reaction kettle, maintain 35 DEG C of hydro-thermal reaction 8min,
41 parts of sodium hydrate aqueous solutions are added in hydrothermal reaction kettle, maintain 39 DEG C of hydro-thermal reaction 5min, product is through filtering, water washing
To neutrality, it is dried in vacuo 14min in 65 DEG C, -0.06MPa, by product and 39 parts of hydroxyacetic acids, 6 parts of lactic acid, 4.5 parts of concentrated sulfuric acids
It is added in reaction kettle with 11 parts of phosphorus pentoxides, mixing speed 91r/min, 119 DEG C of maintenance system temperature, -0.07MPa
Under the conditions of react 2.5h, product is through filtering, water washing to neutrality, 67 DEG C, -0.07MPa vacuum drying 10min are to get to hydroxyl
Acetic acid modified polyvinyl chloride；
(4), 88 parts of hydroxyacetic acid modified polyvinyl chlorides, 19 parts of ammonium oxalate, 14 parts of ammonium carbonates and 9 parts of ammonium phosphate are weighed and are added to height
In fast mixing machine, with high-speed mixer in 174 DEG C of hybrid reaction 3min of temperature, with extruder in 177 DEG C of extruding pelletizations of temperature, i.e.,
Obtain modified polyvinyl chloride；
(5), 82 parts of modified polyvinyl chlorides, 39 parts of modified calcium carbonates, 48 parts of modified calcium oxalates are weighed to be added in high-speed mixer,
With high-speed mixer in 179 DEG C of hybrid reaction 2min of temperature, with extruder in 183 DEG C of extruding pelletizations of temperature to get to polychlorostyrene second
Alkenyl wear resistant filler.
Embodiment 6
A kind of polyvinyl chloride-based wear resistant filler, preparation method includes the following steps：
(1), 10 parts of oxalic acid, 67 parts of calcium stearates, 146 parts of ethyl alcohol, 40 parts of water and 99 parts of 1- butyl -3- methylimidazoles 12 are weighed
Alkylsulfonate is added in hydrothermal reaction kettle, 35min is reacted under the conditions of 39 DEG C of maintenance system temperature, product is through 78 DEG C of 1L
Benzene wash 3 times, 65 DEG C of 500mL ethyl alcohol wash 2 times, be dried in vacuo 20min in 53 DEG C, -0.09MPa, crush, obtain modified grass
Sour calcium；
(2), 70 parts of calcium chloride, 128 parts of 1- decyl -2,3- methylimidazoles toluenesulfonates, 118 parts of ammonium hydrogen carbonate are weighed
It is added in reaction kettle with 11 parts of ammonium oleates, mixing speed 96r/min, is reacted under the conditions of 112 DEG C of maintenance system temperature
2.5h, product are dried in vacuo 11min through 1L ethyl alcohol concussion washing 3 times, in 65 DEG C, -0.07MPa, crush, and obtain modified carbonic acid
Calcium；
(3), 83 parts of polyvinyl chloride are weighed and 51 parts of sodium ethoxides are added in hydrothermal reaction kettle, maintain 35 DEG C of hydro-thermal reaction 8min,
43 parts of sodium hydrate aqueous solutions are added in hydrothermal reaction kettle, maintain 39 DEG C of hydro-thermal reaction 5min, product is through filtering, water washing
To neutrality, it is dried in vacuo 14min in 65 DEG C, -0.06MPa, by product and 40 parts of hydroxyacetic acids, 6.5 parts of lactic acid, 4.3 parts of dense sulphur
Acid and 13 parts of phosphorus pentoxides are added in reaction kettle, mixing speed 90r/min, 127 DEG C of maintenance system temperature ,-
React 2.7h under the conditions of 0.07MPa, product through filtering, water washing to neutrality, 67 DEG C, -0.07MPa vacuum drying 10min to get
To hydroxyacetic acid modified polyvinyl chloride；
(4), 88 parts of hydroxyacetic acid modified polyvinyl chlorides, 22 parts of ammonium oxalate, 16 parts of ammonium carbonates and 11 parts of ammonium phosphate are weighed to be added to
In high-speed mixer, with high-speed mixer in 174 DEG C of hybrid reaction 2min of temperature, with extruder in 176 DEG C of extruding pelletizations of temperature,
Obtain modified polyvinyl chloride；
(5), 82 parts of modified polyvinyl chlorides, 41 parts of modified calcium carbonates, 50 parts of modified calcium oxalates are weighed to be added in high-speed mixer,
With high-speed mixer in 182 DEG C of hybrid reaction 2min of temperature, with extruder in 186 DEG C of extruding pelletizations of temperature to get to polychlorostyrene second
Alkenyl wear resistant filler.
Embodiment 7
A kind of polyvinyl chloride-based wear resistant filler, preparation method includes the following steps：
(1), 10 parts of oxalic acid, 69 parts of calcium stearates, 147 parts of ethyl alcohol, 41 parts of water and 110 parts of 1- butyl -3- methylimidazoles ten are weighed
Dialkyl group sulfonate is added in hydrothermal reaction kettle, 35min is reacted under the conditions of 39 DEG C of maintenance system temperature, product is through 78 DEG C of 1L
Benzene wash 3 times, 65 DEG C of 500mL ethyl alcohol wash 2 times, be dried in vacuo 20min in 53 DEG C, -0.09MPa, crush, obtain modified grass
Sour calcium；
(2), 70 parts of calcium chloride, 131 parts of 1- decyl -2,3- methylimidazoles toluenesulfonates, 119 parts of ammonium hydrogen carbonate are weighed
It is added in reaction kettle with 13 parts of ammonium oleates, mixing speed 92r/min, is reacted under the conditions of 113 DEG C of maintenance system temperature
1.8h, product are dried in vacuo 11min through 1L ethyl alcohol concussion washing 3 times, in 65 DEG C, -0.07MPa, crush, and obtain modified carbonic acid
Calcium；
(3), 83 parts of polyvinyl chloride are weighed and 50 parts of sodium ethoxides are added in hydrothermal reaction kettle, maintain 35 DEG C of hydro-thermal reaction 8min,
43 parts of sodium hydrate aqueous solutions are added in hydrothermal reaction kettle, maintain 39 DEG C of hydro-thermal reaction 5min, product is through filtering, water washing
To neutrality, it is dried in vacuo 14min in 65 DEG C, -0.06MPa, by product and 39 parts of hydroxyacetic acids, 6.5 parts of lactic acid, 4.5 parts of dense sulphur
Acid and 11 parts of phosphorus pentoxides are added in reaction kettle, mixing speed 90r/min, 126 DEG C of maintenance system temperature ,-
React 3.5h under the conditions of 0.07MPa, product through filtering, water washing to neutrality, 67 DEG C, -0.07MPa vacuum drying 10min to get
To hydroxyacetic acid modified polyvinyl chloride；
(4), 88 parts of hydroxyacetic acid modified polyvinyl chlorides, 21 parts of ammonium oxalate, 16 parts of ammonium carbonates and 10 parts of ammonium phosphate are weighed to be added to
In high-speed mixer, with high-speed mixer in 174 DEG C of hybrid reaction 3min of temperature, with extruder in 175 DEG C of extruding pelletizations of temperature,
Obtain modified polyvinyl chloride；
(5), 82 parts of modified polyvinyl chlorides, 43 parts of modified calcium carbonates, 46 parts of modified calcium oxalates are weighed to be added in high-speed mixer,
With high-speed mixer in 183 DEG C of hybrid reaction 2min of temperature, with extruder in 187 DEG C of extruding pelletizations of temperature to get to polychlorostyrene second
Alkenyl wear resistant filler.
Embodiment 8
A kind of polyvinyl chloride-based wear resistant filler, preparation method includes the following steps：
(1), 10 parts of oxalic acid, 68 parts of calcium stearates, 144 parts of ethyl alcohol, 44 parts of water and 113 parts of 1- butyl -3- methylimidazoles ten are weighed
Dialkyl group sulfonate is added in hydrothermal reaction kettle, 35min is reacted under the conditions of 37 DEG C of maintenance system temperature, product is through 78 DEG C of 1L
Benzene wash 3 times, 65 DEG C of 500mL ethyl alcohol wash 2 times, be dried in vacuo 20min in 53 DEG C, -0.09MPa, crush, obtain modified grass
Sour calcium；
(2), 70 parts of calcium chloride, 131 parts of 1- decyl -2,3- methylimidazoles toluenesulfonates, 123 parts of ammonium hydrogen carbonate are weighed
It is added in reaction kettle with 11 parts of ammonium oleates, mixing speed 95r/min, is reacted under the conditions of 110 DEG C of maintenance system temperature
2.5h, product are dried in vacuo 11min through 1L ethyl alcohol concussion washing 3 times, in 65 DEG C, -0.07MPa, crush, and obtain modified carbonic acid
Calcium；
(3), 83 parts of polyvinyl chloride are weighed and 51 parts of sodium ethoxides are added in hydrothermal reaction kettle, maintain 35 DEG C of hydro-thermal reaction 8min,
40 parts of sodium hydrate aqueous solutions are added in hydrothermal reaction kettle, maintain 39 DEG C of hydro-thermal reaction 5min, product is through filtering, water washing
To neutrality, it is dried in vacuo 14min in 65 DEG C, -0.06MPa, by product and 37 parts of hydroxyacetic acids, 7.5 parts of lactic acid, 3.9 parts of dense sulphur
Acid and 11.2 parts of phosphorus pentoxides are added in reaction kettle, mixing speed 88r/min, 123 DEG C of maintenance system temperature ,-
React 3.5h under the conditions of 0.07MPa, product through filtering, water washing to neutrality, 67 DEG C, -0.07MPa vacuum drying 10min to get
To hydroxyacetic acid modified polyvinyl chloride；
(4), 88 parts of hydroxyacetic acid modified polyvinyl chlorides, 22 parts of ammonium oxalate, 15 parts of ammonium carbonates and 11 parts of ammonium phosphate are weighed to be added to
In high-speed mixer, with high-speed mixer in 175 DEG C of hybrid reaction 2min of temperature, with extruder in 176 DEG C of extruding pelletizations of temperature,
Obtain modified polyvinyl chloride；
(5), 82 parts of modified polyvinyl chlorides, 41 parts of modified calcium carbonates, 48 parts of modified calcium oxalates are weighed to be added in high-speed mixer,
With high-speed mixer in 179 DEG C of hybrid reaction 3min of temperature, with extruder in 185 DEG C of extruding pelletizations of temperature to get to polychlorostyrene second
Alkenyl wear resistant filler.
Reference examples 1
In this reference examples, modified calcium oxalate is not added, and other components and preparation method are same as Example 1.
Reference examples 2
In this reference examples, modified calcium carbonate is not added, other components and preparation method are same as Example 1.
Reference examples 3
The modification calcium oxalate in common calcium oxalate alternate embodiment 1, other components and preparation side are selected in this reference examples, in formula
Method is same as Example 1.
Reference examples 4
The modified calcium carbonate in ordinary calcium carbonate alternate embodiment 1, other components and preparation side are selected in this reference examples, in formula
Method is same as Example 1.
Reference examples 5
The hydroxyacetic acid modified polyvinyl chloride in common polyvinyl chloride alternate embodiment 1 is selected in this reference examples, in formula, it is other
Component is same as Example 1 with preparation method.
Reference examples 6
The modified polyvinyl chloride in common polyvinyl chloride alternate embodiment 1, other components and system are selected in this reference examples, in formula
Preparation Method is same as Example 1.
The performance parameter of polyvinyl chloride-based wear resistant filler made from 1 embodiment 1 of table and reference examples 1~6
| Embodiment 1 | Reference examples 1 | Reference examples 2 | Reference examples 3 | Reference examples 4 | Reference examples 5 | Reference examples 6 | |
| Thermal coefficient/W/ (m.K) | 0.89 | 0.65 | 0.76 | 0.57 | 0.73 | 0.76 | 0.75 |
| Wearability/turn | 9312 | 6735 | 7312 | 7863 | 7896 | 5549 | 5367 |
The above is the preferred embodiment of the invention, it is noted that for those skilled in the art,
Under the premise of not departing from the inventive principle, several improvements and modifications can also be made, these improvements and modifications are also considered as the hair
Bright protection domain.
Claims (3)
1. a kind of preparation method of polyvinyl chloride-based wear resistant filler, it is characterised in that：Including following raw material components：Modified polyvinyl chloride
Alkene, modified calcium carbonate, modified calcium oxalate, the modified polyvinyl chloride, modified calcium carbonate, the quality parts ratio for being modified calcium oxalate
It is 82：35~44：45~51, wherein the modified polyvinyl chloride is by hydroxyacetic acid modified polyvinyl chloride, ammonium oxalate, carbonic acid
Ammonium and ammonium phosphate reaction are made, the mass fraction of the hydroxyacetic acid modified polyvinyl chloride, ammonium oxalate, ammonium carbonate and ammonium phosphate
Than being 88：17~23：12~18：8~12, the hydroxyacetic acid modified polyvinyl chloride is by polyvinyl chloride, hydroxyacetic acid, breast
Acid, sodium ethoxide, sodium hydrate aqueous solution, the concentrated sulfuric acid and phosphorus pentoxide reaction are made, the polyvinyl chloride, hydroxyacetic acid,
Lactic acid, sodium ethoxide, sodium hydrate aqueous solution, the concentrated sulfuric acid and phosphorus pentoxide quality parts ratio be 83：35~41：5~8：45
~53：39~44：3~5：9~14, the modified calcium carbonate is by calcium chloride, 1- decyl -2,3- methylimidazoles to methylbenzene
Sulfonate, ammonium hydrogen carbonate and ammonium oleate reaction are made, and the calcium chloride, 1- decyls -2,3- methylimidazole are to methylbenzene sulphur
The quality parts ratio of hydrochlorate, ammonium hydrogen carbonate and ammonium oleate is 70：120~134：112~126：9~15, the modification oxalic acid
Calcium is reacted by oxalic acid, calcium stearate, ethyl alcohol, water and 1- butyl -3- methylimidazole dodecane sulfonates to be made, the grass
Acid, calcium stearate, ethyl alcohol, water and 1- butyl -3- methylimidazole dodecane sulfonates quality parts ratio be 10：63~71：
137~151：35~46：95~116.
2. a kind of preparation method of polyvinyl chloride-based wear resistant filler according to claim 1, it is characterised in that：The polychlorostyrene
Vinyl wear resistant filler is made from following preparation method：(1), by oxalic acid, calcium stearate, ethyl alcohol, water and 1- butyl -3- first
Base imidazoles dodecane sulfonate is 10 according to quality parts ratio：63~71：137~151：35~46：95~116 are added to water
In thermal response kettle, 35min is reacted under the conditions of 32~45 DEG C of maintenance system temperature, product washs 3 times, 65 DEG C through 78 DEG C of 1L benzene
500mL ethyl alcohol washs 2 times, is dried in vacuo 20min in 53 DEG C, -0.09MPa, crushes, obtains modified calcium oxalate；(2), by chlorination
Calcium, 1- decyl -2,3- methylimidazoles toluenesulfonate, ammonium hydrogen carbonate and ammonium oleate are 70 according to quality parts ratio：120
~134：112~126：9~15 are added in reaction kettle, and mixing speed is 88~97r/min, maintenance system temperature 93~115
1~3h is reacted under the conditions of DEG C, product is dried in vacuo 11min through 1L ethyl alcohol concussion washing 3 times, in 65 DEG C, -0.07MPa, crushes,
Obtain modified calcium carbonate；(3), by polyvinyl chloride and sodium ethoxide according to quality parts ratio 83：45~53 are added to hydrothermal reaction kettle
In, 35 DEG C of hydro-thermal reaction 8min are maintained, the sodium hydrate aqueous solution that quality parts ratio is 39~44 is added to hydrothermal reaction kettle
In, maintain 39 DEG C of hydro-thermal reaction 5min, product to be dried in vacuo 14min through filtering, water washing to neutrality, in 65 DEG C, -0.06MPa,
It is 35~41 by product and quality parts ratio：5~8：3~5：9~14 hydroxyacetic acid, lactic acid, the concentrated sulfuric acid and phosphorus pentoxide
It is added in reaction kettle, mixing speed is 83~95r/min, anti-under the conditions of 118~131 DEG C of maintenance system temperature, -0.07MPa
Answer 2~4h, product is through filtering, water washing to neutrality, 67 DEG C, -0.07MPa vacuum drying 10min is modified to get to hydroxyacetic acid
Polyvinyl chloride；(4), by hydroxyacetic acid modified polyvinyl chloride, ammonium oxalate, ammonium carbonate and ammonium phosphate according to quality parts ratio 88：17
~23：12~18：8~12 are added in high-speed mixer, with high-speed mixer 173~176 DEG C of hybrid reactions 1 of temperature~
4min, with extruder in 174~177 DEG C of extruding pelletizations of temperature to get to modified polyvinyl chloride；(5), by modified polyvinyl chloride,
Modified calcium carbonate, modified calcium oxalate are according to quality parts ratio 82：35~44：45~51 are added in high-speed mixer, with high speed
Mixing machine in 178~185 DEG C of 1~4min of hybrid reaction of temperature, with extruder 178~187 DEG C of extruding pelletizations of temperature to get to
Polyvinyl chloride-based wear resistant filler.
3. a kind of preparation method of polyvinyl chloride-based wear resistant filler according to claim 2, it is characterised in that：The hydrogen-oxygen
Change sodium water solution a concentration of 12%（wt.%）.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101864123A (en) * | 2010-06-18 | 2010-10-20 | 吉林吉瑞莱板材科技有限公司 | Nano microcrystal wood floor and production method thereof |
| CN103937126A (en) * | 2014-04-30 | 2014-07-23 | 沈阳三普高分子材料有限公司 | Polyvinyl chloride wear-resisting smooth material |
| CN104194194A (en) * | 2014-07-29 | 2014-12-10 | 安徽九子山塑业有限公司 | Special-purpose filler for oxidization-resistant wear-resisting PVC (polyvinyl chloride) tube and preparation method for special-purpose fertilizer |
| CN104194197A (en) * | 2014-07-29 | 2014-12-10 | 安徽九子山塑业有限公司 | Special packing for PVC tube with high wearing resistance and thermal stability and preparation method of special packing |
-
2018
- 2018-02-25 CN CN201810158061.9A patent/CN108329629A/en not_active Withdrawn
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101864123A (en) * | 2010-06-18 | 2010-10-20 | 吉林吉瑞莱板材科技有限公司 | Nano microcrystal wood floor and production method thereof |
| CN103937126A (en) * | 2014-04-30 | 2014-07-23 | 沈阳三普高分子材料有限公司 | Polyvinyl chloride wear-resisting smooth material |
| CN104194194A (en) * | 2014-07-29 | 2014-12-10 | 安徽九子山塑业有限公司 | Special-purpose filler for oxidization-resistant wear-resisting PVC (polyvinyl chloride) tube and preparation method for special-purpose fertilizer |
| CN104194197A (en) * | 2014-07-29 | 2014-12-10 | 安徽九子山塑业有限公司 | Special packing for PVC tube with high wearing resistance and thermal stability and preparation method of special packing |
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