CN107141660A - A kind of fluorescer modified polyvinyl chloride material and preparation method thereof - Google Patents

A kind of fluorescer modified polyvinyl chloride material and preparation method thereof Download PDF

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CN107141660A
CN107141660A CN201710532628.XA CN201710532628A CN107141660A CN 107141660 A CN107141660 A CN 107141660A CN 201710532628 A CN201710532628 A CN 201710532628A CN 107141660 A CN107141660 A CN 107141660A
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周佳瑜
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K13/00Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
    • C08K13/02Organic and inorganic ingredients
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    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B25/00Phosphorus; Compounds thereof
    • C01B25/16Oxyacids of phosphorus; Salts thereof
    • C01B25/26Phosphates
    • C01B25/45Phosphates containing plural metal, or metal and ammonium
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
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    • C08K5/00Use of organic ingredients
    • C08K5/04Oxygen-containing compounds
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    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00Use of organic ingredients
    • C08K5/49Phosphorus-containing compounds
    • C08K5/51Phosphorus bound to oxygen
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    • C09K11/77Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
    • C09K11/7706Aluminates
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    • C09K11/00Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/77Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
    • C09K11/7709Phosphates
    • C09K11/771Phosphates with alkaline earth metals
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/32Phosphorus-containing compounds
    • C08K2003/321Phosphates
    • C08K2003/327Aluminium phosphate

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Abstract

The invention is related to a kind of fluorescer modified polyvinyl chloride material, including following raw material components:Polyvinyl chloride, doped yttrium aluminum phosphate calcium lithium, cerium dopping calcium silicates, triphenylphosphine, anacardol, the different certain herbaceous plants with big flowers ester of pentaerythritol diphosphite two, magnesium stearate, doped yttrium aluminum phosphate calcium lithium is reacted by yttrium acetate, aluminum phosphate calcium lithium, Sr 10 and cetomacrogol 1000 to be made, aluminum phosphate calcium lithium is made by tetrachloro-lithium aluminate, calcium dihydrogen phosphate, aluminium dihydrogen phosphate, polyacrylamide, glycerine and hydroperoxidation, and cerium dopping calcium silicates is reacted by cerous acetate, tetraethyl orthosilicate, calcium formate, water and amylose to be made.The invention has excellent fluorescence property and mechanical property.

Description

A kind of fluorescer modified polyvinyl chloride material and preparation method thereof
Technical field
The invention is related to a kind of fluorescer modified polyvinyl chloride material and preparation method thereof.
Background technology
Igelite is thermoplastic resin prepared by a kind of chloroethylene polymerization, with lightweight, corrosion-resistant, flowing resistance The advantage such as power is small, electric insulating quality is good, is widely used in the fields such as artificial leather, tubing, route protection pipe, film, commodity.
At present, pvc material needs further lifting in fluorescence property and mechanical property.The invention uses polychlorostyrene second Alkene, doped yttrium aluminum phosphate calcium lithium, cerium dopping calcium silicates, triphenylphosphine, anacardol are prepared for fluorescer modified polyvinyl chloride material, Various plastic products, fluorescer modified polyvinyl chloride prepared by this method are prepared into by techniques such as extrusion, injection, molding, blowings Alkene material has excellent fluorescence property and mechanical property.
The content of the invention
The purpose of the invention is to provide a kind of preparation method of fluorescer modified polyvinyl chloride material, and this method is by changing Become reactant feed and technology mode, the material of preparation has excellent fluorescence property and mechanical property.
To achieve these goals, the technical scheme of the invention is as follows.
A kind of fluorescer modified polyvinyl chloride material and preparation method thereof, specifically includes following steps:(1), by cerous acetate, Tetraethyl orthosilicate, calcium formate, water and amylose are 5 according to quality parts ratio:125~140:78~88:90~100:30~ 40 are added in reactor, and mixing speed is 75~92r/min, and reaction 0.5 under the conditions of 55~65 DEG C of maintenance system temperature~ 0.8h, product obtains cerium dopping silicon through 300 DEG C of roasting 2h, 400 DEG C of roasting 2h, 500 DEG C of roasting 2h, 600 DEG C of roasting 2h, grinding Sour calcium;(2), by tetrachloro-lithium aluminate, calcium dihydrogen phosphate, aluminium dihydrogen phosphate, polyacrylamide, glycerine and hydrogen peroxide according to quality Portion rate 10:25~35:75~90:9~15:12~18:15~20 are added in reactor, and mixing speed is 95~125r/ Under the conditions of min, 60~75 DEG C of maintenance system temperature react 0.5~1h, product through 100 DEG C, -0.07MPa vacuum distillation 0.5h, 300 DEG C of roasting 2h, 400 DEG C of roasting 2h, 500 DEG C of roasting 2h, 600 DEG C of roasting 2h, grinding obtains aluminum phosphate calcium lithium;(3), by second Sour yttrium, aluminum phosphate calcium lithium, Sr-10 and cetomacrogol 1000 are according to quality parts ratio 3:100~125:10~20:12~18 add Into reactor, mixing speed is 0.3~0.7h of reaction, production under the conditions of 45~65r/min, 80~95 DEG C of maintenance system temperature Thing obtains yttrium through 300 DEG C of roasting 2h, 400 DEG C of roasting 2h, 500 DEG C of roasting 2h, 600 DEG C of roasting 2h, 700 DEG C of roasting 2h, grinding Doping phosphoric acid aluminium calcium lithium;(4), by polyvinyl chloride, doped yttrium aluminum phosphate calcium lithium, cerium dopping calcium silicates, triphenylphosphine, anacardol, The different certain herbaceous plants with big flowers ester of pentaerythritol diphosphite two, magnesium stearate are according to quality parts ratio 100:1~5:2~6:18~33:35~50: 3~7:4~10 are added in mill, with mill in 150~180 DEG C of 0.1~0.5h of hybrid reaction of temperature, are existed with extruder 151~185 DEG C of extruding pelletizations of temperature, that is, obtain fluorescer modified polyvinyl chloride material.
The preparation method of fluorescer modified polyvinyl chloride material described in the invention, comprises the following steps:
(1) it is, 5 according to quality parts ratio by cerous acetate, tetraethyl orthosilicate, calcium formate, water and amylose:125~140:78 ~88:90~100:30~40 are added in reactor, and mixing speed is 75~92r/min, 55~65 DEG C of maintenance system temperature Under the conditions of react 0.5~0.8h, product through 300 DEG C roasting 2h, 400 DEG C roasting 2h, 500 DEG C roasting 2h, 600 DEG C roasting 2h, grind Mill, obtains cerium dopping calcium silicates;The purpose of described calcium formate is in order to accelerate the hydrolysis of tetraethyl orthosilicate;Described amylose Purpose in order to improve the dispersiveness of raw material.
(2), by tetrachloro-lithium aluminate, calcium dihydrogen phosphate, aluminium dihydrogen phosphate, polyacrylamide, glycerine and hydrogen peroxide according to Quality parts ratio 10:25~35:75~90:9~15:12~18:15~20 are added in reactor, mixing speed be 95~ 0.5~1h is reacted under the conditions of 125r/min, 60~75 DEG C of maintenance system temperature, product is through 100 DEG C, -0.07MPa vacuum distillations 0.5h, 300 DEG C of roasting 2h, 400 DEG C of roasting 2h, 500 DEG C of roasting 2h, 600 DEG C of roasting 2h, grinding obtains aluminum phosphate calcium lithium;It is described Tetrachloro-lithium aluminate purpose in order to provide silicon source and lithium source, while accelerate hydrogen peroxide hydrolysis rate.
(3), by yttrium acetate, aluminum phosphate calcium lithium, Sr-10 and cetomacrogol 1000 according to quality parts ratio 3:100~125: 10~20:12~18 are added in reactor, and mixing speed is 45~65r/min, under the conditions of 80~95 DEG C of maintenance system temperature 0.3~0.7h is reacted, product is through 300 DEG C of roastings 2h, 400 DEG C of roastings 2h, 500 DEG C of roastings 2h, 600 DEG C of roasting 2h, 700 DEG C of roastings 2h, grinding, that is, obtain doped yttrium aluminum phosphate calcium lithium;Described Sr-10 purpose is in order to improve the mixing uniformity of raw material.
(4), by polyvinyl chloride, doped yttrium aluminum phosphate calcium lithium, cerium dopping calcium silicates, triphenylphosphine, anacardol, diphosphorous acid The different certain herbaceous plants with big flowers ester of pentaerythritol ester two, magnesium stearate are according to quality parts ratio 100:1~5:2~6:18~33:35~50:3~7:4~ 10 are added in mill, with mill in 150~180 DEG C of 0.1~0.5h of hybrid reaction of temperature, with extruder in temperature 151 ~185 DEG C of extruding pelletizations, that is, obtain fluorescer modified polyvinyl chloride material;Described triphenylphosphine and the purpose of anacardol in order to Improve the mechanical strength of polyvinyl chloride.
The beneficial effect of the invention is:
1st, calcium formate has reproducibility, when heated, and calcium formate decomposes generation calcium oxide, and calcium oxide can accelerate tetraethyl orthosilicate Hydrolysis, under the booster action of amylose, cerium dopping calcium silicates is prepared through high-temperature roasting;Cerium dopping calcium silicates can improve poly- The fluorescence property of vinyl chloride;
2nd, tetrachloro-lithium aluminate has acidity, can accelerate the decomposition of hydrogen peroxide, and the water that hydrogen peroxide decomposes generation can promote four again The hydrolysis of chlorine lithium aluminate, under polyacrylamide booster action, aluminum phosphate calcium lithium is prepared through high-temperature roasting;
3rd, Sr-10 has chemical reactivity, can improve dispersiveness and wetability of the yttrium acetate in material, improves yttrium in phosphoric acid The dispersiveness on aluminium calcium lithium surface;Doped yttrium aluminum phosphate calcium lithium can improve the fluorescence property of polyvinyl chloride;
4th, triphenylphosphine and anacardol can react generation three-dimensional net structure, can improve the mechanical property of polyvinyl chloride.
Embodiment
The embodiment of the invention is described with reference to embodiment, to be better understood from the invention.
Embodiment 1
A kind of fluorescer modified polyvinyl chloride material, its preparation method comprises the following steps:
(1) 5 parts of cerous acetates, 130 parts of tetraethyl orthosilicates, 82 parts of calcium formates, 93 parts of water and 36 portions of amyloses, are weighed to be added to instead Answer in device, mixing speed is that 0.7h is reacted under the conditions of 82r/min, 59 DEG C of maintenance system temperature, product through 300 DEG C of roasting 2h, 400 DEG C of roasting 2h, 500 DEG C of roasting 2h, 600 DEG C of roasting 2h, grinding obtains cerium dopping calcium silicates;
(2), weigh 10 parts of tetrachloro-lithium aluminates, 33 parts of calcium dihydrogen phosphates, 82 parts of aluminium dihydrogen phosphates, 12 parts of polyacrylamides, 16 parts Glycerine and 18 parts of hydrogen peroxide are added in reactor, and mixing speed is anti-under the conditions of 115r/min, 68 DEG C of maintenance system temperature 0.7h is answered, product is through 100 DEG C, -0.07MPa vacuum distillations 0.5h, 300 DEG C of roastings 2h, 400 DEG C of roasting 2h, and 500 DEG C are calcined 2h, 600 DEG C of roasting 2h, grinding obtains aluminum phosphate calcium lithium;
(3) 3 parts of yttrium acetates, 109 parts of aluminum phosphate calcium lithiums, 17 parts of Sr-10 and 15 part of cetomacrogol 1000s, are weighed and are added to reactor In, mixing speed is that 0.5h is reacted under the conditions of 60r/min, 85 DEG C of maintenance system temperature, and product is through 300 DEG C of roasting 2h, 400 DEG C 2h is calcined, 500 DEG C of roasting 2h, 600 DEG C of roasting 2h, 700 DEG C of roasting 2h, grinding obtains doped yttrium aluminum phosphate calcium lithium;
(4) 100 parts of polyvinyl chloride, 2 parts of doped yttrium aluminum phosphate calcium lithiums, 4 parts of cerium dopping calcium silicates, 23 parts of triphenylphosphines, 43, are weighed Part anacardol, the different certain herbaceous plants with big flowers ester of 5 parts of pentaerythritol diphosphites two, 7 parts of magnesium stearates are added in mill, with mill in temperature 158 DEG C of hybrid reaction 0.3h are spent, with extruder in 168 DEG C of extruding pelletizations of temperature, that is, fluorescer modified polyvinyl chloride material are obtained.
Embodiment 2
A kind of fluorescer modified polyvinyl chloride material, its preparation method comprises the following steps:
(1) 5 parts of cerous acetates, 125 parts of tetraethyl orthosilicates, 78 parts of calcium formates, 90 parts of water and 30 portions of amyloses, are weighed to be added to instead Answer in device, mixing speed is that 0.5h is reacted under the conditions of 75r/min, 55 DEG C of maintenance system temperature, product through 300 DEG C of roasting 2h, 400 DEG C of roasting 2h, 500 DEG C of roasting 2h, 600 DEG C of roasting 2h, grinding obtains cerium dopping calcium silicates;
(2), weigh 10 parts of tetrachloro-lithium aluminates, 25 parts of calcium dihydrogen phosphates, 75 parts of aluminium dihydrogen phosphates, 9 parts of polyacrylamides, 12 parts it is sweet Oil and 15 parts of hydrogen peroxide are added in reactor, and mixing speed is reaction under the conditions of 95r/min, 60 DEG C of maintenance system temperature 0.5h, product is through 100 DEG C, -0.07MPa vacuum distillations 0.5h, 300 DEG C of roastings 2h, 400 DEG C of roasting 2h, and 500 DEG C are calcined 2h, 600 DEG C roasting 2h, grinding, obtain aluminum phosphate calcium lithium;
(3) 3 parts of yttrium acetates, 100 parts of aluminum phosphate calcium lithiums, 10 parts of Sr-10 and 12 part of cetomacrogol 1000s, are weighed and are added to reactor In, mixing speed is that 0.3h is reacted under the conditions of 45r/min, 80 DEG C of maintenance system temperature, and product is through 300 DEG C of roasting 2h, 400 DEG C 2h is calcined, 500 DEG C of roasting 2h, 600 DEG C of roasting 2h, 700 DEG C of roasting 2h, grinding obtains doped yttrium aluminum phosphate calcium lithium;
(4) 100 parts of polyvinyl chloride, 1 part of doped yttrium aluminum phosphate calcium lithium, 2 parts of cerium dopping calcium silicates, 18 parts of triphenylphosphines, 35, are weighed Part anacardol, the different certain herbaceous plants with big flowers ester of 3 parts of pentaerythritol diphosphites two, 4 parts of magnesium stearates are added in mill, with mill in temperature 180 DEG C of hybrid reaction 0.1h are spent, with extruder in 185 DEG C of extruding pelletizations of temperature, that is, fluorescer modified polyvinyl chloride material are obtained.
Embodiment 3
A kind of fluorescer modified polyvinyl chloride material, its preparation method comprises the following steps:
(1) 5 parts of cerous acetates, 140 parts of tetraethyl orthosilicates, 88 parts of calcium formates, 100 parts of water and 40 portions of amyloses, are weighed to be added to In reactor, mixing speed is that 0.8h is reacted under the conditions of 92r/min, 65 DEG C of maintenance system temperature, product through 300 DEG C of roasting 2h, 400 DEG C of roasting 2h, 500 DEG C of roasting 2h, 600 DEG C of roasting 2h, grinding obtains cerium dopping calcium silicates;
(2), weigh 10 parts of tetrachloro-lithium aluminates, 35 parts of calcium dihydrogen phosphates, 90 parts of aluminium dihydrogen phosphates, 15 parts of polyacrylamides, 18 parts Glycerine and 20 parts of hydrogen peroxide are added in reactor, and mixing speed is anti-under the conditions of 125r/min, 75 DEG C of maintenance system temperature 1h is answered, product is through 100 DEG C, -0.07MPa vacuum distillations 0.5h, 300 DEG C of roastings 2h, 400 DEG C of roasting 2h, and 500 DEG C are calcined 2h, 600 DEG C roasting 2h, grinding, obtain aluminum phosphate calcium lithium;
(3) 3 parts of yttrium acetates, 125 parts of aluminum phosphate calcium lithiums, 20 parts of Sr-10 and 18 part of cetomacrogol 1000s, are weighed and are added to reactor In, mixing speed is that 0.7h is reacted under the conditions of 65r/min, 95 DEG C of maintenance system temperature, and product is through 300 DEG C of roasting 2h, 400 DEG C 2h is calcined, 500 DEG C of roasting 2h, 600 DEG C of roasting 2h, 700 DEG C of roasting 2h, grinding obtains doped yttrium aluminum phosphate calcium lithium;
(4) 100 parts of polyvinyl chloride, 5 parts of doped yttrium aluminum phosphate calcium lithiums, 6 parts of cerium dopping calcium silicates, 33 parts of triphenylphosphines, 50, are weighed Part anacardol, the different certain herbaceous plants with big flowers ester of 7 parts of pentaerythritol diphosphites two, 10 parts of magnesium stearates are added in mill, are existed with mill 150 DEG C of hybrid reaction 0.5h of temperature, with extruder in 151 DEG C of extruding pelletizations of temperature, that is, obtain fluorescer modified polyvinyl chloride material Material.
Embodiment 4
A kind of fluorescer modified polyvinyl chloride material, its preparation method comprises the following steps:
(1) 5 parts of cerous acetates, 130 parts of tetraethyl orthosilicates, 80 parts of calcium formates, 95 parts of water and 36 portions of amyloses, are weighed to be added to instead Answer in device, mixing speed is that 0.6h is reacted under the conditions of 80r/min, 60 DEG C of maintenance system temperature, product through 300 DEG C of roasting 2h, 400 DEG C of roasting 2h, 500 DEG C of roasting 2h, 600 DEG C of roasting 2h, grinding obtains cerium dopping calcium silicates;
(2), weigh 10 parts of tetrachloro-lithium aluminates, 30 parts of calcium dihydrogen phosphates, 80 parts of aluminium dihydrogen phosphates, 12 parts of polyacrylamides, 15 parts Glycerine and 17 parts of hydrogen peroxide are added in reactor, and mixing speed is anti-under the conditions of 100r/min, maintenance system temperature 70 C 0.7h is answered, product is through 100 DEG C, -0.07MPa vacuum distillations 0.5h, 300 DEG C of roastings 2h, 400 DEG C of roasting 2h, and 500 DEG C are calcined 2h, 600 DEG C of roasting 2h, grinding obtains aluminum phosphate calcium lithium;
(3) 3 parts of yttrium acetates, 110 parts of aluminum phosphate calcium lithiums, 15 parts of Sr-10 and 14 part of cetomacrogol 1000s, are weighed and are added to reactor In, mixing speed is that 0.6h is reacted under the conditions of 55r/min, 85 DEG C of maintenance system temperature, and product is through 300 DEG C of roasting 2h, 400 DEG C 2h is calcined, 500 DEG C of roasting 2h, 600 DEG C of roasting 2h, 700 DEG C of roasting 2h, grinding obtains doped yttrium aluminum phosphate calcium lithium;
(4) 100 parts of polyvinyl chloride, 3 parts of doped yttrium aluminum phosphate calcium lithiums, 5 parts of cerium dopping calcium silicates, 20 parts of triphenylphosphines, 40, are weighed Part anacardol, the different certain herbaceous plants with big flowers ester of 4 parts of pentaerythritol diphosphites two, 5 parts of magnesium stearates are added in mill, with mill in temperature 155 DEG C of hybrid reaction 0.4h are spent, with extruder in 160 DEG C of extruding pelletizations of temperature, that is, fluorescer modified polyvinyl chloride material are obtained.
Embodiment 5
A kind of fluorescer modified polyvinyl chloride material, its preparation method comprises the following steps:
(1) 5 parts of cerous acetates, 135 parts of tetraethyl orthosilicates, 85 parts of calcium formates, 96 parts of water and 33 portions of amyloses, are weighed to be added to instead Answer in device, mixing speed is that 0.7h is reacted under the conditions of 78r/min, 57 DEG C of maintenance system temperature, product through 300 DEG C of roasting 2h, 400 DEG C of roasting 2h, 500 DEG C of roasting 2h, 600 DEG C of roasting 2h, grinding obtains cerium dopping calcium silicates;
(2), weigh 10 parts of tetrachloro-lithium aluminates, 28 parts of calcium dihydrogen phosphates, 79 parts of aluminium dihydrogen phosphates, 10 parts of polyacrylamides, 13 parts Glycerine and 19 parts of hydrogen peroxide are added in reactor, and mixing speed is anti-under the conditions of 98r/min, 73 DEG C of maintenance system temperature 0.7h is answered, product is through 100 DEG C, -0.07MPa vacuum distillations 0.5h, 300 DEG C of roastings 2h, 400 DEG C of roasting 2h, and 500 DEG C are calcined 2h, 600 DEG C of roasting 2h, grinding obtains aluminum phosphate calcium lithium;
(3) 3 parts of yttrium acetates, 109 parts of aluminum phosphate calcium lithiums, 14 parts of Sr-10 and 16 part of cetomacrogol 1000s, are weighed and are added to reactor In, mixing speed is that 0.5h is reacted under the conditions of 49r/min, 83 DEG C of maintenance system temperature, and product is through 300 DEG C of roasting 2h, 400 DEG C 2h is calcined, 500 DEG C of roasting 2h, 600 DEG C of roasting 2h, 700 DEG C of roasting 2h, grinding obtains doped yttrium aluminum phosphate calcium lithium;
(4) 100 parts of polyvinyl chloride, 2 parts of doped yttrium aluminum phosphate calcium lithiums, 5 parts of cerium dopping calcium silicates, 19 parts of triphenylphosphines, 43, are weighed Part anacardol, the different certain herbaceous plants with big flowers ester of 5 parts of pentaerythritol diphosphites two, 7 parts of magnesium stearates are added in mill, with mill in temperature 160 DEG C of hybrid reaction 0.4h are spent, with extruder in 169 DEG C of extruding pelletizations of temperature, that is, fluorescer modified polyvinyl chloride material are obtained.
Embodiment 6
A kind of fluorescer modified polyvinyl chloride material, its preparation method comprises the following steps:
(1) 5 parts of cerous acetates, 129 parts of tetraethyl orthosilicates, 83 parts of calcium formates, 94 parts of water and 32 portions of amyloses, are weighed to be added to instead Answer in device, mixing speed is that 0.7h is reacted under the conditions of 90r/min, 64 DEG C of maintenance system temperature, product through 300 DEG C of roasting 2h, 400 DEG C of roasting 2h, 500 DEG C of roasting 2h, 600 DEG C of roasting 2h, grinding obtains cerium dopping calcium silicates;
(2), weigh 10 parts of tetrachloro-lithium aluminates, 33 parts of calcium dihydrogen phosphates, 88 parts of aluminium dihydrogen phosphates, 12 parts of polyacrylamides, 17 parts Glycerine and 19 parts of hydrogen peroxide are added in reactor, and mixing speed is anti-under the conditions of 120r/min, 67 DEG C of maintenance system temperature 0.6h is answered, product is through 100 DEG C, -0.07MPa vacuum distillations 0.5h, 300 DEG C of roastings 2h, 400 DEG C of roasting 2h, and 500 DEG C are calcined 2h, 600 DEG C of roasting 2h, grinding obtains aluminum phosphate calcium lithium;
(3) 3 parts of yttrium acetates, 115 parts of aluminum phosphate calcium lithiums, 19 parts of Sr-10 and 15 part of cetomacrogol 1000s, are weighed and are added to reactor In, mixing speed is that 0.4h is reacted under the conditions of 63r/min, 91 DEG C of maintenance system temperature, and product is through 300 DEG C of roasting 2h, 400 DEG C 2h is calcined, 500 DEG C of roasting 2h, 600 DEG C of roasting 2h, 700 DEG C of roasting 2h, grinding obtains doped yttrium aluminum phosphate calcium lithium;
(4) 100 parts of polyvinyl chloride, 4 parts of doped yttrium aluminum phosphate calcium lithiums, 4 parts of cerium dopping calcium silicates, 31 parts of triphenylphosphines, 46, are weighed Part anacardol, the different certain herbaceous plants with big flowers ester of 5 parts of pentaerythritol diphosphites two, 8 parts of magnesium stearates are added in mill, with mill in temperature 165 DEG C of hybrid reaction 0.3h are spent, with extruder in 172 DEG C of extruding pelletizations of temperature, that is, fluorescer modified polyvinyl chloride material are obtained.
Embodiment 7
A kind of fluorescer modified polyvinyl chloride material, its preparation method comprises the following steps:
(1) 5 parts of cerous acetates, 139 parts of tetraethyl orthosilicates, 86 parts of calcium formates, 97 parts of water and 38 portions of amyloses, are weighed to be added to instead Answer in device, mixing speed is that 0.7h is reacted under the conditions of 83r/min, 61 DEG C of maintenance system temperature, product through 300 DEG C of roasting 2h, 400 DEG C of roasting 2h, 500 DEG C of roasting 2h, 600 DEG C of roasting 2h, grinding obtains cerium dopping calcium silicates;
(2), weigh 10 parts of tetrachloro-lithium aluminates, 32 parts of calcium dihydrogen phosphates, 86 parts of aluminium dihydrogen phosphates, 14 parts of polyacrylamides, 17 parts Glycerine and 19 parts of hydrogen peroxide are added in reactor, and mixing speed is anti-under the conditions of 123r/min, 71 DEG C of maintenance system temperature 0.8h is answered, product is through 100 DEG C, -0.07MPa vacuum distillations 0.5h, 300 DEG C of roastings 2h, 400 DEG C of roasting 2h, and 500 DEG C are calcined 2h, 600 DEG C of roasting 2h, grinding obtains aluminum phosphate calcium lithium;
(3) 3 parts of yttrium acetates, 118 parts of aluminum phosphate calcium lithiums, 13 parts of Sr-10 and 16 part of cetomacrogol 1000s, are weighed and are added to reactor In, mixing speed is that 0.6h is reacted under the conditions of 56r/min, 89 DEG C of maintenance system temperature, and product is through 300 DEG C of roasting 2h, 400 DEG C 2h is calcined, 500 DEG C of roasting 2h, 600 DEG C of roasting 2h, 700 DEG C of roasting 2h, grinding obtains doped yttrium aluminum phosphate calcium lithium;
(4) 100 parts of polyvinyl chloride, 3 parts of doped yttrium aluminum phosphate calcium lithiums, 5 parts of cerium dopping calcium silicates, 28 parts of triphenylphosphines, 46, are weighed Part anacardol, the different certain herbaceous plants with big flowers ester of 4 parts of pentaerythritol diphosphites two, 8 parts of magnesium stearates are added in mill, with mill in temperature 170 DEG C of hybrid reaction 0.3h are spent, with extruder in 175 DEG C of extruding pelletizations of temperature, that is, fluorescer modified polyvinyl chloride material are obtained.
Embodiment 8
A kind of fluorescer modified polyvinyl chloride material, its preparation method comprises the following steps:
(1) 5 parts of cerous acetates, 137 parts of tetraethyl orthosilicates, 79 parts of calcium formates, 98 parts of water and 34 portions of amyloses, are weighed to be added to instead Answer in device, mixing speed is that 0.6h is reacted under the conditions of 87r/min, 61 DEG C of maintenance system temperature, product through 300 DEG C of roasting 2h, 400 DEG C of roasting 2h, 500 DEG C of roasting 2h, 600 DEG C of roasting 2h, grinding obtains cerium dopping calcium silicates;
(2), weigh 10 parts of tetrachloro-lithium aluminates, 33 parts of calcium dihydrogen phosphates, 88 parts of aluminium dihydrogen phosphates, 13 parts of polyacrylamides, 17 parts Glycerine and 19 parts of hydrogen peroxide are added in reactor, and mixing speed is anti-under the conditions of 117r/min, 71 DEG C of maintenance system temperature 0.8h is answered, product is through 100 DEG C, -0.07MPa vacuum distillations 0.5h, 300 DEG C of roastings 2h, 400 DEG C of roasting 2h, and 500 DEG C are calcined 2h, 600 DEG C of roasting 2h, grinding obtains aluminum phosphate calcium lithium;
(3) 3 parts of yttrium acetates, 119 parts of aluminum phosphate calcium lithiums, 16 parts of Sr-10 and 17 part of cetomacrogol 1000s, are weighed and are added to reactor In, mixing speed is that 0.4h is reacted under the conditions of 53r/min, 92 DEG C of maintenance system temperature, and product is through 300 DEG C of roasting 2h, 400 DEG C 2h is calcined, 500 DEG C of roasting 2h, 600 DEG C of roasting 2h, 700 DEG C of roasting 2h, grinding obtains doped yttrium aluminum phosphate calcium lithium;
(4) 100 parts of polyvinyl chloride, 4 parts of doped yttrium aluminum phosphate calcium lithiums, 3 parts of cerium dopping calcium silicates, 26 parts of triphenylphosphines, 43, are weighed Part anacardol, the different certain herbaceous plants with big flowers ester of 6 parts of pentaerythritol diphosphites two, 9 parts of magnesium stearates are added in mill, with mill in temperature 173 DEG C of hybrid reaction 0.2h are spent, with extruder in 178 DEG C of extruding pelletizations of temperature, that is, fluorescer modified polyvinyl chloride material are obtained.
Reference examples 1
In this reference examples, without cerium dopping calcium silicates, other components and preparation method are same as Example 1.
Reference examples 2
In this reference examples, without doped yttrium aluminum phosphate calcium lithium, other components and preparation method are same as Example 1.
Reference examples 3
In this reference examples, without triphenylphosphine, other components and preparation method are same as Example 1.
Reference examples 4
In this reference examples, without anacardol, other components and preparation method are same as Example 1.
Reference examples 5
In this reference examples, the cerium dopping calcium silicates selected in formula in common cerium dopping calcium silicates alternate embodiment 1, other components It is same as Example 1 with preparation method.
Reference examples 6
In this reference examples, from the aluminum phosphate calcium lithium in aluminum phosphate calcium lithium alternate embodiment 1 in formula, other components and preparation side Method is same as Example 1.
The performance parameter of fluorescer modified polyvinyl chloride material made from the embodiment 1 of table 1 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
Fluorescence exciting wavelength/nm 430 468 576 435 432 451 498
Tensile strength/MPa 53 52 51 38 40 52 51
Described above is the preferred embodiment of the invention, it is noted that for those skilled in the art, On the premise of the inventive principle is not departed from, some improvements and modifications can also be made, these improvements and modifications are also considered as the hair Bright protection domain.

Claims (2)

1. a kind of preparation method of fluorescer modified polyvinyl chloride material, it is characterised in that:Including following raw material components:Polychlorostyrene second Alkene, doped yttrium aluminum phosphate calcium lithium, cerium dopping calcium silicates, triphenylphosphine, anacardol, the different certain herbaceous plants with big flowers ester of pentaerythritol diphosphite two, Magnesium stearate, described polyvinyl chloride, doped yttrium aluminum phosphate calcium lithium, cerium dopping calcium silicates, triphenylphosphine, anacardol, two phosphorous The sour different certain herbaceous plants with big flowers ester of pentaerythritol ester two, the quality parts ratio of magnesium stearate are 100:1~5:2~6:18~33:35~50:3~7:4 ~10, wherein, described doped yttrium aluminum phosphate calcium lithium is reacted by yttrium acetate, aluminum phosphate calcium lithium, Sr-10 and cetomacrogol 1000 to be made , described yttrium acetate, aluminum phosphate calcium lithium, the quality parts ratio of Sr-10 and cetomacrogol 1000 are 3:100~125:10~ 20:12~18, described aluminum phosphate calcium lithium is by tetrachloro-lithium aluminate, calcium dihydrogen phosphate, aluminium dihydrogen phosphate, polyacrylamide, glycerine It is made with hydroperoxidation, described tetrachloro-lithium aluminate, calcium dihydrogen phosphate, aluminium dihydrogen phosphate, polyacrylamide, glycerine and mistake The quality parts ratio of hydrogen oxide is 10:25~35:75~90:9~15:12~18:15~20, described cerium dopping calcium silicates by Cerous acetate, tetraethyl orthosilicate, calcium formate, water and amylose reaction are made, described cerous acetate, tetraethyl orthosilicate, calcium formate, The quality parts ratio of water and amylose is 5:125~140:78~88:90~100:30~40.
2. a kind of preparation method of fluorescer modified polyvinyl chloride material according to claim 1, it is characterised in that:Described Fluorescer modified polyvinyl chloride material is as made from following preparation method:(1), by cerous acetate, tetraethyl orthosilicate, calcium formate, Water and amylose are 5 according to quality parts ratio:125~140:78~88:90~100:30~40 are added in reactor, stir Speed is mixed for 75~92r/min, 0.5~0.8h is reacted under the conditions of 55~65 DEG C of maintenance system temperature, product is through 300 DEG C of roastings 2h, 400 DEG C of roasting 2h, 500 DEG C of roasting 2h, 600 DEG C of roasting 2h, grinding obtains cerium dopping calcium silicates;(2), by tetrachloro aluminic acid Lithium, calcium dihydrogen phosphate, aluminium dihydrogen phosphate, polyacrylamide, glycerine and hydrogen peroxide are according to quality parts ratio 10:25~35:75 ~90:9~15:12~18:15~20 are added in reactor, and mixing speed is 95~125r/min, maintenance system temperature 60 0.5~1h is reacted under the conditions of~75 DEG C, product is through 100 DEG C, -0.07MPa vacuum distillations 0.5h, 300 DEG C of roasting 2h, 400 DEG C of roastings 2h is burnt, 500 DEG C of roasting 2h, 600 DEG C of roasting 2h, grinding obtains aluminum phosphate calcium lithium;(3), by yttrium acetate, aluminum phosphate calcium lithium, Sr- 10 and cetomacrogol 1000 according to quality parts ratio 3:100~125:10~20:12~18 are added in reactor, mixing speed For 45~65r/min, 0.3~0.7h is reacted under the conditions of 80~95 DEG C of maintenance system temperature, product is through 300 DEG C of roasting 2h, 400 DEG C roasting 2h, 500 DEG C roasting 2h, 600 DEG C roasting 2h, 700 DEG C roasting 2h, grinding, that is, obtain doped yttrium aluminum phosphate calcium lithium;(4)、 By polyvinyl chloride, doped yttrium aluminum phosphate calcium lithium, cerium dopping calcium silicates, triphenylphosphine, anacardol, pentaerythritol diphosphite two Different certain herbaceous plants with big flowers ester, magnesium stearate are according to quality parts ratio 100:1~5:2~6:18~33:35~50:3~7:4~10 are added to mill In machine, with mill in 150~180 DEG C of 0.1~0.5h of hybrid reaction of temperature, made with extruder in 151~185 DEG C of extrusions of temperature Grain, that is, obtain fluorescer modified polyvinyl chloride material.
CN201710532628.XA 2017-07-03 2017-07-03 A kind of fluorescer modified polyvinyl chloride material and preparation method thereof Pending CN107141660A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101475803A (en) * 2009-01-19 2009-07-08 上海富顺单向透视材料有限公司 Self-luminescent material and preparation thereof
CN104098850A (en) * 2014-06-18 2014-10-15 安徽省振云塑胶有限公司 Anti-impact PVC water supply pipe and preparation method thereof
CN105255048A (en) * 2015-10-30 2016-01-20 永高股份有限公司 Preparation method of high-performance environment-friendly U-PVC (unplasticized-polyvinyl chloride) pipe

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101475803A (en) * 2009-01-19 2009-07-08 上海富顺单向透视材料有限公司 Self-luminescent material and preparation thereof
CN104098850A (en) * 2014-06-18 2014-10-15 安徽省振云塑胶有限公司 Anti-impact PVC water supply pipe and preparation method thereof
CN105255048A (en) * 2015-10-30 2016-01-20 永高股份有限公司 Preparation method of high-performance environment-friendly U-PVC (unplasticized-polyvinyl chloride) pipe

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