CN101429317B - Nano-PVC modifier and producing method thereof - Google Patents
Nano-PVC modifier and producing method thereof Download PDFInfo
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- CN101429317B CN101429317B CN2008102315161A CN200810231516A CN101429317B CN 101429317 B CN101429317 B CN 101429317B CN 2008102315161 A CN2008102315161 A CN 2008102315161A CN 200810231516 A CN200810231516 A CN 200810231516A CN 101429317 B CN101429317 B CN 101429317B
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Abstract
The invention discloses a nanometer PVC modifier and a method for producing the same. The nanometer PVC modifier comprises the following components in weight percentage: 50 to 70 percent of silicon whisker, 5 to 20 percent of dioctylphthalate, 5 to 20 percent of coupling agent, 5 to 20 percent of dispersing agent, and 5 to 20 percent of PVC resin. The method comprises the following steps: the raw materials are stirred at high speed in a high-speed mixer until the temperature of the materials is raised to between 110 and 140 DEG C, the materials are transferred into a cooling mixer, and the materials are discharged when the temperature is dropped to between 40 and 70 DEG C; the materials are mixed and granulated at a temperature of between 150 and 180 DEG C; and then the materials are ground to obtain the nanometer PVC modifier. The PVC modifier has the advantages of high strength, stable chemical performance, high temperature resistance, good insulativity and low oil absorbing rate, thus the modifier is a functionality-enhanced plasticizing material; and the PVC modifier has high melting point, and the refractoriness of the PVC modifier reaches 1,720 DEG C. The fire resistance and the heat distortion temperature of the PVC product are improved, and the cost of raw materials is lower; and the preparation method has the advantages of simple process, easy operation, less investment, and easy production.
Description
One, technical field:
The present invention relates to a kind of plastic modifier, particularly relate to a kind of nano-PVC modifier and production method thereof.
Two, background technology:
Polyvinyl chloride (PVC) material have good rigidly, intensity height, fire-retardant, corrosion-resistant, electric insulating quality is good, and advantage such as soft or hard is adjustable, but also there are shortcomings such as poor processability, notched Izod impact strength and heat-drawn wire are low, poor heat stability, therefore the PVC plastics are difficult to substitute engineering plastics, this is very limited its application, and this is the technical barrier that existing market need solve.
Anti-impact modifier is a kind of very important auxiliary agent of PVC modification, along with the development of PVC modification technology for many years, PVC develops three big toughened system: CPE (chlorinatedpolyethylene) systems, ACR (esters of acrylic acid) system, EVA (its polymers of ethene-vinyl acetate) system gradually with anti-impact modifier.In recent years, because the appearance of nano material, people have adopted inorganic nano-particle to improve the mechanical property of material.In the prior art, the report that adopts nano-calcium carbonate and other anti-impact modifier to improve the PVC impact property has jointly been arranged.Simultaneously, in the prior art, though also add lime carbonate, it generally be as a kind of additive for reducing cost and improve melt strength etc., rather than in order to improve impact property, and add-on can reduce the impact property of material when big.Though further the effect that nano-calcium carbonate also has part to improve impact property is found in research,, it also must use jointly with other anti-impact modifier.
The patent No. for 02120913.8 patent a kind of PVC is provided the nano level anti-impact modifier, comprise nanometer grade calcium carbonate, water and elastomer latices or longer chain fatty acid, these components mix in common high-speed mixer and get final product.Though when this anti-impact modifier is used for the production of PVC section bar, PVC section bar performance is had certain improvement, but still awaits improving.
Three, summary of the invention:
The technical problem to be solved in the present invention: a kind of intensity height, stable chemical performance, high temperature resistant, nano-PVC modifier and production method thereof that cost is low are provided.
Technical scheme of the present invention:
A kind of nano-PVC modifier is represented with weight percent, contains silicon whisker 50～70%, dioctyl phthalate (DOP) 5～20%, couplant 5～20%, dispersion agent 5～20% and polyvinyl chloride resin 5～20% in the composition.
Silicon whisker 55～65%, dioctyl phthalate (DOP) 5～15%, couplant 5～15%, dispersion agent 5～15% and polyvinyl chloride resin 5～15% in the described composition.
Described couplant is any in stearyl-isopropyl titanate, sec.-propyl two oleic acid acyloxy (dioctyl phosphoric acid acyloxy) titanic acid ester, sec.-propyl three oily acyloxy titanic acid ester and sec.-propyl three (dodecyl benzenesulfonyl) titanic acid ester.
Described dispersion agent is any in ethylene bis stearic acid amide, barium stearate, calcium stearate and the paraffin.
Also contain lime carbonate 5～10% in the described composition.
A kind of preparation method of described nano-PVC modifier, after taking by weighing raw material by prescription, add polyvinyl chloride resin, silicon whisker, dioctyl phthalate (DOP), couplant, dispersion agent in the high-speed mixer successively, high-speed stirring, rise to 110～140 ℃ until temperature of charge, change in the cooling mixing machine when temperature is reduced to 40～70 ℃ discharging over to; Material is dropped into tablets press, at 150～180 ℃ of mixing granulators; Promptly obtain nano-PVC modifier then behind the abrasive dust.
Temperature of charge rises to 120 ℃ in the described high-speed stirring, reduces to 60 ℃ to temperature in cooling mixing machine.
Described couplant is choosing any one kind of them in stearyl-isopropyl titanate, sec.-propyl two oleic acid acyloxy (dioctyl phosphoric acid acyloxy) titanic acid ester, sec.-propyl three oily acyloxy titanic acid ester and sec.-propyl three (dodecyl benzenesulfonyl) titanic acid ester; Described dispersion agent is choosing any one kind of them in ethylene bis stearic acid amide, barium stearate, calcium stearate and the paraffin.
Positive beneficial effect of the present invention:
(1) nano-PVC modifier of the present invention, claim NPG-1 type properties-correcting agent again, be a kind of fiber physique structure functional material, outward appearance is pure white, intensity is high, stable chemical performance, high temperature resistant, good insulating, oil absorbency are low, is functional enhancing, the toughening material that a kind of modifying plastics is used; PVC properties-correcting agent fusing point height of the present invention, refractoriness reaches 1720 ℃, and high temperature is difficult for down decomposing, and has improved the flame retardant resistance and the heat-drawn wire of PVC goods, is mainly used in coloured PVC material.
The performance of nano-PVC modifier is as follows:
| Project | Unit | Numerical value |
| Corpus fibrosum length | μm | 4～20 |
| Tap density | g/cm 2 | 0.78 |
| Color and luster (whiteness) | ％ | ≥94 |
| Oil absorbency | g/100g | 20～30 |
| PH value | 6.80 | |
| Moisture content | ％ | ≤0.3 |
| Refractoriness | ℃ | 1720 |
| Mohs' hardness | 7 |
(2) PVC properties-correcting agent of the present invention has good dispersiveness, can be scattered in fully in the polyvinyl chloride resin system, and than resistance height, water-intake rate is low, can be used safely in aspects such as cable insulation material and circuit; This PVC properties-correcting agent can keep stable performance in various organic solvents and soda acid solvent, improved the ageing resistance of goods, and price has only 1/2～1/3 of staple fibre, can reduce product cost.
(3) the PVC properties-correcting agent of method preparation of the present invention makes an addition in the PVC material, can make goods have good dimensional stability, improves rigidity, toughness, heat resisting temperature and insulativity, improves the cost performance of goods.The common PVC material is along with the adding of calcium powder, and its tensile strength straight line descends, and resistance to impact shock also reduces comparatively fast; And the present invention is having now under the constant situation of PVC material prescription, add 20% left and right sides properties-correcting agent of the present invention and substitute the use of PVC major ingredient, its tensile strength, heatproof, resistance to impact shock all have the raising of 20-30%, particularly the resistance to impact shock of product can improve more than 50%, and raw materials cost can reduce 200-300 unit/ton.
(4) preparation method's technology of PVC properties-correcting agent of the present invention is simple, and easy handling is invested lessly, is easy to go into operation.
Four, embodiment:
Embodiment one, nano-PVC modifier prescription: represent silicon whisker 60%, dioctyl phthalate (DOP) 10%, couplant stearyl-isopropyl titanate 10%, dispersion agent ethylene bis stearic acid amide 10% and polyvinyl chloride resin 10% in the composition with weight percent.
The preparation method of nano-PVC modifier: after taking by weighing raw material by prescription, add in the high-speed mixer successively by polyvinyl chloride resin, silicon whisker, dioctyl phthalate (DOP), couplant, dispersion agent, high-speed stirring, rise to 120 ℃ until temperature of charge, change in the cooling mixing machine and mix, when temperature is reduced to 60 ℃, discharging; Material is dropped into tablets press, at 160 ℃ of mixing granulators; Promptly obtain nano-PVC modifier after dropping into the pulverizing mill abrasive dust then.
The use of nano-PVC modifier:
PVC properties-correcting agent is used for existing P VC goods, and alternative PVC major ingredient uses, and adding proportion is 20～25% of a PVC major ingredient, and this example is 20%, presses PVC batching kneading procedure operation and gets final product.Detailed process is: after PVC major ingredient, the weighing of PVC properties-correcting agent, add the high-speed mixer high speed successively and stir, stop to stir when temperature of charge rises to 120 ℃, change when being stirred to temperature of charge in the cooling mixing machine and being 50 ℃ of left and right sides discharging, standby over to.
Embodiment two, no longer repeat with embodiment one something in common, difference is:
Nano-PVC modifier prescription: silicon whisker 50%, dioctyl phthalate (DOP) 5%, couplant stearyl-isopropyl titanate 20%, dispersion agent ethylene bis stearic acid amide 5% and polyvinyl chloride resin 20%.
The preparation method is: add polyvinyl chloride resin, silicon whisker, dioctyl phthalate (DOP), couplant, dispersion agent in the high-speed mixer successively, rotating speed high-speed stirring with 3000r/min, rise to 110 ℃ until temperature of charge, change in the cooling mixing machine and mix, discharging when temperature is reduced to 40 ℃; At 150 ℃ of mixing granulators; Abrasive dust promptly obtains nano-PVC modifier then.
The use of nano-PVC modifier: different with embodiment one is, PVC properties-correcting agent can add use in addition in PVC goods original formulation, adding proportion is 20% of a PVC goods raw material, PVC properties-correcting agent should be added in raw material cooling and stirring process, and press normal cooling whipping procedure operation and get final product.
Embodiment three, no longer repeat with embodiment one something in common, difference is:
Nano-PVC modifier prescription: silicon whisker 70%, dioctyl phthalate (DOP) 5%, couplant stearyl-isopropyl titanate 5%, dispersion agent ethylene bis stearic acid amide 5% and polyvinyl chloride resin 15%.
The preparation method is: polyvinyl chloride resin, silicon whisker, dioctyl phthalate (DOP), couplant, dispersion agent are added in the high-speed mixer successively, and high-speed stirring rises to 140 ℃ until temperature of charge, changes in the cooling mixing machine and mixes, discharging when temperature is reduced to 70 ℃; At 180 ℃ of mixing granulators; Abrasive dust promptly obtains nano-PVC modifier then.
Embodiment four, no longer repeat with embodiment one something in common, difference is:
Nano-PVC modifier prescription: silicon whisker 55%, dioctyl phthalate (DOP) 15%, couplant stearyl-isopropyl titanate 5%, dispersion agent ethylene bis stearic acid amide 20% and polyvinyl chloride resin 5%.
The preparation method is: polyvinyl chloride resin, silicon whisker, dioctyl phthalate (DOP), couplant, dispersion agent are added the high-speed mixer high speed successively stir, rise to 115 ℃ until temperature of charge, change in the cooling mixing machine and mix, discharging when temperature is reduced to 65 ℃; At 170 ℃ of mixing granulators; Abrasive dust promptly obtains nano-PVC modifier then.
Embodiment five, no longer repeat with embodiment one something in common, difference is:
Nano-PVC modifier prescription: silicon whisker 60%, dioctyl phthalate (DOP) 8%, couplant stearyl-isopropyl titanate 18%, dispersion agent ethylene bis stearic acid amide 8% and polyvinyl chloride resin 6%.
The preparation method is: polyvinyl chloride resin, silicon whisker, dioctyl phthalate (DOP), couplant, dispersion agent are added the high-speed mixer high speed successively stir, rise to 130 ℃ until temperature of charge, change in the cooling mixing machine and mix, discharging when temperature is reduced to 55 ℃; At 170 ℃ of mixing granulators; Abrasive dust promptly obtains nano-PVC modifier then.
Embodiment six, no longer repeat with embodiment one something in common, difference is:
Nano-PVC modifier prescription: silicon whisker 65%, dioctyl phthalate (DOP) 6%, couplant stearyl-isopropyl titanate 5%, dispersion agent ethylene bis stearic acid amide 15% and polyvinyl chloride resin 9%.
The preparation method is: polyvinyl chloride resin, silicon whisker, dioctyl phthalate (DOP), couplant, dispersion agent are added the high-speed mixer high speed successively stir, rise to 125 ℃ until temperature of charge, change in the cooling mixing machine and mix, discharging when temperature is reduced to 55 ℃ is at 175 ℃ of mixing granulators; Abrasive dust promptly obtains nano-PVC modifier then.
Embodiment seven,
Nano-PVC modifier prescription: silicon whisker 68%, dioctyl phthalate (DOP) 7%, couplant stearyl-isopropyl titanate 5%, dispersion agent ethylene bis stearic acid amide 5% and polyvinyl chloride resin 15%.
Embodiment eight,
Nano-PVC modifier prescription: silicon whisker 70%, dioctyl phthalate (DOP) 6%, couplant stearyl-isopropyl titanate 8%, dispersion agent ethylene bis stearic acid amide 6% and polyvinyl chloride resin 10%.
Embodiment nine,
Nano-PVC modifier prescription: silicon whisker 58%, dioctyl phthalate (DOP) 18%, couplant stearyl-isopropyl titanate 7%, dispersion agent ethylene bis stearic acid amide 12% and polyvinyl chloride resin 5%.
Embodiment ten,
Nano-PVC modifier prescription: silicon whisker 65%, dioctyl phthalate (DOP) 16%, couplant stearyl-isopropyl titanate 5%, dispersion agent ethylene bis stearic acid amide 5% and polyvinyl chloride resin 9%.
Embodiment 11,
Nano-PVC modifier prescription: silicon whisker 50%, dioctyl phthalate (DOP) 5%, couplant sec.-propyl two oleic acid acyloxy (dioctyl phosphoric acid acyloxy) titanic acid ester 15%, dispersion agent barium stearate 10% and polyvinyl chloride resin 20%.
Embodiment 12,
Nano-PVC modifier prescription: silicon whisker 50%, dioctyl phthalate (DOP) 20%, couplant sec.-propyl three oily acyloxy titanic acid ester 5%, dispersion agent barium stearate 20% and polyvinyl chloride resin 5%.
Embodiment 13,
Nano-PVC modifier prescription: silicon whisker 60%, dioctyl phthalate (DOP) 17%, couplant sec.-propyl three (dodecyl benzenesulfonyl) titanic acid ester 8%, dispersion agent calcium stearate 8% and polyvinyl chloride resin 7%.
Embodiment 14,
Nano-PVC modifier prescription: silicon whisker 60%, dioctyl phthalate (DOP) 12%, couplant stearyl-isopropyl titanate 6%, dispersion agent calcium stearate 10% and polyvinyl chloride resin 12%.
Embodiment 15,
Nano-PVC modifier prescription: silicon whisker 60%, dioctyl phthalate (DOP) 12%, couplant stearyl-isopropyl titanate 6%, dispersion agent solid paraffin 10%, polyvinyl chloride resin 6%, lime carbonate 6%.
Embodiment 16,
Nano-PVC modifier prescription: silicon whisker 55%, dioctyl phthalate (DOP) 10%, couplant stearyl-isopropyl titanate 10%, dispersion agent solid paraffin 10% and polyvinyl chloride resin 5%, lime carbonate 10%.
Embodiment 17,
Nano-PVC modifier prescription: silicon whisker 60%, dioctyl phthalate (DOP) 10%, couplant stearyl-isopropyl titanate 15%, dispersant liq paraffin 5% and polyvinyl chloride resin 5%, lime carbonate 5%.
Embodiment 18,
Nano-PVC modifier prescription: silicon whisker 65%, dioctyl phthalate (DOP) 8%, couplant stearyl-isopropyl titanate 7%, dispersion agent ethylene bis stearic acid amide 5% and polyvinyl chloride resin 7%, lime carbonate 8%.
Embodiment 19,
Nano-PVC modifier prescription: silicon whisker 60%, dioctyl phthalate (DOP) 5%, couplant sec.-propyl two oleic acid acyloxy (dioctyl phosphoric acid acyloxy) titanic acid ester 5%, dispersion agent barium stearate 14% and polyvinyl chloride resin 10%, lime carbonate 6%.
Embodiment 20,
Nano-PVC modifier prescription: silicon whisker 70%, dioctyl phthalate (DOP) 5%, couplant sec.-propyl three oily acyloxy titanic acid ester 5%, dispersion agent ethylene bis stearic acid amide 5% and polyvinyl chloride resin 10%, lime carbonate 5%.
In embodiment seven～20, the preparation method of nano-PVC modifier is with embodiment one, when in the raw material lime carbonate being arranged and dispersion agent together add high-speed mixer and get final product; Its using method is identical with embodiment one or embodiment two, specifically no longer repeats.
Claims (6)
1. a nano-PVC modifier is characterized in that: represent with weight percent, be made of following composition, silicon whisker 50～70%, dioctyl phthalate (DOP) 5～20%, couplant 5～20%, dispersion agent 5～20% and polyvinyl chloride resin 5～20%; Described couplant is any in stearyl-isopropyl titanate, sec.-propyl two oleic acid acyloxy (dioctyl phosphoric acid acyloxy) titanic acid ester, sec.-propyl three oily acyloxy titanic acid ester and sec.-propyl three (dodecyl benzenesulfonyl) titanic acid ester; Described dispersion agent is any in ethylene bis stearic acid amide, barium stearate, calcium stearate and the paraffin.
2. nano-PVC modifier according to claim 1 is characterized in that: silicon whisker 55～65%, dioctyl phthalate (DOP) 5～15%, couplant 5～15%, dispersion agent 5～15% and polyvinyl chloride resin 5～15% in the described composition.
3. nano-PVC modifier, it is characterized in that: represent with weight percent, constitute silicon whisker 50～70%, dioctyl phthalate (DOP) 5～20%, couplant 5～20%, dispersion agent 5～20% and polyvinyl chloride resin 5～20%, lime carbonate 5～10% by following composition; Described couplant is any in stearyl-isopropyl titanate, sec.-propyl two oleic acid acyloxy (dioctyl phosphoric acid acyloxy) titanic acid ester, sec.-propyl three oily acyloxy titanic acid ester and sec.-propyl three (dodecyl benzenesulfonyl) titanic acid ester; Described dispersion agent is any in ethylene bis stearic acid amide, barium stearate, calcium stearate and the paraffin.
4. the preparation method of the described nano-PVC modifier of claim 1, it is characterized in that: described take by weighing raw material by prescription after, add polyvinyl chloride resin, silicon whisker, dioctyl phthalate (DOP), couplant, dispersion agent in the high-speed mixer successively, high-speed stirring, rise to 110～140 ℃ until temperature of charge, change in the cooling mixing machine when temperature is reduced to 40～70 ℃ discharging over to; Material is dropped into tablets press, at 150～180 ℃ of mixing granulators; Promptly obtain nano-PVC modifier then behind the abrasive dust.
5. the preparation method of nano-PVC modifier according to claim 4, it is characterized in that: temperature of charge rises to 120 ℃ in the described high-speed stirring, reduces to 60 ℃ to temperature in cooling mixing machine.
6. the preparation method of nano-PVC modifier according to claim 4, it is characterized in that: described couplant is any in stearyl-isopropyl titanate, sec.-propyl two oleic acid acyloxy (dioctyl phosphoric acid acyloxy) titanic acid ester, sec.-propyl three oily acyloxy titanic acid ester and sec.-propyl three (dodecyl benzenesulfonyl) titanic acid ester; Described dispersion agent is any in ethylene bis stearic acid amide, barium stearate, calcium stearate and the paraffin.
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| CN2008102315161A CN101429317B (en) | 2008-12-25 | 2008-12-25 | Nano-PVC modifier and producing method thereof |
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| CN101429317B true CN101429317B (en) | 2011-03-30 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102085941A (en) * | 2011-01-10 | 2011-06-08 | 周良文 | Nanometer plastic packing belt |
| CN102719117B (en) * | 2011-12-14 | 2013-12-11 | 内蒙古华生高岭土有限责任公司 | Preparation method of modified aluminum silicate for polyvinyl chloride (PVC) profile |
| CN110665615B (en) * | 2019-10-10 | 2022-04-19 | 青岛瓷兴新材料有限公司 | Preparation method of superfine silicon powder |
| CN111534027A (en) * | 2020-06-17 | 2020-08-14 | 德裕(安徽)科技有限公司 | Modified PVC material with impact resistance |
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