CN102051007A - Soft polrvinyl chloride composition and preparation method thereof - Google Patents
Soft polrvinyl chloride composition and preparation method thereof Download PDFInfo
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- CN102051007A CN102051007A CN2009102366577A CN200910236657A CN102051007A CN 102051007 A CN102051007 A CN 102051007A CN 2009102366577 A CN2009102366577 A CN 2009102366577A CN 200910236657 A CN200910236657 A CN 200910236657A CN 102051007 A CN102051007 A CN 102051007A
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Abstract
The invention provides a soft polrvinyl chloride composition, which comprises the following components: polyvinyl chloride resin, powdered rubber with a cross-linked structure, a dispersant, a plasticizer and fly ash. Based on the weight of polyvinyl chloride resin, the soft polrvinyl chloride composition comprises 100 parts of polyvinyl chloride resin, 30 to 50 parts of powdered rubber with the cross-linked structure, 0.5 to 3.0 parts of dispersant, 50 to 100 parts of plasticizer and 5 to 50 parts of fly ash. The soft polrvinyl chloride composition provided by the invention has outstanding temperature resistance and higher tensile strength and elongation, can be used as sinks of temperature-resistance cables and coating material for special metal pipes, and can be widely used in many fields such as electronic, machinery, chemical and instrument fields.
Description
Technical field
The present invention relates to a kind of polyvinyl chloride, say further, relate to a kind of soft polyvinyl chloride composition and preparation method thereof.
Background technology
Polyvinyl chloride (PVC) is that a kind of output is big, purposes wide, the general-purpose plastics of high comprehensive performance, and soft PVC is as the big class of one in the polyvinyl chloride, and Application Areas is extensive.The outstanding advantage of soft PVC goods is flame retardancy, oil-proofness, wear resistance, resistance to chemical corrosion, gas steam low-permeability.Comprehensive mechanical performance, goods properties of transparency, electrical insulating property, heat insulation, noise elimination in addition, damping property are also relatively good, are the very superior versatility materials of the ratio of performance to price.But have defectives such as thermostability, tensile property difference because of it, limited PVC and be widely used at many special dimensions as coating material of heat-resisting cable crust or metal pipe material etc.
Normally modification obtains common soft polyvinyl chloride to polyvinyl chloride resin by processing aid based on softening agent (as DOP or DBP etc.), as Chinese patent CN 1004759B.But have following shortcoming when using as common soft pvc: (1) softening agent moves easily and makes it hardening; (2) winter hardiness is poor; (3) poor dimensional stability; (4) solvent-proof extracting is poor.
In order to overcome the deficiency of ordinary soft polyvinyl chloride resin, document (technical journal " polyvinyl chloride " is arranged, 43～45 pages of 2000 the 6th phases, 49 pages, " Study on powder NBR modifying soft PVC ") report uses Powdered acrylonitrile-butadiene rubber to come the modified soft polyvinyl chloride resin, is used for improving the oil resistant of soft polyvinyl chloride, cold-resistant, wear-resisting and shock resistance etc.The employed Powdered acrylonitrile-butadiene rubber of the document is that the trade mark that U.S. Goodyear company produces is the Chemigum P83 Powdered acrylonitrile-butadiene rubber of (being called for short P83).The U.S. Pat 5,739,203, US 5,840,236, the US6 that are applied for as Goodyear company, disclosed in 054,524, this kind Powdered acrylonitrile-butadiene rubber gets through free-radical emulsion polymerization.Emulsion after the polymerization can obtain a kind of granulous cross-linked powdery acrylonitrile butadiene through flocculating and adding an amount of separant (as lime carbonate, Zinic stearas, calcium stearate or polyvinyl chloride resin etc.).Its particle diameter is not more than 250 μ m, preferably is not more than 150 μ m, more preferably no more than 100 μ m.In the polymerization process of this Powdered acrylonitrile-butadiene rubber, added linking agent, so the Powdered acrylonitrile-butadiene rubber of gained has higher degree of crosslinking.
In the patent that above-mentioned Goodyear company is applied for, be that this kind Powdered acrylonitrile-butadiene rubber is mixed with the common plasticizers of PVC earlier, mix with the PVC paste again, make a kind of acrylic sol composition.Said composition can be made the hollow rubber goods by the forming method of hollow blow molding, as gloves, shoes, boots etc.Also said composition is flooded some moulding product, form by methods such as oven dry again and be coated with the outer field goods of plastic cement.In these were used, this kind powdered rubber had improved the performances such as anti-solvent transport property, slip resistance and low temperature elasticity that pasted the plastisol that is equipped with by PVC.
The disclosed technology of above-mentioned document " Study on powder NBR modifying soft PVC " then is to utilize this kind powder NBR modifying soft PVC resin, though its oil-proofness and anti-solvent transport property are improved, but because the particle diameter of this Powdered acrylonitrile-butadiene rubber is bigger, resulting modified effect is very not remarkable, still needs to improve.And this kind Powdered acrylonitrile-butadiene rubber is owing to utilize synthesis method preparation, complex process, and control condition requires high, so the preparation cost of particle own is very high, thereby makes that the cost of the polyvinyl chloride that uses its modification is also very high.
Summary of the invention
For solving problems of the prior art, the present invention replaces pearl filler commonly used in the PVC processing with flyash, can obviously improve the ageing-resistant performance of material, and can improve flowability, the heat conductivility of material to a certain extent.
The purpose of this invention is to provide a kind of novel soft polyvinyl chloride composition.Another object of the present invention provides the preparation method of this kind soft polyvinyl chloride composition.
Soft polyvinyl chloride composition of the present invention includes the following component of blend: polyvinyl chloride (PVC) RESINS, the powdered rubber with crosslinking structure, dispersion agent, softening agent, flyash.
In the soft polyvinyl chloride composition of the present invention, the polymerization degree of polyvinyl chloride (PVC) RESINS is more than or equal to 1000.
In the soft polyvinyl chloride composition of the present invention, powdered rubber with crosslinking structure is that average particle size range is at 20～200nm, preferred 30～120nm, more preferably 50～100nm, gel content is counted 60% weight or higher with weight ratio, preferred 80% weight or higher, rubber particles is preferably equal phase structure.Described powdered rubber is preferably carboxyl butyronitrile powdered rubber, powder nbr rubber or its mixing.Described powdered rubber with crosslinking structure also can be the mixing of above-mentioned fully vulcanized powder rubber and cross-linked powdered rubber.Among the present invention, the add-on of powdered rubber is lower, can reduce cost.In polyvinyl chloride is that 100 parts by weight powdered rubber content are 3～50 parts, is preferably 15～30 parts by weight.
Described powdered rubber with crosslinking structure is to be selected from the prepared fully vulcanized powder rubber of submitting on December 3rd, 1999 according to the applicant of Chinese patent application 99125530.5 (International Patent Application Publication No. is WO 01/40356), comprises full sulfuration carboxyl butyronitrile powdered rubber or vulcanizes powder nbr rubber entirely.This kind fully vulcanized powder rubber is by in rubber latex, behind the adding crosslinking coagent, carries out radiation vulcanization, and obtain after spray-dried.Be to need not with separant or extraordinary stablizer after a kind of drying or do special stabilizing treatment to get final product the rubber micro mist that unrestricted flow is difficult for adhesion.Variation to some extent is preferably 60% weight or higher to the gel content of this fully vulcanized powder rubber according to irradiation dose is different, and more excellent is 75% weight or higher.The median size of should full sulfuration carboxyl butyronitrile powdered rubber or vulcanizing powder nbr rubber entirely is 20～200nm, preferred 30～120nm, more preferably 50～100nm.Each particulate in this fully vulcanized powder rubber all is a homogeneous, and promptly single particulate all is a homogeneous on forming, and does not find layering in the particulate under the observation of existing microtechnique, divides the phenomenon that equates uneven phase.This kind fully vulcanized powder rubber preparation technology is comparatively easy, so this kind powdered rubber preparation cost is lower.This kind powdered rubber also can be buied by the China Petrochemical Industry Beijing Chemical Research Institute at present.
In the soft polyvinyl chloride composition of the present invention, dispersion agent is that carbonatoms is 10～20, one or more in preferred 12～18 the stearylamide; Perhaps dispersion agent is that described stearylamide and carbonatoms are 3～20, is preferably the mixture of 8～18 fatty acid alkyl ester, and wherein the carbonatoms of alkyl is 3～10; In stearylamide is 100 weight parts, and the content of fatty acid alkyl ester is 0～30 part, is preferably 5～20 parts, more preferably 10～20 parts.Described dispersion agent can make powdered rubber in polyvinyl chloride resin with uniform, rough class spheroidal particle form homodisperse.Thereby can be good at improving the tensile strength and the elongation at break of polyvinyl chloride resin, have good comprehensive performances simultaneously.With polyvinyl chloride is that the total consumption of 100 parts by weight score powder is 0.5～3 part, is preferably 1.0～2.0 parts by weight.
In the soft polyvinyl chloride composition of the present invention, particle size range 1250 orders of flyash are to 2500 orders.Can obviously improve the ageing-resistant performance of material with pearl filler commonly used in coal ash instead this area, and improve the performances such as flowability, thermal conductivity of material to a certain extent.In polyvinyl chloride is that the total consumption of 100 parts by weight flyash is 5～50 parts, is preferably 15～30 parts by weight.
Softening agent in the polychloroethylene composition of the present invention is a plasticizer for polyvinyl chloride general in the prior art, preferred triisooctyl trimellitate TOTM, Di Iso Decyl Phthalate DIDP, dioctyl phthalate (DOP) DOP, among dibutyl phthalate DBP, the dioctyl sebacate DOS one or more, its consumption is that 100 weight parts are counted 50～100 parts with polyvinyl chloride usually, is preferably 50～80 weight parts.
Soft polyvinyl chloride composition of the present invention also comprises acrylic acid ester class (ACR) modifier that general being used in the existing polyvinyl chloride processing technology improves the PVC processing characteristics.Its consumption is a conventional amount used, is 100 weight in polyvinyl chloride resin generally, can be 5～15 parts.
The present invention also includes stablizer general in the polyvinyl chloride processing technology, as: organic tin, barium zinc class or lead salts stablizer, its consumption are conventional amount used.The consumption of lead salts stablizer is that 100 weight parts can be preferred 5～15 parts in polyvinyl chloride resin.
In addition, can also include polyvinyl chloride processing lubricant (as: polyethylene wax, oxidic polyethylene etc.), tinting material and other processing aid etc. commonly used in the prior art in the polychloroethylene composition of the present invention.Its consumption is conventional amount used, or adjusts according to practical situation.
The preparation method of soft polyvinyl chloride composition of the present invention is polychloroethylene composition preparation method commonly used in this area, comprise described component is mixed in proportion, extrude or step such as injection by melt blending, make the soft polyvinyl chloride composition goods.Used melt temperature is the common melt processing temperature of polyvinyl chloride, and used processing units also is an industry common equipment.As: high-speed mixer, single screw extrusion machine, injector etc.
Soft polyvinyl chloride composition of the present invention has higher draw tensile strength, elongation at break and better heat-resisting and flowability, remedied the deficiency of aspects such as low in the prior art, poor heat resistance, had wide range of applications in preparation soft PVC materials tensile strength.
Embodiment
Below in conjunction with embodiment, further specify the present invention.
Embodiment 1～2
With polyvinyl chloride (PVC) RESINS (Beijing chemical industry two factories, trade mark SG-2, mean polymerisation degree is 1350～1434) put into the low speed mixer stirring with, ACR modifier (Japanese Wu Yu chemical company, trade mark KM355P), TOTM (productions of Shandong, Shandong softening agent factory), barium zinc stabilizer (Beijing Chemical Factory No. 3's productions), flyash (commercially available) and cool off.To room temperature, ((Beijing Chemical Research Institute produces the form of finely divided powder, mehtod paracril to add full sulfuration carboxyl butyronitrile powdered rubber, the trade mark is VP401, gel content is more than 83% weight, after particle diameter is 80～110nm), dispersion agent (self-control) mixes, again through mixing plasticizing of open mixing roll and following sheet.Melting temperature is: 165 ℃ of preliminary rollers, 163 ℃ on back roller.Behind 185 ℃ of compressing tablets, make the standard batten by tabletting machine again, carry out various Mechanics Performance Testings.Concrete prescription sees Table 1, and wherein each component concentration is all in parts by weight.Testing standard and results of property are shown in table 1, table 2.
The dispersion agent preparation: with N, the two ethylene group stearylamides (wherein the carbonatoms of stearylamide is 12, and is commercially available), 2 of N, 2,2-trimethylammonium 1, (U.S. Yi Si Man produces the 3-pentanediol diisobutyrate, trade mark TXIB) fully stirs, mix and obtain mixture.Wherein with N, the two ethylene group stearylamides of N are 100 parts by weight meters, 2,2, and 2-trimethylammonium 1,3-pentanediol diisobutyrate are 17 parts.
Comparative example 1
In addition, all the other compositions and preparation condition are all identical with embodiment 1 except that the form of finely divided powder, mehtod paracril being replaced to Powdered acrylonitrile-butadiene rubber (U.S. Goodyear company produces trade mark P83, median size 0.5mm).Concrete prescription and batten test result are as shown in table 1.
Comparative example 2～3
With polyvinyl chloride (PVC) RESINS (Beijing chemical industry two factories, trade mark SG-2, mean polymerisation degree is 1350～1434) with, ACR modifier (Japanese Wu Yu chemical company, trade mark KM355P), TOTM (production of Shandong, Shandong softening agent factory), barium zinc stabilizer (Beijing Chemical Factory No. 3's production), water-ground limestone (the inferior lime carbonate in Shen, Shanghai factory produces 1250 orders), put into that low speed mixer stirs and cooling.To room temperature, after adding Powdered acrylonitrile-butadiene rubber (U.S. Goodyear company produces trade mark P83, median size 0.5mm), dispersion agent (self-control is with embodiment 1) mix, again through mixing plasticizing of open mixing roll and following sheet.Melting temperature is: 165 ℃ of preliminary rollers, 163 ℃ on back roller.Behind 185 ℃ of compressing tablets, make the standard batten by tabletting machine again, carry out various Mechanics Performance Testings.Concrete prescription sees Table 1, and wherein each component concentration is all in parts by weight.Testing standard and results of property are shown in table 1, table 2.
The test result of embodiment and comparative example sees Table 1
Tensile strength and elongation at break conservation rate test condition are 100 ℃ of x 240 hours;
The temperature tolerance test is under 170 ℃, and PVC material space clad metal takes place by the isolating time.
Table 1 test result
Numerical value in the clump table as can be seen, the temperature tolerance of embodiment 1 and embodiment 2 has had with respect to comparative example and has significantly improved, tensile strength and elongation also are improved to some extent simultaneously.
Claims (10)
1. soft polyvinyl chloride composition includes the following component of blend:
Described PVC resin polymerization degree is more than or equal to 1000;
Described powdered rubber with crosslinking structure is equal phase structure, and average particle size range is at 20～200nm, and gel content is counted 60% weight or higher with weight ratio;
The particle size range of described flyash is 1250 orders～2500 orders;
Described dispersion agent is that carbonatoms is one or more in 10～20 the stearylamide; Perhaps described dispersion agent is that carbonatoms is that 10～20 stearylamide and carbonatoms are the mixture of 3～20 fatty alkyl ester, and wherein the carbonatoms of alkyl is 3～10; In described stearylamide is 100 weight parts, and the content of described fatty acid alkyl ester is 0～30 part.
2. soft polyvinyl chloride composition as claimed in claim 1 is characterized in that including the following component of blend:
3. soft polyvinyl chloride composition as claimed in claim 1 is characterized in that: described have the powdered rubber average particle size range of crosslinking structure at 30～120nm.
4. soft polyvinyl chloride composition as claimed in claim 3 is characterized in that: described powdered rubber average particle size range with crosslinking structure is at 50～100nm, and gel content is counted 80% weight or higher with weight ratio.
5. soft polyvinyl chloride composition as claimed in claim 1 is characterized in that: described powdered rubber with crosslinking structure is carboxyl butyronitrile powdered rubber, powder nbr rubber or its combination.
6. soft polyvinyl chloride composition as claimed in claim 1 is characterized in that: described stearylamide carbonatoms is 12～18; The carbonatoms of described fatty alkyl ester is 8～18.
7. soft polyvinyl chloride composition as claimed in claim 1 is characterized in that: in described stearylamide is 100 weight parts, and the content of described fatty acid alkyl ester is 5～20 parts.
8. soft polyvinyl chloride composition as claimed in claim 7 is characterized in that: in described stearylamide is 100 weight parts, and the content of described fatty acid alkyl ester is 10～20 parts.
9. soft polyvinyl chloride composition as claimed in claim 1, it is characterized in that: described softening agent is triisooctyl trimellitate TOTM, Di Iso Decyl Phthalate DIDP, dioctyl phthalate (DOP) DOP, one or more among dibutyl phthalate DBP, the dioctyl sebacate DOS.
10. each described soft polyvinyl chloride preparation of compositions method according to claim 1～9, be to include above-described powdered rubber with crosslinking structure, softening agent, flyash, dispersion agent, and make soft polyvinyl chloride composition at interior component and described polyvinyl chloride resin melt blending.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102964724A (en) * | 2012-11-27 | 2013-03-13 | 宁波一舟塑胶有限公司 | Thin-wall insulated wire material for automobile and preparation method thereof |
| CN103346519A (en) * | 2013-07-23 | 2013-10-09 | 上海远洲管业有限公司 | Abrasion-resistant anti-impact multi-hole cable protective pipe and preparing method thereof |
| CN104250411A (en) * | 2014-01-26 | 2014-12-31 | 安徽省忠宏管业科技有限公司 | PVC hose |
| CN105153502A (en) * | 2015-07-16 | 2015-12-16 | 安徽华宇电缆集团有限公司 | Special oil-resistant and heat-resistant cable for offshore oil platform |
| CN105524481A (en) * | 2016-01-22 | 2016-04-27 | 安徽环宇电缆集团有限公司 | Formula for cable sheath |
| CN106496874A (en) * | 2016-11-18 | 2017-03-15 | 威海市麦特瑞奥科技发展有限公司 | Modified coal ash filled PVC foamed building material and its template |
| CN109251443A (en) * | 2018-09-15 | 2019-01-22 | 漯河科莱堡洁具配件有限公司 | The modified spiral winded PVC hose and preparation method thereof that eliminates the unusual smell of sanitary ware superfined flyash |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102964724A (en) * | 2012-11-27 | 2013-03-13 | 宁波一舟塑胶有限公司 | Thin-wall insulated wire material for automobile and preparation method thereof |
| CN102964724B (en) * | 2012-11-27 | 2015-01-14 | 宁波一舟塑胶有限公司 | Thin-wall insulated wire material for automobile and preparation method thereof |
| CN103346519A (en) * | 2013-07-23 | 2013-10-09 | 上海远洲管业有限公司 | Abrasion-resistant anti-impact multi-hole cable protective pipe and preparing method thereof |
| CN103346519B (en) * | 2013-07-23 | 2016-01-27 | 上海远洲管业有限公司 | A kind of wear-resisting anti-impact perforated lines cable protection tubing and preparation method thereof |
| CN104250411A (en) * | 2014-01-26 | 2014-12-31 | 安徽省忠宏管业科技有限公司 | PVC hose |
| CN105153502A (en) * | 2015-07-16 | 2015-12-16 | 安徽华宇电缆集团有限公司 | Special oil-resistant and heat-resistant cable for offshore oil platform |
| CN105524481A (en) * | 2016-01-22 | 2016-04-27 | 安徽环宇电缆集团有限公司 | Formula for cable sheath |
| CN106496874A (en) * | 2016-11-18 | 2017-03-15 | 威海市麦特瑞奥科技发展有限公司 | Modified coal ash filled PVC foamed building material and its template |
| CN109251443A (en) * | 2018-09-15 | 2019-01-22 | 漯河科莱堡洁具配件有限公司 | The modified spiral winded PVC hose and preparation method thereof that eliminates the unusual smell of sanitary ware superfined flyash |
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