CN100348658C - Hard polyvinyl chloride composition and its preparation method - Google Patents
Hard polyvinyl chloride composition and its preparation method Download PDFInfo
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- CN100348658C CN100348658C CNB2004100862917A CN200410086291A CN100348658C CN 100348658 C CN100348658 C CN 100348658C CN B2004100862917 A CNB2004100862917 A CN B2004100862917A CN 200410086291 A CN200410086291 A CN 200410086291A CN 100348658 C CN100348658 C CN 100348658C
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Abstract
The present invention provides a hard polyvinyl chloride composition and a preparation method thereof, which belongs to the field of hard polyvinyl chloride. The polyvinyl chloride composition contains powdered rubber with the gel content of at least 60%, dispersing agents and polyvinyl chloride resin which are blended, wherein the average grain size of the powdered rubber is from 20 nm to 200 nm, and the powdered rubber has a crosslinked structure. The dispersing agents contain stearamide with 3 to 20 carbon atoms. The polymerization degree of the polyvinyl chloride resin is greater than or equal to 700. When the polyvinyl chloride resin is measured by 100 parts by weight, the content of the powdered rubber is 3 to 30 parts, and the content of the dispersing agents is 0.5 to 3.0 parts. Components containing the matters are melted and blended to prepare the hard polyvinyl chloride composition. The hard polyvinyl chloride composition has the advantages of high fracture elongation rate, impact resistant performance, favorable rigidity and thermodynamic performance. The hard polyvinyl chloride can be used for preparing sectional materials to be favorably used in the fields of plastic doors and windows, pipe materials, etc. The preparation method of the hard polyvinyl chloride composition has simple process and easy operation, and is suitable for industrialized application.
Description
Technical field
The present invention relates to a kind of polychloroethylene composition, further, relate to a kind of hard 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 rigid polyvinyl chloride has very big Application Areas as a big class of polyvinyl chloride.The outstanding advantage of hard polrvinyl chloride product is flame retardancy, wear resistance, resistance to chemical corrosion, the low seepage excellence of gas steam.Comprehensive mechanical performance, the goods transparency, electrical insulating property, heat insulation, noise elimination in addition, weakening are also better, are the most superior versatility materials of the ratio of performance to price.Its shortcoming is that thermostability, tensile property, shock resistance are relatively poor.The notched Izod impact strength of pure rigid polyvinyl chloride has only 3～5KJ/m
2, elongation at break is also very low, belongs to hard and fragile material.Because hard pvc usually is used to prepare section bar, its these shortcomings cause the anti-bending of its prepared section bar and processibility bad.The mode of blending and modifyings such as general both at home and abroad at present employing adding ACR class (esters of acrylic acid) modifier, chlorinated polyethylene resin (CPE), paracril, Powdered acrylonitrile-butadiene rubber (trade mark that U.S. Goodyear company produces is Chemigum P83, and its median size is about 0.5mm), grafting ethylene-propylene rubber(EPR) improves the shock resistance and the elongation at break of hard PVC material.But though ACR class properties-correcting agent and CPE resin can improve the impact property and the elongation at break of hard PVC material to a certain extent, effect can't be satisfactory.Providing a kind of as U.S. Pat 67068151 has improved shock strength and has had certain inflexible hard PVC matrix material.The main body composition of this invention is polyvinyl chloride resin, ethylene/olefin interpolymers, cl content chlorinated alkenes multipolymer, the lime carbonate at 20-40%.Though but the adding of rubber-like can significantly promote above two performances of polyvinyl chloride resin, but make the heat-drawn wire of material and rigidity descend more.
Summary of the invention
In order to remedy prior art in the deficiency aspect the modified hard polyethylene chloride, the inventor finds after deliberation, the use particle diameter is very little, and (20～200nm) powdered rubber comes modified hard polyethylene chloride, and cooperate certain dispersion agent, make it homodisperse in polyvinyl chloride resin, can be in the toughening PVC resin loss aspect rigidity (flexural strength, modulus in flexure), thermomechanical property very little.
Therefore, the invention provides a kind of hard polyvinyl chloride composition of modification, it has high elongation at break, impact property, has rigidity and thermomechanical property preferably simultaneously.
The present invention also provides the preparation method of the hard polyvinyl chloride composition of above-mentioned modification.
Polychloroethylene composition of the present invention is a kind of hard polyvinyl chloride composition, includes the following component of blend: polyvinyl chloride (PVC) RESINS, the powdered rubber with crosslinking structure and dispersion agent.Be 100 weight parts in polyvinyl chloride (PVC) RESINS wherein, powdered rubber content is 3～30 parts, is preferably 3～15 parts, more preferably 3～10 parts; Dispersant is 0.5～3.0 part, is preferably 1～1.5 part.
In the hard polyvinyl chloride composition of the present invention, described polyvinyl chloride (PVC) RESINS is the polymerization degree more than or equal to 700 polyvinyl chloride (PVC) RESINS.
In the hard polyvinyl chloride composition of the present invention, described dispersion agent is that carbonatoms is 10～20, is preferably in 12～18 the stearylamide one or more; Perhaps dispersion agent is that described stearylamide and carbonatoms are 3～20, is preferably 4～12, the mixture of 4～8 effective for treatment of premature ejaculation more preferably, and wherein the carbonatoms of alkyl is 3～10.In stearylamide is 100 parts by weight, and the content of fatty acid alkyl ester is 0～30 part, is preferably 5～20 parts, more preferably 10～20 parts.This kind dispersion agent can make powdered rubber in polyvinyl chloride resin with uniform, rough class spheroidal particle form homodisperse.Thereby can be good at improving elongation at break and the impact property of PVC, have good comprehensive performances simultaneously.
The powdered rubber that has crosslinking structure in the hard polyvinyl chloride composition of the present invention, for median size at 20～200nm, gel content is counted 60% weight or higher powdered rubber with weight ratio.Its rubber particles is preferably equal phase structure.The median size of this kind powdered rubber is for being preferably 30nm～120nm, 50nm～100nm more preferably, preferred 80% weight of its gel content or higher.This kind powdered rubber is preferably carboxyl butyronitrile powdered rubber, powder nbr rubber or its mixing.
Described powdered rubber with crosslinking structure can adopt according to the inventor in the prepared fully vulcanized powder rubber of the Chinese patent ZL00816450.9 of on September 18th, 2000 application (is right of priority with Chinese patent application 99125530.5, priority date on December 3rd, 1999).Be preferably a kind of or its mixing in form of finely divided powder, mehtod paracril, the form of finely divided powder, mehtod carboxy nitrile rubber.This kind fully vulcanized powder rubber gel content reaches 60% weight or higher, need not after the drying to get final product unrestricted flow with separant.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 fully vulcanized powder rubber gets by to the rubber latex cross-linking radiation rubber particles particle diameter being fixed.So the particle diameter of latex particle is consistent substantially in its median size and the rubber latex, the size scope of the latex particle that described rubber latex obtains when synthetic is the particle size range of gained fully vulcanized powder rubber particle, be generally 20～2000nm, preferred 30～1500nm, more preferably 50～500nm.
The above powdered rubber with crosslinking structure can also adopt the prepared cross-linked powdered rubber of Chinese patent ZL00130386.4 in application on November 3rd, 2000 according to the applicant.Be preferably a kind of or its mixing in cross-linked powdery acrylonitrile butadiene, the cross-linked powdery carboxy nitrile rubber.This kind cross-linked powdered rubber is a kind ofly (to have some rubber latexs between the rubber molecule certain cross can take place in the synthetic process with cross-linking type synthetic rubber latex, thereby make resulting rubber latex have certain crosslinking degree, be referred to as crosslinking-type rubber latex) be raw material, the powdered rubber that drying obtains.The particle diameter of latex particle is consistent substantially in its median size and the crosslinking-type rubber latex, and the size scope of the latex particle that crosslinking-type rubber latex obtains when synthetic is the particle size range of gained cross-linked powdered rubber particle, is generally 50～300nm.This cross-linked powdered rubber need not add separant and get final product unrestricted flow.Its gel content is consistent with gel content as the cross-linking type synthetic rubber latex of raw material, is 80% weight or higher, is preferably 85% weight or higher.Each particulate in this cross-linked powdered 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.
Described powdered rubber with crosslinking structure also can be the mixing of the above fully vulcanized powder rubber and cross-linked powdered rubber.
Hard polyvinyl chloride composition of the present invention also comprises ACR class (esters of acrylic acid) 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 that 100 weight parts can be 5～15 weight parts in polyvinyl chloride resin generally.
Hard polyvinyl chloride composition of the present invention also comprises general stablizer in the existing polyvinyl chloride processing technology, comprises organic tin, barium zinc class or lead salts stablizer.Its consumption is a conventional amount used.The consumption of lead salts stablizer can be that 100 weight parts are counted 5～15 weight parts with polyvinyl chloride resin preferably in the present invention.
In addition, can also include common used lubricant (as Ployethylene Wax, oxidic polyethylene etc.), mineral filler, tinting material and other processing aid etc. of polyvinyl chloride processing in the prior art in the polychloroethylene composition of the present invention.Its consumption is conventional amount used, or adjusts according to practical requirements.
The preparation method of hard polyvinyl chloride composition of the present invention comprises and will include described polyvinyl chloride (PVC) RESINS, have the step of component by melt blending of powdered rubber, the dispersion agent of crosslinking structure, and makes hard polyvinyl chloride composition.
Polyvinyl chloride (PVC) RESINS described in the inventive method is the polymerization degree more than or equal to 700 polyvinyl chloride (PVC) RESINS.
Dispersion agent described in the method for the present invention is that described dispersion agent is that carbonatoms is 10～20, is preferably in 12～18 the stearylamide one or more; Perhaps dispersion agent is that described stearylamide and carbonatoms are 3～20, is preferably 4～12, the mixture of 4～8 effective for treatment of premature ejaculation more preferably, and wherein the carbonatoms of alkyl is 3～10.In stearylamide is 100 parts by weight, and the content of fatty acid alkyl ester is 0～30 part, is preferably 5～20 parts, more preferably 10～20 parts.
At the powdered rubber with crosslinking structure described in the aforesaid method is median size 20～200m, is preferably 30～120nm, more preferably the powdered rubber of 50～100nm.Its gel content is 60% weight or higher, is preferably 80% weight or higher.The rubber particles of this kind powdered rubber is preferably equal phase structure.(with Chinese patent application 99125530.5 is right of priority to the powdered rubber with crosslinking structure described in the inventive method Chinese patent ZL00816450.9 preferred above-mentioned, that the inventor applied on September 18th, 2000, priority date on December 3rd, 1999) cross-linked powdered rubber that the fully vulcanized powder rubber that is provided, and/or the inventor is provided in the Chinese patent ZL00130386.4 of application on November 3rd, 2000.
Also comprise ACR class modifier general in the existing polyvinyl chloride processing technology in the preparation method's of the present invention component, its consumption is a conventional amount used, is that 100 weight parts can be 5～15 weight parts in polyvinyl chloride resin generally.
Also comprise general stablizer in the existing polyvinyl chloride processing technology in the preparation method's of the present invention component, comprise organic tin, barium zinc class or lead salts stablizer.Its consumption is a conventional amount used.The consumption of lead salts stablizer can be that 100 weight parts are counted 5～15 weight parts with polyvinyl chloride resin preferably in the present invention.
In preparation process, the blending temperature of material is the common processing temperature of polyvinyl chloride, should select not only guaranteeing the complete fusion of polyvinyl chloride but also can not make in the scope of its decomposition, generally at 165～220 ℃, is preferably 175～190 ℃.In addition, according to the processing needs, can in the blend material, add conventional auxiliary agent such as lubricant (as Ployethylene Wax, oxidic polyethylene etc.), mineral filler, tinting material and other processing aid etc. of polyvinyl chloride processing in right amount.Its consumption is conventional amount used, or adjusts according to practical requirements.
Employed melt blending equipment can be disclosed mill, Banbury mixer, single screw extrusion machine or twin screw extruder etc. in the rubber plastic blend technology among this preparation method.
The present invention adopts and is adding the small particle size powdered rubber and cooperating the method for dispersion agent to come modified hard PVC.Lose on the very little basis at flexural strength, modulus in flexure, heat-drawn wire, Vicat softening point, make the elongation at break of hard PVC matrix material improve nearly 4 times, and have good impact property.Hard pvc of the present invention can be applicable to profiled material, can solve profiled material in bad phenomenon such as turning white of occurring often of bending process, necking down, distortion.This material also can be applicable to fields such as plastic door-window and tubing simultaneously.Preparation method's technology of the present composition is simple, easy handling, is suitable for industrial applications.
Embodiment
Further describe the present invention below in conjunction with embodiment.Scope of the present invention is not subjected to the restriction of these embodiment, and scope of the present invention proposes in claims.
Embodiment 1～2:
(chemical industry two groups of factory in Beijing produce with polyvinyl chloride resin, the trade mark is SG-5, five types, the polymerization degree is 800), complex lead salt stabilizer (consonance chemical plant, Nanjing), ACR modifier (Japanese Wu Yu chemical company, trade mark KM355P), water-ground limestone (the inferior lime carbonate in Shen, Shanghai factory produces 1250 orders) in high-speed stirring down to mixing.(Beijing Chemical Research Institute produces, and the trade mark is VP401, and gel content is more than 83% weight, and particle diameter is 80～110nm), dispersion agent (self-control) stirs to add the form of finely divided powder, mehtod paracril again.Concrete prescription sees Table 1.Adopt two roller mill mixings, melting temperature is 170-180 ℃.Through compression molding instrument compressing tablet, the compressing tablet temperature is 190-210 ℃.Be processed into test bars through milling machine, carry out the test of various mechanical properties, its result is as shown in table 1.
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:
Except that not adding the form of finely divided powder, mehtod paracril, all the other compositions and preparation condition are all identical with embodiment 1.Concrete prescription and batten test result are as shown in table 1.
Comparative example 2～3:
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.
Table 1
| Embodiment 1 | Comparative example 1 | Comparative example 2 | Comparative example 3 | Embodiment 2 | Unit | Testing standard | |
| PVC | 100 | 100 | 100 | 100 | 100 | - | - |
| ACR | 9 | 9 | 9 | 9 | 9 | - | - |
| One package stabilizer | 5 | 5 | 5 | 5 | 5 | - | - |
| Water-ground limestone | 13 | 13 | 13 | 13 | 13 | - | - |
| VP401 | 3 | 0 | 0 | 0 | 8 | - | - |
| P83 | 0 | 0 | 3 | 15 | 0 | - | - |
| Dispersion agent | 1.0 | 1.0 | 1.0 | 1.0 | 1.0 | - | - |
| Tensile strength | 41.2 | 42.3 | 44.7 | 40.7 | 40.7 | MPa | GB/T1040-1992 |
| Elongation at break | 49 | 10 | 12 | 22 | 52 | ％ | GB/T1040-1992 |
| Izod shock strength (23 ℃) | 12.8 | 10.7 | 8.42 | 7.96 | 13.9 | KJ/m 2 | GB/T1843-1996 |
| Flexural strength | 56.5 | 66.2 | 64.8 | 56.6 | 53.4 | MPa | GB/T9341-2000 |
| The bending amount of touching | 2.34 | 2.68 | 2.51 | 2.24 | 2.30 | GPa | GB/T9341-2000 |
| Thermal denaturation temperature | 75.8 | 77.5 | 76.4 | 64.6 | 73.5 | ℃(0.45MPa) | GB/T1634-1979 |
| Vicat softening point | 87.2 | 90 | 88.4 | 77.8 | 86.8 | ℃ | GB/T1633-2000 |
The PVC composition of the embodiment of the invention and comparative example 1,2,3, in the PVC composition compare, as seen hard polyvinyl chloride composition of the present invention is when significantly improving elongation at break, shock strength also is improved to some extent, and the rigidity of material, thermal denaturation temperature, Vicat softening point still can be kept level preferably.
Claims (9)
1. hard polyvinyl chloride composition includes the following component of blend:
A. polyvinyl chloride (PVC) RESINS 100 weight parts
B. powdered rubber 3～30 weight parts that have crosslinking structure
C. dispersion agent 0.5～3.0 weight part
Wherein polyvinyl chloride (PVC) RESINS is the polymerization degree more than or equal to 700 polyvinyl chloride (PVC) RESINS; The powdered rubber that wherein has crosslinking structure, median size are 20～200nm, and gel content is 60% weight or higher;
Wherein dispersion agent is that carbonatoms is one or more in 10～20 the stearylamide; Perhaps dispersion agent is that carbonatoms is that 10～20 stearylamide and carbonatoms are the mixture of 3～20 effective for treatment of premature ejaculation, wherein the carbonatoms of alkyl is 3～10, in the stearic acid alkyl ester is 100 parts by weight, and the content of fatty acid alkyl ester is 0～30 part.
2. hard polyvinyl chloride composition according to claim 1 includes the following component of blend:
A. polyvinyl chloride (PVC) RESINS 100 weight parts
B. powdered rubber 3～15 weight parts that have crosslinking structure
C. dispersion agent 1～1.5 weight part.
3. hard polyvinyl chloride composition according to claim 1, wherein said powdered rubber with crosslinking structure be selected from powder nbr rubber, carboxyl butyronitrile powdered rubber or its mixing.
4. hard polyvinyl chloride composition according to claim 1, wherein said median size with powdered rubber of crosslinking structure is 30～120nm.
5. hard polyvinyl chloride composition according to claim 1, wherein said particle with powdered rubber of crosslinking structure is equal phase structure.
6. hard polyvinyl chloride composition according to claim 1, wherein said gel content with powdered rubber of crosslinking structure is 80% weight or higher.
7. according to each described hard polyvinyl chloride composition of claim 1～6, the powdered rubber that wherein has crosslinking structure is one or more in fully vulcanized powder rubber and the cross-linked powdered rubber.
8. hard polyvinyl chloride composition according to claim 1 is 100 parts by weight in stearylamide in the wherein said dispersion agent, and the content of fatty acid alkyl ester is 5～20 parts.
9. preparation method according to each described hard polyvinyl chloride composition of claim 1～8 comprises that the step of component by melt blending that will include above-described polyvinyl chloride (PVC) RESINS, have powdered rubber, a dispersion agent of crosslinking structure makes hard polyvinyl chloride composition.
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Cited By (3)
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| CN104602043A (en) * | 2007-03-19 | 2015-05-06 | 三星电子株式会社 | content provision apparatus and method |
| EP2995647A4 (en) * | 2013-05-09 | 2016-09-28 | Shandong Rike Chemical Co Ltd | Polyvinyl chloride mixture and preparation method therefor |
| EP2995646A4 (en) * | 2013-05-09 | 2016-09-28 | Shandong Rike Chemical Co Ltd | Polyvinyl chloride modifier and composite, and preparation method therefor |
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| CN102051007B (en) * | 2009-10-27 | 2013-02-27 | 中国石油化工股份有限公司 | Soft polrvinyl chloride composition and preparation method thereof |
| CN102276941B (en) * | 2010-06-11 | 2013-12-25 | 德标管业(上海)有限公司 | Rigid polyvinyl chloride (PVC) injection molding material |
| CN102453291B (en) * | 2010-10-25 | 2013-11-06 | 中国石油化工股份有限公司 | Anti-impact polyvinyl chloride composition and preparation method thereof |
| CN102775693B (en) * | 2011-05-13 | 2015-02-11 | 中国石油化工股份有限公司 | Transparent polyvinyl chloride composition and its preparation method |
| CN105602160A (en) * | 2016-03-24 | 2016-05-25 | 哈尔滨中大型材科技股份有限公司 | PVC (polyvinyl chloride) composite modified material and preparation method thereof |
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| CN1353135A (en) * | 2000-11-03 | 2002-06-12 | 中国石油化工股份有限公司 | Toughened plastics and its preparing process |
| CN1513906A (en) * | 2002-12-31 | 2004-07-21 | 中国石油化工股份有限公司 | Soft polyvinyl chloride composition and its preparation method |
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| CN1353135A (en) * | 2000-11-03 | 2002-06-12 | 中国石油化工股份有限公司 | Toughened plastics and its preparing process |
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| CN104602043A (en) * | 2007-03-19 | 2015-05-06 | 三星电子株式会社 | content provision apparatus and method |
| EP2995647A4 (en) * | 2013-05-09 | 2016-09-28 | Shandong Rike Chemical Co Ltd | Polyvinyl chloride mixture and preparation method therefor |
| EP2995646A4 (en) * | 2013-05-09 | 2016-09-28 | Shandong Rike Chemical Co Ltd | Polyvinyl chloride modifier and composite, and preparation method therefor |
| US9580589B2 (en) | 2013-05-09 | 2017-02-28 | Shandong Rike Chemical Co., Ltd. | Polyvinyl chloride mixture and preparation method therefor |
| US9587101B2 (en) | 2013-05-09 | 2017-03-07 | Shandong Rike Chemical Co., Ltd. | Polyvinyl chloride modifier and composite, and preparation method therefor |
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