CN101235197B - Plasticizing modifying treatment method for mould nylon - Google Patents
Plasticizing modifying treatment method for mould nylon Download PDFInfo
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- CN101235197B CN101235197B CN 200710037055 CN200710037055A CN101235197B CN 101235197 B CN101235197 B CN 101235197B CN 200710037055 CN200710037055 CN 200710037055 CN 200710037055 A CN200710037055 A CN 200710037055A CN 101235197 B CN101235197 B CN 101235197B
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Abstract
The invention relates to a toughening modification processing method of molding nylon, which comprises firstly conducting the grinding process for ethylene-octene copolymer using as the first modifier after melting and grafting with polar group, then carrying out the preprocess for short glass fiber with coupling agent, then conducting with the grinding process as the second modifier, mixing the first modifier and the second modifier with caprolactam monomer, heating up to melt, adding catalyst and catalyst promoter after dehydration, heating up and stirring at high speed to mix, casting into a mould, carrying out polymerization and slow-cooling, and finally conducting with mould unloading. Compared with the prior art, the material of the invention has excellent impact strength which can increase over 30%, and the tension and bending strength can basically keep the same.
Description
Technical field
The invention belongs to materials science field, relate to a kind of plasticizing modifying treatment method of monomer cast nylon.
Background technology
Monomer cast nylon is called monomer moulding casting nylon (MC nylon), is a kind of engineering materials of excellent property.It has, and polymerization temperature is low, and technology is easier, and degree of crystallinity height, the molecular weight of polymkeric substance can reach 7-10 about ten thousand, is higher than general nylon several times, and its degree of crystallinity can surpass 50%, and density is also bigger.Therefore every mechanical property is well, and excellent wear resistant and self lubricity are arranged, and the energy resistance to chemical attack is widely used in the engineering field: mine metallurgy, petrochemical complex, industry light industry textile industry, railway traffic etc.
But pure MC nylon often is difficult to satisfy some special applications requirements, under the condition of some HI high impact, its notched Izod impact strength is relatively poor, compare with metallic substance such as ferrous materials, lower physical strength is arranged, be difficult to be applied on the heavy construction part of high-strength, high-ductility.
The macromolecular material ethylene-octene copolymer is a kind of novel elastomer material, because its unique molecular chain structure makes it have excellent toughening effect.Adopt the ethylene-octene copolymer of melting method grafting polar monomer, strengthened surperficial polarity, tightr with the caprolactam monomer consistency can increase the toughness of MC nylon simultaneously.
In domestic and foreign literature, the patent, do not see the report that the toughening agent modified monomer cast nylon of this type of polyolefin is arranged.
Summary of the invention
Purpose of the present invention is exactly the plasticizing modifying treatment method that a kind of notched Izod impact strength, monomer cast nylon that impelling strength is high are provided in order to overcome the weak point that above-mentioned prior art exists.
Purpose of the present invention can be achieved through the following technical solutions:
A kind of plasticizing modifying treatment method of monomer cast nylon is characterized in that, this method may further comprise the steps:
(1) pre-treatment of properties-correcting agent one
Get ethylene-octene copolymer 100 weight parts, polar group maleic anhydride 0.5-2 weight part, initiator 0.5-2 weight part and a small amount of oxidation inhibitor and dispersion agent stearic acid, in high speed agitator after uniform mixing 3-5 minute, in counter rotation twin screw extruder, carry out melting graft reaction, after pellet after the granulation put into horizontal pan mill and carry out repeatedly milling for several times, took out in 80 ℃ baking oven dry 1 hour, standby;
(2) processing of properties-correcting agent two
With γ-An Bingjisanyiyangjiguiwan, be dissolved in small amount of acetone, evenly stir into solution, pending short glass fiber was immersed in wherein 0.5-1 hour, put into ball grinder, ball milling for several times takes out good glass micro mist of ball milling or the little bits of glass in 80 ℃ baking oven dry 1 hour repeatedly, and airing is standby;
(3) with adding in the reaction vessel behind caprolactam monomer 70-85 weight part, properties-correcting agent one 10-20 weight part, the properties-correcting agent two 5-10 weight part uniform mixing, be heated to 110-120 ℃, regulate vacuum tightness, kept 20 minutes, to the moisture content Ex-all to 750mmHg;
(4) close vacuum unit, add Primary Catalysts, wherein the mol ratio of Primary Catalysts add-on is, Primary Catalysts: hexanolactam=0.002-0.005: 1, regulate vacuum tightness to 750mmHg, and kept 20 minutes, to the moisture content Ex-all;
(5) close vacuum unit, add promotor, wherein the mol ratio of promotor add-on is, promotor: hexanolactam=0.002-0.005: 1, regulate vacuum tightness to 750mmHg, and with agitator vigorous stirring 2-3 minute;
(6) after the abundant reaction, close vacuum unit, promptly material is poured in the mould of preheating, continue to allow mould slowly cool to room temperature, the demoulding after 15-30 minute again in insulation under 170-180 ℃.
Counter rotation twin screw extruder rotating speed in the described step (1) is 200 rev/mins, and each distinguishes processing temperature: 150 ℃, and 160 ℃, 170 ℃, 190 ℃, 200 ℃, 210 ℃.
γ-An Bingjisanyiyangjiguiwan in the described step (2) is KH560, accounts for 1% weight part of pending fiber.
The mean diameter of the glass fibre in the described step (2) is 10 μ m.
Primary Catalysts in the described step (4) comprises sodium hydroxide.
Promotor in the described step (5) comprises hexamethylene diisocyanate (HDI) or 4,4 '-diphenylmethanediisocyanate (MDI).
Compared with prior art, the present invention is based on copolymer-modified dose one of novel high polymer and toughener two to improve the monomer cast nylon material of its mechanical property, its major technique characteristics are: notched Izod impact strength reaches: 8-10KJ/m2, compare with common monomer cast nylon, impelling strength improves about 30%, and mechanical property keeps substantially.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described.
Embodiment 1
It is material modified to follow these steps to prepare monomer cast nylon:
(1) preparation of properties-correcting agent one and aftertreatment: get high molecular polymer ethylene-octene copolymer (POE) 100 weight parts, polar group maleic anhydride (MAH) 0.5 weight part, initiator dicumyl peroxide (DCP) 0.5 weight part, 1010 oxidation inhibitor, 0.005 weight part and dispersion agent stearic acid 0.005 weight part, uniform mixing is 3 minutes in high speed agitator.In counter rotation twin screw extruder, carry out melting graft reaction.Twin screw extruder is set: 200 rev/mins of screw speeds, each distinguishes processing temperature: 150 ℃, 160 ℃, 170 ℃, 190 ℃, 200 ℃, 210 ℃, extrude and granulation.Then pellet is put into horizontal pan mill and pulverized, after milling for several times repeatedly, took out in 80 ℃ baking oven dry 1 hour, standby;
(2) processing of properties-correcting agent two: with γ-An Bingjisanyiyangjiguiwan (KH560 accounts for 1% weight part of pending fiber), be dissolved in small amount of acetone, evenly stir into solution.(mean diameter 10 μ m) were immersed in wherein 0.5 hour with pending short glass fiber, put into ball grinder, and ball milling for several times repeatedly.Take out good glass micro mist of ball milling or the little bits of glass in 80 ℃ baking oven dry 1 hour, airing is standby;
(3) with caprolactam monomer 70 weight parts, properties-correcting agent one 20 weight parts, properties-correcting agent 2 10 weight parts add in the reaction vessel behind the uniform mixing, are heated to 110 ℃, at the uniform velocity stir, and open vacuum pump and regulate vacuum tightness to 750mmHg, keep 20 minutes, to the moisture content Ex-all;
(4) close vacuum unit, inflation is decompressed to normal pressure, with Primary Catalysts sodium hydroxide, add-on: with the hexanolactam mol ratio be 0.002: 1, put into and melt glassware, open vacuum pump and regulate vacuum tightness to 750mmHg, kept 20 minutes, to the moisture content Ex-all;
(5) close vacuum unit, inflation is decompressed to normal pressure, with promotor MDI, add-on: with the hexanolactam mol ratio be 0.002: 1, put into and melt glassware, open vacuum pump and regulate vacuum tightness, and with agitator vigorous stirring 2 minutes to 750mmHg;
(6) after the abundant reaction, close vacuum unit, inflation is decompressed to normal pressure, promptly material is poured in the mould of preheating, continues to allow mould slowly cool to room temperature, the demoulding in insulation under 170 ℃ after 15 minutes again.
Embodiment 2
It is material modified to follow these steps to prepare monomer cast nylon:
(1) preparation of properties-correcting agent one and aftertreatment: get high molecular polymer ethylene-octene copolymer (POE) 100 weight parts, polar group maleic anhydride (MAH) 2 weight parts, initiator dicumyl peroxide (DCP) 2 weight parts, 1010 oxidation inhibitor, 0.01 weight part and dispersion agent stearic acid 0.01 weight part, uniform mixing is 5 minutes in high speed agitator.In counter rotation twin screw extruder, carry out melting graft reaction.Twin screw extruder is set: 200 rev/mins of screw speeds, and each distinguishes processing temperature: 150 ℃, 160 ℃, 170 ℃, 190 ℃, 200 ℃, 210 ℃,, extrude and granulation.Then pellet is put into horizontal pan mill and pulverized, after milling for several times repeatedly, took out in 80 ℃ baking oven dry 1 hour, standby;
(2) processing of properties-correcting agent two: with γ-An Bingjisanyiyangjiguiwan (KH560 accounts for 1% weight part of pending fiber), be dissolved in small amount of acetone, evenly stir into solution.(mean diameter 10 μ m) were immersed in wherein 1 hour with pending short glass fiber, put into ball grinder, and ball milling for several times repeatedly.Take out good glass micro mist of ball milling or the little bits of glass in 80 ℃ baking oven dry 1 hour, airing is standby;
(3) with caprolactam monomer 85 weight parts, properties-correcting agent one 10 weight parts, properties-correcting agent 25 weight parts add in the reaction vessel behind the uniform mixing, are heated to 120 ℃, at the uniform velocity stir, and open vacuum pump and regulate vacuum tightness to 750mmHg, keep 20 minutes, to the moisture content Ex-all;
(4) close vacuum unit, inflation is decompressed to normal pressure, with Primary Catalysts sodium hydroxide, add-on: with the hexanolactam mol ratio be 0.005: 1, put into and melt glassware, open vacuum pump and regulate vacuum tightness to 750mmHg, kept 20 minutes, to the moisture content Ex-all;
(5) close vacuum unit, inflation is decompressed to normal pressure, with promotor MDI, add-on: with the hexanolactam mol ratio be 0.005: 1, put into and melt glassware, open vacuum pump and regulate vacuum tightness, and with agitator vigorous stirring 3 minutes to 750mmHg;
(6) after the abundant reaction, close vacuum unit, inflation is decompressed to normal pressure, promptly material is poured in the mould of preheating, continues to allow mould slowly cool to room temperature, the demoulding in insulation under 170 ℃ after 30 minutes again.
Embodiment 3
It is material modified to follow these steps to prepare monomer cast nylon:
(1) preparation of properties-correcting agent one and aftertreatment: get high molecular polymer ethylene-octene copolymer (POE) 100 weight parts, polar group maleic anhydride (MAH) 1 weight part, initiator dicumyl peroxide (DCP) 1 weight part, 1012 oxidation inhibitor, 0.08 weight part and dispersion agent stearic acid 0.08 weight part, uniform mixing is 4 minutes in high speed agitator.In counter rotation twin screw extruder, carry out melting graft reaction.Twin screw extruder is set: 200 rev/mins of screw speeds, each distinguishes processing temperature: 150 ℃, 160 ℃, 170 ℃, 190 ℃, 200 ℃, 210 ℃, extrude and granulation.Then pellet is put into horizontal pan mill and pulverized, after milling for several times repeatedly, took out in 80 ℃ baking oven dry 1 hour, standby;
(2) processing of properties-correcting agent two: with γ-An Bingjisanyiyangjiguiwan (KH560 accounts for 1% weight part of pending fiber), be dissolved in small amount of acetone, evenly stir into solution.(mean diameter 10 μ m) were immersed in wherein 0.5 hour with pending short glass fiber, put into ball grinder, and ball milling for several times repeatedly.Take out good glass micro mist of ball milling or the little bits of glass in 80 ℃ baking oven dry 1 hour, airing is standby;
(3) with caprolactam monomer 75 weight parts, properties-correcting agent one 15 weight parts, properties-correcting agent 2 10 weight parts add in the reaction vessel behind the uniform mixing, are heated to 120 ℃, at the uniform velocity stir, and open vacuum pump and regulate vacuum tightness to 750mmHg, keep 20 minutes, to the moisture content Ex-all;
(4) close vacuum unit, inflation is decompressed to normal pressure, with Primary Catalysts sodium hydroxide, add-on: with the hexanolactam mol ratio be 0.003: 1, put into and melt glassware, open vacuum pump and regulate vacuum tightness to 750mmHg, kept 20 minutes, to the moisture content Ex-all;
(5) close vacuum unit, inflation is decompressed to normal pressure, with promotor MDI, add-on: with the hexanolactam mol ratio be 0.003: 1, put into and melt glassware, open vacuum pump and regulate vacuum tightness, and with agitator vigorous stirring 3 minutes to 750mmHg;
(6) after the abundant reaction, close vacuum unit, inflation is decompressed to normal pressure, promptly material is poured in the mould of preheating, continues to allow mould slowly cool to room temperature, the demoulding in insulation under 170 ℃ after 40 minutes again.
Embodiment 4
It is material modified to follow these steps to prepare monomer cast nylon:
(1) preparation of properties-correcting agent one and aftertreatment: get high molecular polymer ethylene-octene copolymer (POE) 100 weight parts, polar group maleic anhydride (MAH) 1.5 weight parts, initiator dicumyl peroxide (DCP) 1.5 weight parts, 1012 oxidation inhibitor, 0.015 weight part and dispersion agent stearic acid 0.015 weight part, uniform mixing is 5 minutes in high speed agitator.In counter rotation twin screw extruder, carry out melting graft reaction.Twin screw extruder is set: 200 rev/mins of screw speeds, and each distinguishes processing temperature: 150 ℃, 160 ℃, 170 ℃, 190 ℃, 200 ℃, 210 ℃,, extrude and granulation.Then pellet is put into horizontal pan mill and pulverized, after milling for several times repeatedly, took out in 80 ℃ baking oven dry 1 hour, standby;
(2) processing of properties-correcting agent two: with γ-An Bingjisanyiyangjiguiwan (KH560 accounts for 1% weight part of pending fiber), be dissolved in small amount of acetone, evenly stir into solution.(mean diameter 10 μ m) were immersed in wherein 1 hour with pending short glass fiber, put into ball grinder, and ball milling for several times repeatedly.Take out good glass micro mist of ball milling or the little bits of glass in 80 ℃ baking oven dry 1 hour, airing is standby;
(3) with caprolactam monomer 80 weight parts, properties-correcting agent one 10 weight parts, properties-correcting agent 2 10 weight parts add in the reaction vessel behind the uniform mixing, are heated to 120 ℃, at the uniform velocity stir, and open vacuum pump and regulate vacuum tightness to 750mmHg, keep 20 minutes, to the moisture content Ex-all;
(4) close vacuum unit, inflation is decompressed to normal pressure, with Primary Catalysts sodium hydroxide, add-on: with the hexanolactam mol ratio be 0.004: 1, put into and melt glassware, open vacuum pump and regulate vacuum tightness to 750mmHg, kept 20 minutes, to the moisture content Ex-all;
(5) close vacuum unit, inflation is decompressed to normal pressure, with promotor HDI, add-on: with the hexanolactam mol ratio be 0.004: 1, put into and melt glassware, open vacuum pump and regulate vacuum tightness, and with agitator vigorous stirring 3 minutes to 750mmHg;
(6) after the abundant reaction, close vacuum unit, inflation is decompressed to normal pressure, promptly material is poured in the mould of preheating, continues to allow mould slowly cool to room temperature, the demoulding in insulation under 170 ℃ after 40 minutes again.
Subordinate list mechanical property consolidated statement
| Project | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Pure monomer cast nylon |
| Socle girder notched Izod impact strength (KJ/M2) | 10 | 7 | 9 | 8 | 5 |
| Tensile strength (MPa) | 79 | 70 | 75 | 75 | 75 |
| Flexural strength (MPa) | 145 | 140 | 142 | 141 | 140 |
Claims (6)
1. the plasticizing modifying treatment method of a monomer cast nylon is characterized in that, this method may further comprise the steps:
(1) pre-treatment of properties-correcting agent one
Get ethylene-octene copolymer 100 weight parts, polar group maleic anhydride 0.5-2 weight part, initiator 0.5-2 weight part and 1010 oxidation inhibitor, 0.005 weight part and dispersion agent stearic acid 0.005 weight part or 1010 oxidation inhibitor, 0.01 weight part and dispersion agent stearic acid 0.01 weight part, perhaps 1012 oxidation inhibitor, 0.015 weight part and dispersion agent stearic acid 0.015 weight part or 1012 oxidation inhibitor, 0.08 weight part and dispersion agent stearic acid 0.08 weight part, in high speed agitator after uniform mixing 3-5 minute, in counter rotation twin screw extruder, carry out melting graft reaction, after pellet after the granulation put into horizontal pan mill and carry out repeatedly milling for several times, taking-up in 80 ℃ baking oven dry 1 hour, standby;
(2) processing of properties-correcting agent two
With γ-An Bingjisanyiyangjiguiwan, be dissolved in small amount of acetone, evenly stir into solution, pending short glass fiber was immersed in wherein 0.5-1 hour, put into ball grinder, ball milling for several times takes out good glass micro mist of ball milling or the little bits of glass in 80 ℃ baking oven dry 1 hour repeatedly, and airing is standby;
(3) with adding in the reaction vessel behind caprolactam monomer 70-85 weight part, properties-correcting agent one 10-20 weight part, the properties-correcting agent two 5-10 weight part uniform mixing, be heated to 110-120 ℃, regulate vacuum tightness, kept 20 minutes, to the moisture content Ex-all to 750mmHg;
(4) close vacuum unit, add Primary Catalysts, wherein the mol ratio of Primary Catalysts add-on is, Primary Catalysts: hexanolactam=0.002-0.005: 1, regulate vacuum tightness to 750mmHg, and kept 20 minutes, to the moisture content Ex-all;
(5) close vacuum unit, add promotor, wherein the mol ratio of promotor add-on is, promotor: hexanolactam=0.002-0.005: 1, regulate vacuum tightness to 750mmHg, and with agitator vigorous stirring 2-3 minute;
(6) after the abundant reaction, close vacuum unit, promptly material is poured in the mould of preheating, continue to allow mould slowly cool to room temperature, the demoulding after 15-30 minute again in insulation under 170-180 ℃.
2. the plasticizing modifying treatment method of a kind of monomer cast nylon according to claim 1 is characterized in that, the counter rotation twin screw extruder rotating speed in the described step (1) is 200 rev/mins, each distinguishes processing temperature: 150 ℃, and 160 ℃, 170 ℃, 190 ℃, 200 ℃, 210 ℃.
3. the plasticizing modifying treatment method of a kind of monomer cast nylon according to claim 1 is characterized in that, the γ-An Bingjisanyiyangjiguiwan in the described step (2) is KH560, accounts for 1% weight part of pending fiber.
4. the plasticizing modifying treatment method of a kind of monomer cast nylon according to claim 1 is characterized in that, the mean diameter of the glass fibre in the described step (2) is 10 μ m.
5. the plasticizing modifying treatment method of a kind of monomer cast nylon according to claim 1 is characterized in that, the Primary Catalysts in the described step (4) is a sodium hydroxide.
6. the plasticizing modifying treatment method of a kind of monomer cast nylon according to claim 1 is characterized in that, the promotor in the described step (5) is hexamethylene diisocyanate (HDI) or 4,4 '-diphenylmethanediisocyanate (MDI).
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Families Citing this family (9)
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| CN101367991B (en) * | 2008-09-25 | 2011-01-05 | 上海交通大学 | Method of manufacturing polycarbonate/vinyl cyanide-butadiene-styrol copolymer alloy |
| CN102002160B (en) * | 2010-11-02 | 2012-03-21 | 北京三联虹普新合纤技术服务股份有限公司 | Production process for preparing nylon slices for new membranes by using caprolactam |
| CN102532524B (en) * | 2010-12-28 | 2015-05-13 | 合肥杰事杰新材料股份有限公司 | Nylon chopped fiber/cast nylon composite material and preparation method thereof |
| CN102618028B (en) * | 2012-03-20 | 2013-11-06 | 株洲时代新材料科技股份有限公司 | Side bearing abrasion plate for roadway wagon and production process of side bearing abrasion plate |
| CN103232595A (en) * | 2012-04-16 | 2013-08-07 | 齐齐哈尔北坤合成高分子材料有限公司 | Modified MC nylon |
| CN102977361A (en) * | 2012-12-28 | 2013-03-20 | 湖南汇中新材料有限公司 | Method for preparing glass fiber reinforced nylon 6 by in situ polymerization |
| CN103254638B (en) * | 2013-05-14 | 2016-02-10 | 厦门建霖工业有限公司 | A kind of high filling fiber glass reinforced polyamide composite material and preparation method thereof |
| CN109648724A (en) * | 2018-12-26 | 2019-04-19 | 柳州申通汽车科技有限公司 | A kind of processing technology of activeness and quietness nylon composite materials |
| CN113529208A (en) * | 2021-07-06 | 2021-10-22 | 李春婵 | Production formula and production process of high-strength low-temperature-resistant long-fiber nylon |
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