CN102604365A - Casting polyurethane/diatomite composite material and preparation method thereof - Google Patents
Casting polyurethane/diatomite composite material and preparation method thereof Download PDFInfo
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- CN102604365A CN102604365A CN2012100716489A CN201210071648A CN102604365A CN 102604365 A CN102604365 A CN 102604365A CN 2012100716489 A CN2012100716489 A CN 2012100716489A CN 201210071648 A CN201210071648 A CN 201210071648A CN 102604365 A CN102604365 A CN 102604365A
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Abstract
The invention relates to a casting polyurethane/diatomite composite material and a preparation method thereof. The composite material is prepared from the following raw materials: diatomite (modified by a silane coupling agent), polyurethane prepolymers and a chain extender, wherein the mass of the diatomite (modified by the silane coupling agent) accounts for 0.5-10% of that of the polyurethane prepolymer. The preparation method comprises the following steps: (1) at room temperature, carrying out modification on the diatomite by using a silane coupling agent so as to obtain modified diatomite; and (2) weighting and preheating polyurethane prepolymers, and adding the modified diatomite obtained in the step (1) into the preheated polyurethane prepolymers, mixing and stirring, then carrying out vacuum defoamation on the obtained object so as to obtain a mixture, after the chain extender is heated and molten, adding the molten chain extender into the mixture, mixing and stirring, casting the object into a mould to carry out primary vulcanization, after the primary vulcanization is completed, carrying out demoulding on the obtained object, and finally, carrying out secondary vulcanization on the obtained object. The CPU/diatomite composite material prepared in the invention is good in mechanical properties and heat resistance; and the preparation method disclosed by the invention is simple, direct, low in energy consumption, convenient for processing and forming, and suitable for being applied to industrial production.
Description
Technical field
The invention belongs to casting PU matrix material and preparation field thereof, particularly a kind of casting PU/diatomite composite material and preparation method thereof.
Background technology
Casting PU (CPU) is commonly called as fluid rubber, is to make with oligomer polyol such as polyester or polyethers and POLYMETHYLENE POLYPHENYLISOCYANATE, chainextender reaction.Have good wear resistance, mechanical property and damping property etc., be widely used in departments such as electromechanics, boats and ships, aviation, vehicle, civil construction, light industry, weaving.But poor performance such as the intensity of CPU is not high, and is heat-resisting, water-fast, antistatic, its life-time service temperature can not surpass 80 ℃ generally speaking, and the short-term use temperature can not surpass 120 ℃, thereby has limited its further application.
Zeyssatite is that the remains of the diatoms that in ocean or lake, grows are at subaqueous deposit, through the physical environment effect and a kind of non-metallic minerals that forms gradually.It is big, acidproof to have light weight, porous, specific surface area, and characteristics such as heat-resisting and chemicalstability height can be used as the filler and the toughener of polymer materials and coating.China's diatomite ore resource rich, reserves are more than 2,000,000,000 tons, and low price.Zeyssatite is extensive in sector applications such as acoustical material, material of construction, coating, heat preserving and insulating materials in recent years.People such as J.Z.Liang are at [Melt rheology during extrusion of polypropylene composites filled with diatomite particles.Journal of Reinforced Plastics and Composites; 2010; 29:2744-2752] on reported that the employing twin screw extruder has successfully prepared Vestolen PP 7052/diatomite composite material, and set up the equation between parameters such as diatomaceous particle radius, filling ratio and the matrix material tensile strength.People such as Li Zhihong [the synthetic and performance study of zeyssatite-Z 150PH super absorbent resin. New Chemical Materials, 2008,36 (9): 93-95] on reported that the employing suspension polymerization has made zeyssatite/Z 150PH super absorbent resin.And inquired into factors such as dosage of crosslinking agent, zeyssatite addition, hydrolysis degree to hydroscopicity resin can influence.
Up to the present, Shang Weijian adopts the report of zeyssatite modification CPU matrix material.
Summary of the invention
Technical problem to be solved by this invention provides a kind of casting PU/diatomite composite material and preparation method thereof, this composite materials property and good heat resistance, and this method is simple, direct, pollution-free, suitability for industrialized production.
A kind of casting PU/diatomite composite material of the present invention; The raw material of this matrix material comprises: through silane coupler modified zeyssatite, base polyurethane prepolymer for use as and chainextender; Be 0.5～10% of base polyurethane prepolymer for use as quality through silane coupler modified zeyssatite wherein, the mass ratio of chainextender and urethane is according to computes:
NCO base content mass percent * 4.51 * batch charging coefficient in chainextender consumption (kg)=performed polymer quality (kg) * unit mass prepolymer.
Above-mentioned batch charging coefficient is 0.8～1.
Described chainextender is two amine chainextenders, preferentially uses 4, and 4 '-methylene-bis (3-chloro-2,6-Diethyl Aniline) (M-CDEA).
The preparation method of a kind of casting PU/diatomite composite material of the present invention comprises:
(1) silane coupler modified zeyssatite:
Under the room temperature, zeyssatite is joined in the reaction vessel, add hexanaphthene, Tri N-Propyl Amine and silane coupling agent then successively, stir 30～60min, stir 30～60min down at 50～70 ℃ again in 500～800r/min; Reacted solution at 60～90 ℃ of following rotary evaporation 30～60min, at last at 60～80 ℃ of following vacuum-drying 18～30h, is obtained the zeyssatite after the modification;
(2) prepolymer method prepares the CPU/ diatomite composite material:
Take by weighing base polyurethane prepolymer for use as at 80～95 ℃ of following preheating 1～4h; Add the zeyssatite after the modification that the step (1) of base polyurethane prepolymer for use as massfraction 0.5～10% obtains then; Mix stirring 10～40min in 500～800r/min; In 80～95 ℃ of vacuum defoamation 10～40min, get mixture then; Chainextender is added behind 110～130 ℃ of following heating and meltings in the said mixture, after 500～800r/min mixes stirring 40～60s down, be poured in the mould, once vulcanize; 70～110 ℃ of curing temperatures; Sulfide stress 5～15MPa, curing time 20～60min, the demoulding after once sulfuration is accomplished; Last in post cure 4～20h of 70～150 ℃, get final product.
Diatomaceous granularity is 300～5000 orders in the said step (1), and preferentially using granularity is 2000 purpose zeyssatite.
Silane coupling agent is KH-550 in the said step (1), KH-570, and KH-560, A-151 or A-171 preferentially use KH-570.
The quality proportioning of zeyssatite, hexanaphthene, Tri N-Propyl Amine and silane coupling agent is in the said step (1): 40～60 parts in zeyssatite, 200～1000 parts of hexanaphthenes, 0.5～2 part of Tri N-Propyl Amine, 4～8 parts of silane coupling agents.
The present invention adopts silane coupling agent that zeyssatite is carried out surface treatment, in order to improve the dispersiveness of zeyssatite in CPU.The present invention is utilizing diatomaceous specific surface area big, Heat stability is good, and characteristics such as vesicular structure; It is mixed with base polyurethane prepolymer for use as; Performed polymer is attracted to around the zeyssatite pore structure, produces a kind of inner interlocking structure, and chain extension-crosslinking makes the CPU/ diatomite composite material then.The prepolymer method preparation that the composite material by adopting operating procedure is simple, direct, energy consumption is low.Only need a small amount of diatomaceous earth filler, the mechanical property of CPU and thermotolerance just can obtain bigger raising.
The present invention is directed to this series products of base polyurethane prepolymer for use as of selling on the market, adopt prepolymer method that zeyssatite is dispersed in and prepared the CPU/ diatomite composite material in the performed polymer, improve the mechanical property and the thermotolerance of casting PU material effectively.
Prepared CPU/ diatomite composite material mechanical property and thermotolerance are greatly improved.Wherein, the tensile strength of CPU and tear strength are respectively 40.06MPa and 67.16N/mm, and the tensile strength of matrix material and tear strength are brought up to 47.87MPa and 99.34N/mm respectively after the zeyssatite modification, and amplification reaches 19.5% and 47.9% respectively.The heat decomposition temperature of CPU under 20% weightlessness is 317 ℃, and the heat decomposition temperature of CPU/ diatomite composite material under 20% weightlessness is 340 ℃, improved 23 ℃.
Beneficial effect
(1) this method is simple, direct, energy consumption is low, machine-shaping is convenient, suitability for industrialized production;
(2) prepared CPU/ diatomite composite material mechanical property and thermotolerance are greatly improved;
(3) not only to make zeyssatite can be used for the enhancing of CPU toughness reinforcing in the present invention, and can be used for strengthening toughness reinforcing other rubber and plastics.
Description of drawings
Fig. 1. the field emission scanning electron microscope photo of the CPU/ diatomite composite material section of embodiment 3;
Fig. 2. the thermogravimetric curve of the CPU/ diatomite composite material of embodiment 3;
Fig. 3. the preparation flow figure of CPU/ diatomite composite material of the present invention.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in the restriction scope of the present invention.Should be understood that in addition those skilled in the art can do various changes or modification to the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Embodiment 1
(1) taking by weighing the 20g granularity is that 2000 purpose zeyssatite add in the there-necked flask, adds 400mL hexanaphthene, 0.4g Tri N-Propyl Amine and 2g silane coupling agent KH-560 again, and low whipping speed is stirring at room 30min under the 500r/min, stirs 30min down at 50 ℃ then.Reacted solution at 60 ℃ of following rotary evaporation 1h, subsequently at 60 ℃ of following vacuum-drying 30h, is collected zeyssatite;
(2) take by weighing 100g performed polymer (NCO matrix amount content is 5.0 ± 0.2%) at 80 ℃ of following preheating 1h, the zeyssatite that takes by weighing then after the 0.5g modification adds in the above-mentioned performed polymer, and low whipping speed is that 500r/min mixes down and stirs 10min.Subsequently the mixture that obtains is placed 80 ℃ of vacuum drying oven vacuum defoamation 10min.Take by weighing 21.4g M-CDEA chainextender at 110 ℃ of following heating and meltings, add in the said mixture, low whipping speed is that 500r/min mixes stirring 40s down.Then the gained mixture is poured in the mould, places on the vulcanizing press and once vulcanize (70 ℃ of temperature, pressure 5MPa, time 20min).The demoulding after once sulfuration is accomplished places the sample that obtains 70 ℃ constant temperature air dry oven post cure 4h at last, thereby makes the CPU/ diatomite composite material.
Embodiment 2
(1) taking by weighing the 25g granularity is that 2000 purpose zeyssatite add in the there-necked flask, adds 550mL hexanaphthene, 0.4g Tri N-Propyl Amine and 3g silane resin acceptor kh-550 again, and low whipping speed is stirring at room 40min under the 600r/min, stirs 40min down at 60 ℃ then.Reacted solution at 70 ℃ of following rotary evaporation 1h, subsequently at 65 ℃ of following vacuum-drying 28h, is collected zeyssatite;
(2) take by weighing 100g performed polymer (NCO base content be 5.0 ± 0.2%) at 85 ℃ of following preheating 1.5h, the zeyssatite that takes by weighing then after the 1g modification adds in the above-mentioned performed polymer, and low whipping speed is that 600r/min mixes down and stirs 20min.Subsequently the mixture that obtains is placed 85 ℃ of vacuum drying oven vacuum defoamation 20min.Take by weighing 21.4g M-CDEA chainextender at 115 ℃ of following heating and meltings, add in the said mixture, low whipping speed is that 600r/min mixes stirring 45s down.Then the gained mixture is poured in the mould, places on the vulcanizing press and once vulcanize (80 ℃ of temperature, pressure 7MPa, time 30min).The demoulding after once sulfuration is accomplished places the sample that obtains 90 ℃ constant temperature air dry oven post cure 8h at last, thereby makes the CPU/ diatomite composite material.
Embodiment 3
(1) taking by weighing the 30g granularity is that 2000 purpose zeyssatite add in the there-necked flask, adds 700mL hexanaphthene, 0.5g Tri N-Propyl Amine and 4g silane coupling agent KH-570 again, and low whipping speed is stirring at room 50min under the 650r/min, stirs 50min down at 60 ℃ then.Reacted solution at 80 ℃ of following rotary evaporation 50min, subsequently at 70 ℃ of following vacuum-drying 24h, is collected zeyssatite;
(2) take by weighing 100g performed polymer (NCO base content be 5.0 ± 0.2%) at 88 ℃ of following preheating 2h, the zeyssatite that takes by weighing then after the 3g modification adds in the above-mentioned performed polymer, and low whipping speed is that 650r/min mixes down and stirs 25min.Subsequently the mixture that obtains is placed 88 ℃ of vacuum drying oven vacuum defoamation 25min.Take by weighing 21.4g M-CDEA chainextender at 120 ℃ of following heating and meltings, add in the said mixture, low whipping speed is that 650r/min mixes stirring 50s down.Then the gained mixture is poured in the mould, places on the vulcanizing press and once vulcanize (90 ℃ of temperature, pressure 10MPa, time 40min).The demoulding after once sulfuration is accomplished places the sample that obtains 110 ℃ constant temperature air dry oven post cure 12h at last, thereby makes the CPU/ diatomite composite material.
Table 1 shows that the tensile strength and the tear strength of present embodiment synthetic matrix material are respectively 47.87MPa and 99.34N/mm, and the heat decomposition temperature under 20% weightlessness is 340 ℃.
Fig. 1 is the field emission scanning electron microscope photo of present embodiment synthetic matrix material section, and can find out: diatomite particle is dispersed among the CPU uniformly.Fig. 2 is the thermogravimetric curve of present embodiment synthetic matrix material, can find out: the thermotolerance of CPU/ diatomite composite material is better than CPU.
Embodiment 4
(1) taking by weighing the 35g granularity is that 4000 purpose zeyssatite add in the there-necked flask, adds 800mL hexanaphthene, 0.7g Tri N-Propyl Amine and 5g silane coupling A-151 again, and low whipping speed is stirring at room 55min under the 700r/min, stirs 55min down at 70 ℃ then.Reacted solution at 85 ℃ of following rotary evaporation 40min, subsequently at 75 ℃ of following vacuum-drying 20h, is collected zeyssatite;
(2) take by weighing 100g performed polymer (NCO base content be 5.0 ± 0.2%) at 90 ℃ of following preheating 3h, the zeyssatite that takes by weighing then after the 5g modification adds in the above-mentioned performed polymer, and low whipping speed is that 700r/min mixes down and stirs 30min.Subsequently the mixture that obtains is placed 90 ℃ of vacuum drying oven vacuum defoamation 30min.Take by weighing 22.3g M-CDEA chainextender at 125 ℃ of following heating and meltings, add in the said mixture, low whipping speed is that 700r/min mixes stirring 55s down.Then the gained mixture is poured in the mould, places on the vulcanizing press and once vulcanize (100 ℃ of temperature, pressure 12MPa, time 50min).The demoulding after once sulfuration is accomplished places the sample that obtains 130 ℃ constant temperature air dry oven post cure 16h at last, thereby makes the CPU/ diatomite composite material.
Embodiment 5
(1) taking by weighing the 40g granularity is that 500 purpose zeyssatite add in the there-necked flask, adds 950mL hexanaphthene, 1g Tri N-Propyl Amine and 8g silane coupling agent KH-570 again, and low whipping speed is stirring at room 1h under the 800r/min, stirs 1h down at 70 ℃ then.Reacted solution at 90 ℃ of following rotary evaporation 30min, subsequently at 80 ℃ of following vacuum-drying 18h, is collected zeyssatite;
(2) take by weighing 100g performed polymer (NCO base content be 5.0 ± 0.2%) at 95 ℃ of following preheating 4h, the zeyssatite that takes by weighing then after the 10g modification adds in the above-mentioned performed polymer, and low whipping speed is that 800r/min mixes down and stirs 40min.Subsequently the mixture that obtains is placed 95 ℃ of vacuum drying oven vacuum defoamation 40min.Take by weighing 20.6g M-CDEA chainextender at 130 ℃ of following heating and meltings, add in the said mixture, low whipping speed is that 800r/min mixes stirring 60s down.Then the gained mixture is poured in the mould, places on the vulcanizing press and once vulcanize (110 ℃ of temperature, pressure 15MPa, time 60min).The demoulding after once sulfuration is accomplished places the sample that obtains 150 ℃ constant temperature air dry oven post cure 20h at last, thereby makes the CPU/ diatomite composite material.
Polyurethane elastomer product properties such as following table
The mechanical property and the thermotolerance of table 1 polyurethane elastomer goods
Claims (9)
1. casting PU/diatomite composite material; The raw material of this matrix material comprises: through silane coupler modified zeyssatite, base polyurethane prepolymer for use as and chainextender; Be 0.5～10% of base polyurethane prepolymer for use as quality through silane coupler modified zeyssatite wherein, the mass ratio of chainextender and urethane is according to computes:
NCO base content mass percent * 4.51 * batch charging coefficient in chainextender consumption=performed polymer quality * unit mass prepolymer.
2. a kind of casting PU/diatomite composite material according to claim 1 is characterized in that: described batch charging coefficient is 0.8～1.
3. a kind of casting PU/diatomite composite material according to claim 1 is characterized in that: described chainextender is two amine chainextenders.
4. a kind of casting PU/diatomite composite material according to claim 1 is characterized in that: described chainextender is 4,4 '-methylene-bis (3-chloro-2,6-Diethyl Aniline).
5. the preparation method of a casting PU/diatomite composite material comprises:
(1) under the room temperature, zeyssatite is joined in the reaction vessel, add hexanaphthene, Tri N-Propyl Amine and silane coupling agent then successively, stir 30～60min, stir 30～60min down at 50～70 ℃ again in 500～800r/min; Reacted solution at 60～90 ℃ of following rotary evaporation 30～60min, at last at 60～80 ℃ of following vacuum-drying 18～30h, is obtained the zeyssatite after the modification;
(2) take by weighing base polyurethane prepolymer for use as at 80～95 ℃ of following preheating 1～4h; Add the zeyssatite after the modification that the step (1) of base polyurethane prepolymer for use as massfraction 0.5～10% obtains then; Mix stirring 10～40min in 500～800r/min; In 80～95 ℃ of vacuum defoamation 10～40min, get mixture then; Chainextender is added behind 110～130 ℃ of following heating and meltings in the said mixture, after 500～800r/min mixes stirring 40～60s down, be poured in the mould, once vulcanize; 70～110 ℃ of curing temperatures; Sulfide stress 5～15MPa, curing time 20～60min, the demoulding after once sulfuration is accomplished; Last in post cure 4～20h of 70～150 ℃, get final product.
6. the preparation method of a kind of casting PU/diatomite composite material according to claim 5, it is characterized in that: diatomaceous granularity is 300～5000 orders in the said step (1).
7. the preparation method of a kind of casting PU/diatomite composite material according to claim 5, it is characterized in that: diatomaceous granularity is 2000 orders in the said step (1).
8. the preparation method of a kind of casting PU/diatomite composite material according to claim 5 is characterized in that: silane coupling agent is KH-550, KH-570, KH-560, A-151 or A-171 in the said step (1).
9. the preparation method of a kind of casting PU/diatomite composite material according to claim 5 is characterized in that: the quality proportioning of zeyssatite, hexanaphthene, Tri N-Propyl Amine and silane coupling agent is in the said step (1): 40～60 parts in zeyssatite, 200～1000 parts of hexanaphthenes, 0.5～2 part of Tri N-Propyl Amine, 4～8 parts of silane coupling agents.
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| CN103072230A (en) * | 2012-12-07 | 2013-05-01 | 江苏泰东科技有限公司 | Making method of low free nanometer wear-resistant polyurethane composite steel tube |
| CN105139944A (en) * | 2015-07-15 | 2015-12-09 | 繁昌县菲德通讯材料设计有限公司 | Computer communication cable |
| CN105382992A (en) * | 2015-11-06 | 2016-03-09 | 苏州瑞高新材料有限公司 | Preparing method for heat-resistant damping strengthened modified TPU composite material |
| CN108047427A (en) * | 2017-12-21 | 2018-05-18 | 广东石油化工学院 | A kind of diatomite/compound polyurethane material |
| CN112045914A (en) * | 2020-08-25 | 2020-12-08 | 河北华密橡胶科技股份有限公司 | Method for manufacturing multilayer multi-hardness polyurethane rubber core |
| CN112874082A (en) * | 2021-01-12 | 2021-06-01 | 桐乡市得健家居用品股份有限公司 | Diatom ooze sponge ground mat and preparation method thereof |
| CN113402201A (en) * | 2021-06-18 | 2021-09-17 | Oppo广东移动通信有限公司 | Composite material and preparation method thereof, structural member and preparation method thereof, and electronic equipment |
| CN114957965A (en) * | 2022-07-07 | 2022-08-30 | 福建长泰万泰矿物制品有限公司 | High-heat-resistance polyurethane composition, polyurethane disc and preparation method thereof |
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Cited By (9)
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| CN103072230A (en) * | 2012-12-07 | 2013-05-01 | 江苏泰东科技有限公司 | Making method of low free nanometer wear-resistant polyurethane composite steel tube |
| CN105139944A (en) * | 2015-07-15 | 2015-12-09 | 繁昌县菲德通讯材料设计有限公司 | Computer communication cable |
| CN105382992A (en) * | 2015-11-06 | 2016-03-09 | 苏州瑞高新材料有限公司 | Preparing method for heat-resistant damping strengthened modified TPU composite material |
| CN108047427A (en) * | 2017-12-21 | 2018-05-18 | 广东石油化工学院 | A kind of diatomite/compound polyurethane material |
| CN112045914A (en) * | 2020-08-25 | 2020-12-08 | 河北华密橡胶科技股份有限公司 | Method for manufacturing multilayer multi-hardness polyurethane rubber core |
| CN112874082A (en) * | 2021-01-12 | 2021-06-01 | 桐乡市得健家居用品股份有限公司 | Diatom ooze sponge ground mat and preparation method thereof |
| CN113402201A (en) * | 2021-06-18 | 2021-09-17 | Oppo广东移动通信有限公司 | Composite material and preparation method thereof, structural member and preparation method thereof, and electronic equipment |
| CN113402201B (en) * | 2021-06-18 | 2022-12-27 | Oppo广东移动通信有限公司 | Composite material and preparation method thereof, structural member and preparation method thereof, and electronic equipment |
| CN114957965A (en) * | 2022-07-07 | 2022-08-30 | 福建长泰万泰矿物制品有限公司 | High-heat-resistance polyurethane composition, polyurethane disc and preparation method thereof |
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Application publication date: 20120725 |