CN104177713A - Preparation method of POSS (polyhedral oligomeric silsesquioxane) intercalated rectorite/rubber composite material - Google Patents

Preparation method of POSS (polyhedral oligomeric silsesquioxane) intercalated rectorite/rubber composite material Download PDF

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Publication number
CN104177713A
CN104177713A CN201410423414.5A CN201410423414A CN104177713A CN 104177713 A CN104177713 A CN 104177713A CN 201410423414 A CN201410423414 A CN 201410423414A CN 104177713 A CN104177713 A CN 104177713A
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poss
rec
preparation
rectorite leng
rubber
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龙金林
侯琳熙
易思利
凌坤华
张祥洲
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JIANGSU STERRIC CHEMICAL INDUSTRY Co Ltd
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JIANGSU STERRIC CHEMICAL INDUSTRY Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
    • C08K13/06—Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/02—Elements
    • C08K3/06—Sulfur
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/34—Silicon-containing compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/04—Oxygen-containing compounds
    • C08K5/14—Peroxides
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00—Use of pretreated ingredients
    • C08K9/04—Ingredients treated with organic substances
    • C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/08—Stabilised against heat, light or radiation or oxydation

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The invention discloses a preparation method of a POSS (polyhedral oligomeric silsesquioxane) intercalated rectorite (REC)/rubber composite material. The preparation method comprises the following steps: firstly, taking aminopropylisobutyl POSS (POSS-NH2) as an intercalator, and organically modifying REC to prepare POSS intercalated rectorite (POSS-REC); secondly, preparing POSS-REC/ethylene-propylene-diene monomer (POSS-REC/EPDM), POSS-REC/natural rubber (POSS-REC/NR) and POSS-REC/ethylene vinyl acetate (POSS-REC/EVA) composite materials by adopting a mechanical blending method. The preparation method is simple in process and mild in operation condition. Compared with pure vulcanized rubber, the tensile strength of the POSS-REC/EPDM, POSS-REC/NR and POSS-REC/EVA composite materials is enhanced by 245.5%, 191.7% and 233.7% respectively, and the break elongation rates of the POSS-REC/EPDM, POSS-REC/NR and POSS-REC/EVA composite materials are increased by 113.3%, 82.2% and 113.2% respectively.

Description

The preparation method of POSS intercalation rectorite leng/rubber composite
Technical field
The present invention relates to the preparation method of matrix material, be specifically related to a kind of preparation method of POSS intercalation rectorite leng/rubber composite.
Background technology
Clay of laminar silicate is as a kind of natural mineral, environmental friendliness, and its composite property of preparing as filler is good, has huge commercial value.Rectorite leng is a kind of layer aluminosilicate mineral of rule, has cationic exchange, water swellability, dispersiveness, thermostability etc.Yet rectorite leng interlayer chemical micro-environment is wetting ability, is unfavorable for the insertion of non-polar monomer or polymer macromolecule, easily cause and be separated, thereby affect the performance of matrix material, therefore need to carry out organically-modified to rectorite leng.At present, conventional organic modifiers is organosilicon, chain alkyl ammonium salt, amino acid etc.
POSS(multiaspect oligomeric silsesquioxanes) have three-dimensional inorganic-organic hybridization structure, its chemical constitution is (RSiO 1.5) n, be the spherical of 0.7 ~ 3 nm, its reaction multifunctionality and excellent performance (resistance to elevated temperatures, low sticky low density, high modulus and strength etc.) cause the great interest of people.POSS not only can change the wetting ability of its microenvironment as the organic modifiers of silicate clay, improves the thermostability of organic clay, also can make organic clay obtain larger interlamellar spacing, be conducive to make be uniformly dispersed, the composite polymeric materials of excellent property.
Rubber is being brought into play very important effect in modern industry, military affairs and daily life.Wherein, terpolymer EP rubber (EPDM) is the terpolymer of ethene, propylene and non-conjugated diene hydrocarbon, and its molecular chain is submissive, there is no polar group, belongs to saturated carbon chains rubber.Chemical stability, flexible resistance, rebound resilience and lower temperature resistance that terpolymer EP rubber is good, be widely used in the fields such as automotive industry, electric wire, sealing material and heat-resisting goods.Natural rubber (NR) is a kind of general elastomeric material, has the performances such as good elasticity, insulativity, resistance to medium and wear resistance because of it, applies to widely the fields such as automotive industry, electric wire, medical and health and articles for daily use.Particularly, at tire industry, the usage quantity of natural rubber accounts for it and uses the over half of total amount.Ethylene-vinyl acetate (being called for short EVA) is to be formed by ethene (E) and two kinds of monomer copolymerizations of vinyl acetate (Va), is a kind of conventional macromolecular material, is widely used in the fields such as daily necessities, foam material, hot melt adhesive, electric wire.
Summary of the invention
The object of the invention is to: a kind of preparation method of POSS intercalation rectorite leng/rubber composite is provided, and technique is simple, operational condition is gentle, and tensile strength and the elongation at break of matrix material are improved.
Technical solution of the present invention is that this preparation method comprises the following steps:
(1) preparation of POSS intercalation rectorite leng: deionized water is added in container, under agitation a certain amount of sodium base rectorite leng REC is added to the water, under normal temperature, vigorous stirring is 4 hours fully disperses and swelling sodium base rectorite leng in water, obtains rectorite leng suspension; In another container, under stirring by POSS-NH 2be dissolved in THF completely, then add the hydrochloric acid of mass concentration 10 %, obtain POSS-NH 2mixing solutions; By POSS-NH 2mixing solutions is added in rectorite leng suspension, under normal temperature, continues stirring reaction to the specified time, gets the turbid liquid of upper strata grey, suction filtration and with THF and deionized water wash to solution without free Cl -till; By filter solid 120 ℃ of vacuum-dryings, spend the night, ground 200 mesh sieves, obtain POSS intercalation rectorite leng (POSS-REC);
(2) preparation of matrix material: rubber is put into mill normal temperature and plasticate completely, evenly wrap roller, adjust roll spacing, add the POSS-REC of predetermined amount, open refining under normal temperature evenly; Take a certain amount of vulcanizing agent and join in above-mentioned sizing material, and in mill, open refining for being applicable to the size of forming mould;
(3) moulding of matrix material: step (2) was opened to the bin aging that refined after 6 hours, puts into vulcanizing press, under curing temperature by sizing material at 2 MPa precompressed 30 s, under 15 MPa and curing temperature, vulcanize to sulfurizing time more subsequently, take out, cooling, obtain matrix material.
Wherein, described POSS-NH 2with the mol ratio of REC be 1:1 ~ 3:1.
Wherein, described hydrochloric acid and POSS-NH 2mol ratio be 0.5:1 ~ 2.5:1.
Wherein, the reaction times described in step (1) is 6 h ~ 48 h.
Wherein, described rubber comprises terpolymer EP rubber, natural rubber, ethylene vinyl acetate copolymer.
Wherein, the massfraction of described POSS-REC in matrix material is 1% ~ 5%.
Wherein, for terpolymer EP rubber, described vulcanizing agent is dicumyl peroxide; For natural rubber or ethylene vinyl acetate copolymer, described vulcanizing agent is sulphur.
Wherein, described rubber: vulcanizing agent=100:1 ~ 100:1.5.
Wherein, curing temperature is 160 ℃ ~ 165 ℃.
The invention has the beneficial effects as follows:
1, rubber, POSS intercalation rectorite leng, vulcanizing agent being opened to refining mixes, the chemical compatibility of rubber and POSS intercalation rectorite leng makes out to produce in refining process strong shearing force, rubber molecule enters into organic rectorite sheet interlayer, its interlamellar spacing expands, and opens refining sizing material and vulcanizes and make the nano composite material with different lamella dispersed textures under proper temperature.
2, with the higher POSS-NH of thermostability 2for properties-correcting agent, adopt solution intercalation method to carry out modification to rectorite leng, prepared POSS intercalation rectorite leng, POSS intercalation rectorite leng has larger interlamellar spacing and good thermostability, is the good additive of preparing polymer composites.
3, take POSS intercalation rectorite leng is filler, tensile strength, elongation at break and the thermostability of the polymer composites of preparation are all significantly improved, the tensile strength of POSS-REC/EPDM, POSS-REC/NR and POSS-REC/EVA matrix material has improved respectively 245.5 %, 191.7 % and 233.7 %, elongation at break has improved respectively 113.3 %, 82.2 % and 113.2 %, is conducive to widen range of application and the value of corresponding polymkeric substance.
Accompanying drawing explanation
Fig. 1 is that the POSS intercalation rectorite leng of embodiment 1 preparation contrasts figure with the infrared spectra of raw material.
Fig. 2 is that the POSS intercalation rectorite leng of embodiment 1 preparation contrasts figure with the XRD of raw material.
Fig. 3 is the TEM figure of terpolymer EP rubber/POSS-Rec matrix material (POSS-REC content is 3 %) of embodiment 7 preparations.
Fig. 4 is the TEM figure of terpolymer EP rubber/POSS-Rec matrix material (POSS-REC content is 5 %) of embodiment 8 preparations.
Fig. 5 is the content of POSS-REC and the graph of a relation of tensile strength in the POSS-REC/EPDM matrix material of embodiment 7 preparation.
Fig. 6 is the POSS-REC/NR matrix material transmission electron microscope picture of embodiment 9 preparations.
Fig. 7 is the content of POSS-REC/NR matrix material POSS-REC and the graph of a relation of tensile strength.
Fig. 8 is POSS-REC/EVA matrix material transmission electron microscope picture.
Embodiment
Below in conjunction with specific embodiment, technical scheme of the present invention is described in further detail, these embodiment can not be interpreted as it is the restriction to technical scheme.
The preparation of embodiment 1(POSS intercalation rectorite leng): deionized water is added in container, under agitation a certain amount of sodium base rectorite leng REC is added to the water, under normal temperature, vigorous stirring is 4 hours, and sodium base rectorite leng is fully disperseed and swelling in water, obtains rectorite leng suspension; In another container, under stirring by POSS-NH 2be dissolved in THF completely, then add the hydrochloric acid of mass concentration 10 %, obtain POSS-NH 2mixing solutions; By POSS-NH 2mixing solutions is added in rectorite leng suspension, under normal temperature, continues stirring reaction to the specified time, gets the turbid liquid of upper strata grey, suction filtration and with THF and deionized water wash to solution without free Cl -till; By filter solid 120 ℃ of vacuum-dryings, spend the night, ground 200 mesh sieves, obtain POSS intercalation rectorite leng (POSS-REC); Wherein, POSS-NH 2with the mol ratio of REC be 2.5:1, hydrochloric acid and POSS-NH 2mol ratio be 1.5:1, the reaction times is 24h.
The preparation of embodiment 2 ~ 6(POSS intercalation rectorite leng): concrete steps are identical with embodiment 1, condition and the results are summarized in table 1.
The impact of table 1 preparation condition on carbon element content in POSS-REC
The preparation of embodiment 7:POSS-REC/EPDM matrix material: terpolymer EP rubber is put into mill normal temperature and plasticate completely, evenly wrap roller, adjust roll spacing, add the POSS-REC of predetermined amount, open refining under normal temperature evenly; Take a certain amount of vulcanizing agent dicumyl peroxide and join in above-mentioned sizing material, and in mill, open refining for being applicable to the size of forming mould; By opening the bin aging that refined after 6 hours, put into vulcanizing press, under curing temperature by sizing material at 2 MPa precompressed 30 s, under 15 MPa and curing temperature, vulcanize to sulfurizing time more subsequently, take out, cooling, obtain POSS-REC/EPDM matrix material; Wherein, the massfraction of POSS-REC in matrix material is 3%, rubber: vulcanizing agent=100:1.25, and curing temperature is 160 ℃.
Embodiment 8: concrete steps are identical with embodiment 7, and the add-on of POSS-SEC is 5%, rubber: vulcanizing agent=100:1.5, and curing temperature is 165 ℃.
The preparation of embodiment 9:POSS-REC/NR matrix material: natural rubber is put into mill normal temperature and plasticate completely, evenly wrap roller, adjust roll spacing, add the POSS-REC of predetermined amount, open refining under normal temperature evenly; Take a certain amount of vulcanizing agent sulphur and join in above-mentioned sizing material, and in mill, open refining for being applicable to the size of forming mould; By opening the bin aging that refined after 6 hours, put into vulcanizing press, under curing temperature by sizing material at 2 MPa precompressed 30 s, under 15 MPa and curing temperature, vulcanize to sulfurizing time more subsequently, take out, cooling, obtain POSS-REC/NR matrix material; Wherein, the massfraction of POSS-REC in matrix material is 1%, rubber: vulcanizing agent=100:1, and curing temperature is 162 ℃.
The preparation of embodiment 10:POSS-REC/EVA matrix material: ethylene vinyl acetate copolymer is put into mill normal temperature and plasticate completely, evenly wrap roller, adjust roll spacing, add the POSS-REC of predetermined amount, open refining under normal temperature evenly; Take a certain amount of vulcanizing agent sulphur and join in above-mentioned sizing material, and in mill, open refining for being applicable to the size of forming mould; By opening the bin aging that refined after 6 hours, put into vulcanizing press, under curing temperature by sizing material at 2MPa precompressed 30s, under 15MPa and curing temperature, vulcanize to sulfurizing time more subsequently, take out, cooling, obtain POSS-REC/EVA matrix material; Wherein, the massfraction of POSS-REC in matrix material is 3%, rubber: vulcanizing agent=100:1.5, and curing temperature is 160 ℃.

Claims (9)

  1. The preparation method of 1.POSS intercalation rectorite leng/rubber composite, is characterized in that this preparation method comprises the following steps:
    (1) preparation of POSS intercalation rectorite leng: deionized water is added in container, under agitation a certain amount of sodium base rectorite leng REC is added to the water, under normal temperature, vigorous stirring is 4 hours fully disperses and swelling sodium base rectorite leng in water, obtains rectorite leng suspension; In another container, under stirring by POSS-NH 2be dissolved in THF completely, then add the hydrochloric acid of mass concentration 10 %, obtain POSS-NH 2mixing solutions; By POSS-NH 2mixing solutions is added in rectorite leng suspension, under normal temperature, continues stirring reaction to the specified time, gets the turbid liquid of upper strata grey, suction filtration and with THF and deionized water wash to solution without free Cl -till; By filter solid 120 ℃ of vacuum-dryings, spend the night, ground 200 mesh sieves, obtain POSS intercalation rectorite leng (POSS-REC);
    (2) preparation of matrix material: rubber is put into mill normal temperature and plasticate completely, evenly wrap roller, adjust roll spacing, add the POSS-REC of predetermined amount, open refining under normal temperature evenly; Take a certain amount of vulcanizing agent and join in above-mentioned sizing material, and in mill, open refining for being applicable to the size of forming mould;
    (3) moulding of matrix material: step (2) was opened to the bin aging that refined after 6 hours, puts into vulcanizing press, under curing temperature by sizing material at 2 MPa precompressed 30 s, under 15 MPa and curing temperature, vulcanize to sulfurizing time more subsequently, take out, cooling, obtain matrix material.
  2. 2. the preparation method of POSS intercalation rectorite leng/rubber composite according to claim 1, is characterized in that: described POSS-NH 2with the mol ratio of REC be 1:1 ~ 3:1.
  3. 3. the preparation method of POSS intercalation rectorite leng/rubber composite according to claim 1, is characterized in that: described hydrochloric acid and POSS-NH 2mol ratio be 0.5:1 ~ 2.5:1.
  4. 4. the preparation method of POSS intercalation rectorite leng/rubber composite according to claim 1, is characterized in that: the reaction times described in step (1) is 6 h ~ 48 h.
  5. 5. the preparation method of POSS intercalation rectorite leng/rubber composite according to claim 1, is characterized in that: described rubber comprises terpolymer EP rubber, natural rubber, ethylene vinyl acetate copolymer.
  6. 6. the preparation method of POSS intercalation rectorite leng/rubber composite according to claim 1, is characterized in that: the massfraction of described POSS-REC in matrix material is 1% ~ 5%.
  7. 7. the preparation method of POSS intercalation rectorite leng/rubber composite according to claim 5, is characterized in that: for terpolymer EP rubber, described vulcanizing agent is dicumyl peroxide; For natural rubber or ethylene vinyl acetate copolymer, described vulcanizing agent is sulphur.
  8. 8. the preparation method of POSS intercalation rectorite leng/rubber composite according to claim 7, is characterized in that: described rubber: vulcanizing agent=100:1 ~ 100:1.5.
  9. 9. the preparation method of POSS intercalation rectorite leng/rubber composite according to claim 1, is characterized in that: curing temperature is 160 ℃ ~ 165 ℃.
CN201410423414.5A 2014-08-26 2014-08-26 Preparation method of POSS (polyhedral oligomeric silsesquioxane) intercalated rectorite/rubber composite material Pending CN104177713A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105037918A (en) * 2015-09-10 2015-11-11 福州大学 Organic modified rectorite/EVA composite foam material and preparation method and application thereof
CN109251423A (en) * 2018-09-13 2019-01-22 天津大学 Trap based on POSS modified EPT rubber regulates and controls method
CN109294077A (en) * 2018-09-13 2019-02-01 天津大学 Electric branch suppressing method based on POSS regulation ethylene propylene diene rubber
CN113930169A (en) * 2021-11-01 2022-01-14 南京工程学院 Heat-resistant EVA (ethylene vinyl acetate) adhesive film and preparation method thereof

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101649078A (en) * 2009-09-15 2010-02-17 哈尔滨工业大学 Hydrogenated nitrile-butadiene rubber modified by rectorite and preparation method thereof
CN102229748A (en) * 2011-04-15 2011-11-02 湖北飞宏新材料科技有限公司 Organic rectorite modified fluorosilicone rubber sealing and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101649078A (en) * 2009-09-15 2010-02-17 哈尔滨工业大学 Hydrogenated nitrile-butadiene rubber modified by rectorite and preparation method thereof
CN102229748A (en) * 2011-04-15 2011-11-02 湖北飞宏新材料科技有限公司 Organic rectorite modified fluorosilicone rubber sealing and preparation method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
张祥洲 等: "POSS-NH2自组装改性累托石／EPDM橡胶复合材料的制备与性能研究", 《材料导报》 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105037918A (en) * 2015-09-10 2015-11-11 福州大学 Organic modified rectorite/EVA composite foam material and preparation method and application thereof
CN109251423A (en) * 2018-09-13 2019-01-22 天津大学 Trap based on POSS modified EPT rubber regulates and controls method
CN109294077A (en) * 2018-09-13 2019-02-01 天津大学 Electric branch suppressing method based on POSS regulation ethylene propylene diene rubber
CN113930169A (en) * 2021-11-01 2022-01-14 南京工程学院 Heat-resistant EVA (ethylene vinyl acetate) adhesive film and preparation method thereof

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Application publication date: 20141203