CN107915964A - A kind of toughening modifying composite material and preparation method thereof - Google Patents

A kind of toughening modifying composite material and preparation method thereof Download PDF

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Publication number
CN107915964A
CN107915964A CN201711269739.2A CN201711269739A CN107915964A CN 107915964 A CN107915964 A CN 107915964A CN 201711269739 A CN201711269739 A CN 201711269739A CN 107915964 A CN107915964 A CN 107915964A
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parts
composite material
glass fiber
polyethylene terephthalate
electric field
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舒春柳
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Sichuan Lizhi Jiuchuang Intellectual Property Operations Ltd
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
    • C08L67/02—Polyesters derived from dicarboxylic acids and dihydroxy 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
    • C08K2201/00—Specific properties of additives
    • C08K2201/002—Physical properties
    • C08K2201/003—Additives being defined by their diameter
    • 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
    • C08K2201/00—Specific properties of additives
    • C08K2201/011—Nanostructured additives
    • 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
    • C08K2201/00—Specific properties of additives
    • C08K2201/016—Additives defined by their aspect ratio
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2312/00—Crosslinking

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

Abstract

The invention discloses a kind of toughening modifying composite material and preparation method thereof, including following parts by weight raw material to be prepared：10 20 parts of nanometer glass fiber, 5 10 parts of modifying agent, 5 10 parts of polyurethane, 10 15 parts of butadiene rubber, 40 50 parts of polyethylene terephthalate, 13 parts of coupling agent, 0.3 0.5 parts of crosslinking agent；The present invention is for composite by the nanometer glass fiber Jing Guo specific aim modification and polyethylene terephthalate, and nanometer glass fiber is set to be dispersed in polyethylene terephthalate system, obtained composite material tensile strength performance is excellent, is conducive to application of the polyethylene terephthalate in more areas.

Description

A kind of toughening modifying composite material and preparation method thereof
Technical field
The present invention relates to modified material field, and in particular to a kind of toughening modifying composite material and preparation method thereof.
Background technology
Polyethylene terephthalate be exchanged by dimethyl terephthalate (DMT) with glycol ester or with terephthalic acid (TPA) with Ethylene glycol esterification first synthesizes bishydroxyethyl terephthalate, then carries out polycondensation reaction again and is made, and belongs to crystal type saturated polyester, is Milky or light yellow, highly crystalline polymer.With excellent mechanical performance, rigidity is high, hardness is big, and water imbibition is small, ruler Very little stability is good, good toughness, impact resistance, rub resistance, creep resistance, and chemical resistance is good.In industries such as automobile, aviation, electronics, machineries In be used widely.
With the continuous improvement that people require material tensile property, the modified poly terephthalic acid second of unstretched enhancing Diester has been difficult to meet demand, thus, stretching enhancing modification is carried out to polyethylene terephthalate and is necessitated.Now to poly- The stretching enhancing modification processing method species of ethylene terephthalate is various, and modified effect is also fine, especially with nanometer The appearance and application of material, the tensile strength increase significant effect of polyethylene terephthalate, make poly terephthalic acid second two Ester can largely be used in more areas, but there is also deficiency.Although nano material has, tensile strength enhancing effect is good, additive amount The advantages of small, but there is also difficulties in dispersion, it is of high cost the defects of.In tensile strength modifying process is carried out, nano material is disperseed Inequality can influence it and stretch enhancing effect, and obtained modified material tensile strength is relatively low, and the production and application to modified material are made Into adverse effect.
The content of the invention
The defects of it is an object of the invention to overcome existing polyethylene terephthalate materials tensile strength poor, there is provided A kind of toughening modifying composite material and preparation method thereof；The present invention is by the nanometer glass fiber Jing Guo specific aim modification with gathering Ethylene terephthalate is for composite, and nanometer glass fiber is dispersed in polyethylene terephthalate system, Obtained composite material tensile strength performance is excellent, is conducive to application of the polyethylene terephthalate in more areas.
In order to realize foregoing invention purpose, the present invention provides a kind of toughening modifying composite material, including following parts by weight Raw material are prepared：10-20 parts of nanometer glass fiber, 5-10 parts of modifying agent, 5-10 parts of polyurethane, 10-15 parts Butadiene rubber, 40-50 parts of polyethylene terephthalate, 1-3 parts of coupling agent, 0.3-0.5 parts of crosslinking agent.
A kind of above-mentioned toughening modifying composite material, can increase resin material tensile strength according to nanometer glass fiber and crosslinking Basic principle, not only by targetedly screening modifying agent, coupling agent and the species of crosslinking agent, to improve nanometer glass fiber Compatibility between polyethylene terephthalate, and nanometer glass fiber is disperseed more in polyethylene terephthalate Uniformly, make nanometer glass fiber more preferable to the tensile strength humidification of polyethylene terephthalate, also by controlling poly- pair The degree of polymerization of polyethylene terephthalate makes the modified composite material reach optimum balance between tensile strength and processability Relation, so that the composite material made is under conditions of with excellent tensile strength, it may have excellent processability, makes it It can be applied in more areas.
A kind of above-mentioned toughening modifying composite material, wherein, a diameter of 1-10nm of the nanometer glass fiber, draw ratio is 2-10 ︰ 1；Nanometer glass fiber draw ratio is bigger, and dispersiveness is poorer, and nanometer glass fiber draw ratio is smaller, to poly- terephthaldehyde The tensile strength humidification of sour second diester is poorer；Preferably, a diameter of 3-5nm of the nanometer glass fiber, draw ratio are 3-6 ︰ 1.
A kind of above-mentioned toughening modifying composite material, wherein, the modifying agent is hydroxyethyl methacrylate and acetyl lemon The mixture of lemon acid tributyl composition；The modifying agent can improve nanometer glass fiber and polyethylene terephthalate Compatibility, and polar group can be formed on nanometer glass fiber surface, beneficial to scattered；Preferably, methyl in the modifying agent The ratio between amount of material of hydroxy-ethyl acrylate and tributyl 2-acetylcitrate is 1 ︰ 1.
A kind of above-mentioned toughening modifying composite material, wherein, the degree of polymerization of butadiene rubber is bigger, then composite material after being crosslinked Tensile strength is poorer, and processability is better, and the polymer of butadiene rubber is smaller, then the tensile strength of composite material is better after being crosslinked, Processability is poorer, therefore, selects the rational butadiene rubber degree of polymerization, is the important means of balanced stretch intensive properties and processability. The degree of polymerization of the butadiene rubber is 200-300；Preferably, the degree of polymerization of the butadiene rubber is 230-270；It is optimal , the degree of polymerization of the butadiene rubber is 250；By preferred, obtained composite material both has excellent tensile strength, With preferable processability, it is adapted to the application in more areas.
Wherein, the polyethylene terephthalate degree of polymerization is 1000-1600；Preferably, the poly- terephthaldehyde The degree of polymerization of sour second diester is 1200-1400；Most preferably, the degree of polymerization of the polyethylene terephthalate is 1300； By preferred, obtained composite material both has excellent tensile strength, it may have preferable processability.
A kind of above-mentioned toughening modifying composite material, wherein, the coupling agent is 3-aminopropyltriethoxysilane；3- Aminopropyltriethoxywerene werene can increase the phase between nanometer glass fiber and polyethylene terephthalate and modifying agent Capacitive, improves the performance of composite material.
Wherein, the crosslinking agent is ethylene glycol dimethacrylate, which can be by two kinds of different polymerization degrees Polymer raw materials are suitably crosslinked, and improve the tensile strength of composite material.
A kind of above-mentioned toughening modifying composite material, wherein, its raw material further includes dispersant, plasticizer, antistatic additive, dye One or more auxiliary agents in toner, brightener；Above-mentioned auxiliary agent can improve the processability of composite material, increase its feature etc. Effect, so as to increase its applicability.
In order to realize foregoing invention purpose, further, present invention also offers a kind of system of toughening modifying composite material Preparation Method, comprises the following steps：
（1）Nanometer glass fiber is handled with coupling agent；
（2）Nanometer glass fiber Jing Guo coupling agent treatment is subjected to cladding processing with modifying agent；
（3）The place for composite in the electric field after mixing by the nanometer glass fiber after cladding and polyethylene terephthalate Reason, obtains mixture；
（4）By mixture and butadiene rubber, crosslinking agent, polyurethane, zinc stearate after mixing in processing for composite, obtain Toughening modifying composite material.
A kind of preparation method of toughening modifying composite material, first carries out coupling processing with coupling agent to nanometer glass fiber, Increase nanometer glass fiber and modifying agent, the compatibility of polyethylene terephthalate；Again with modifying agent to nanometer glass fiber Processing is modified, and polar group is formed on its surface；Finally make nanometer glass fiber surface using external electric field and gather to benzene Polar group polarization in dioctyl phthalate second diester chain, it is powered, by repelling each other between electric charge or attracting principle, make nano-glass fine , also can be bonded with the polar group on polyethylene terephthalate chain while tieing up dispersed, so that nano-glass is fine The tensile strength enhancing effect of dimension is farthest embodied, so as to get modification polyethylene terephthalate tensile strength Significantly improve；The preparation method is simple and reliable, is suitable for extensive, the industrialized production of toughening modifying composite material.
A kind of preparation method of above-mentioned toughening modifying composite material, wherein, it is preferred that step 1 carries out coupling processing process In can use ultrasonic wave aid in；Shaken by the high speed of ultrasonic wave, make nanometer glass fiber dispersiveness more preferable, and to coupling processing With facilitation.
A kind of preparation method of above-mentioned toughening modifying composite material, wherein, the electric field energy described in step 3 produces group Polarization, makes group powered, so as to promote the scattered and bonded effect of nanometer glass fiber, improves modified poly- terephthaldehyde The tensile strength of sour second diester.
Preferably, the electric field strength is 1.5-3.2kv/m；Electric field strength is too small, and polarization effect is weak, to nano-glass The dispersion effect of fiber is poor；Electric field strength is excessive, and polarization effect is too strong, and intermolecular force is too big, and strand produces orientation and moves It is dynamic, arrangement and the bonded performance for having an impact, may be decreased composite material to strand；Most preferably, the electric-field strength Spend for 2.0-2.5kv/m.
Wherein, it is preferred that the electric field is the constant parallel electric field of direction of an electric field；The constant parallel electric field of direction of an electric field Best to the polarization effect of polar group, group intermolecular forces are stablized, and the scattered and bonded promotion to nanometer glass fiber is made Use best results.
Compared with prior art, beneficial effects of the present invention：
1st, composite material of the present invention targetedly screens the species of modifying agent, coupling agent and crosslinking agent, make nanometer glass fiber with Compatibility between polyethylene terephthalate is more preferable, and the dispersiveness in polyethylene terephthalate is more preferable, nanometer glass Glass fiber is more preferable to the tensile strength humidification of polyethylene terephthalate.
2nd, composite material of the present invention makes modification by controlling the degree of polymerization of polyethylene terephthalate and butadiene rubber Composite material afterwards reaches optimum balance relation between tensile strength and processability, so as to get composite material with excellent Tensile strength under conditions of, it may have excellent processability.
3rd, the preparation method of composite material of the present invention, using the polarization of external electric field, can promote nanometer glass fiber to exist Scattered and bonded in polyethylene terephthalate system, the tensile strength enhancing effect of nanometer glass fiber is more preferable, obtains Composite material tensile strength higher.
4th, the preparation method of composite material of the present invention is simple, reliable, is adapted to the extensive, industrial of toughening modifying composite material Metaplasia is produced.
Embodiment
With reference to test example and embodiment, the present invention is described in further detail.But this should not be understood Following embodiment is only limitted to for the scope of the above-mentioned theme of the present invention, it is all that this is belonged to based on the technology that present invention is realized The scope of invention.
Embodiment 1
（1）15 parts of nanometer glass fiber is handled with 2 parts of 3-aminopropyltriethoxysilane；
（2）By the nanometer glass fiber Jing Guo coupling agent treatment 4 parts of hydroxyethyl methacrylate and 4 parts of acetyl tributyl citrate Tributyl carries out cladding processing；
（3）Nanometer glass fiber after cladding is uniformly mixed with the polyethylene terephthalate that 45 parts of the degree of polymerization is 1300 Extruded afterwards in the constant parallel electric field of the direction of an electric field that electric field strength is 2.5kv/m, obtain mixture；
（4）The butadiene rubber, 8 parts of polyurethane, 0.4 part of diformazan that the mixture that step 3 is obtained and 12 parts of the degree of polymerization are 250 Base acrylic acid glycol ester is extruded after mixing, obtains toughening modifying composite material.
Embodiment 2
（1）10 parts of nanometer glass fiber is handled with 1 part of 3-aminopropyltriethoxysilane；
（2）By the nanometer glass fiber Jing Guo coupling agent treatment 2.5 parts of hydroxyethyl methacrylate and 2.5 parts of acetyl lemon Lemon acid tributyl carries out cladding processing；
（3）Nanometer glass fiber after cladding is uniformly mixed with the polyethylene terephthalate that 40 parts of the degree of polymerization is 1600 Extruded afterwards in the electric field for being 3.2kv/m in electric field strength, obtain mixture；
（4）The butadiene rubber, 5 parts of polyurethane, 0.3 part of diformazan that the mixture that step 3 is obtained and 10 parts of the degree of polymerization are 200 Base acrylic acid glycol ester is extruded after mixing, obtains toughening modifying composite material.
Embodiment 3
（1）20 parts of nanometer glass fiber is handled with 3 parts of 3-aminopropyltriethoxysilane；
（2）By the nanometer glass fiber Jing Guo coupling agent treatment 5 parts of hydroxyethyl methacrylate and 5 parts of acetyl tributyl citrate Tributyl carries out cladding processing；
（3）Nanometer glass fiber after cladding is uniformly mixed with the polyethylene terephthalate that 50 parts of the degree of polymerization is 1000 Extruded afterwards in the constant parallel electric field of the direction of an electric field that electric field strength is 1.5kv/m, obtain mixture；
（4）Butadiene rubber that the mixture that step 3 is obtained and 15 parts of the degree of polymerization are 300,10 parts of polyurethane, 0.5 part two Methacrylic acid glycol ester is extruded after mixing, obtains toughening modifying composite material.
Comparative example 1
（1）15 parts of nanometer glass fiber is handled with 2 parts of 3-aminopropyltriethoxysilane；
（2）By the nanometer glass fiber Jing Guo coupling agent treatment and 5 parts of dispersant, 45 parts of the degree of polymerization be 1300 it is poly- to benzene Dioctyl phthalate second diester is extruded in the constant parallel electric field of the direction of an electric field that electric field strength is 2.5kv/m after mixing, Obtain mixture；
（3）The butadiene rubber, 8 parts of polyurethane, 0.4 part of diformazan that the mixture that step 2 is obtained and 12 parts of the degree of polymerization are 250 Base acrylic acid glycol ester is extruded after mixing, obtains composite material.
Comparative example 2
（1）15 parts of nanometer glass fiber is handled with 2 parts of 3-aminopropyltriethoxysilane；
（2）By the nanometer glass fiber Jing Guo coupling agent treatment 4 parts of hydroxyethyl methacrylate and 4 parts of acetyl tributyl citrate Tributyl carries out cladding processing；
（3）By polyethylene terephthalate that the nanometer glass fiber after cladding and 45 parts of the degree of polymerization are 1300,12 parts The butadiene rubber, 8 parts of polyurethane, 0.4 part of ethylene glycol dimethacrylate that the degree of polymerization is 250 are squeezed after mixing Go out, obtain composite material.
Comparative example 3
（1）15 parts of nanometer glass fiber is handled with 2 parts of 3-aminopropyltriethoxysilane；
（2）By the nanometer glass fiber Jing Guo coupling agent treatment with 4 parts of butadiene rubber and 4 parts of tributyl 2-acetylcitrate into The processing of row cladding；
（3）Nanometer glass fiber after cladding is uniformly mixed with the polyethylene terephthalate that 45 parts of the degree of polymerization is 1300 Extruded afterwards in the constant parallel electric field of the direction of an electric field that electric field strength is 2.5kv/m, obtain mixture；
（4）The butadiene rubber, 8 parts of polyurethane, 0.4 part of diformazan that the mixture that step 3 is obtained and 12 parts of the degree of polymerization are 250 Base acrylic acid glycol ester is extruded after mixing, obtains composite material.
Comparative example 4
（1）15 parts of nanometer glass fiber is handled with 2 parts of 3-aminopropyltriethoxysilane；
（2）By the nanometer glass fiber Jing Guo coupling agent treatment 4 parts of hydroxyethyl methacrylate and 4 parts of acetyl tributyl citrate Tributyl carries out cladding processing；
（3）By butadiene rubber that the nanometer glass fiber after cladding and 12 parts of the degree of polymerization are 250,8 parts of polyurethane, 0.4 part Ethylene glycol dimethacrylate, the polyethylene terephthalate that 45 parts of the degree of polymerization is 2000 are after mixing in electric-field strength Spend to be extruded in the constant parallel electric field of the direction of an electric field of 2.5kv/m, obtain composite material.
Comparative example 5
（1）15 parts of nanometer glass fiber is handled with 2 parts of 3-aminopropyltriethoxysilane；
（2）By the nanometer glass fiber Jing Guo coupling agent treatment 4 parts of hydroxyethyl methacrylate and 4 parts of acetyl tributyl citrate Tributyl carries out cladding processing；
（3）Nanometer glass fiber after cladding is uniformly mixed with the polyethylene terephthalate that 45 parts of the degree of polymerization is 900 Extruded afterwards in the constant parallel electric field of the direction of an electric field that electric field strength is 2.5kv/m, obtain mixture；
（4）The butadiene rubber, 8 parts of polyurethane, 0.4 part of diformazan that the mixture that step 3 is obtained and 12 parts of the degree of polymerization are 180 Base acrylic acid glycol ester is extruded after mixing, obtains composite material.
By the composite material in above-described embodiment 1-3 and comparative example 1-5, performance detection is carried out, record data are as follows：
Performance Tensile strength（MPa） Elongation at break（%） Processability
Embodiment 1 137 76 ++++
Embodiment 2 134 89 ++++
Embodiment 3 136 63 ++++
Comparative example 1 108 58 ++++
Comparative example 2 113 42 ++++
Comparative example 3 115 45 ++++
Comparative example 4 123 68 ++++
Comparative example 5 136 31 ++
Polyethylene terephthalate 75 62 +++
Note："+" is more, illustrates that performance is better.
The toughening modifying composite material of the present invention being prepared in embodiment 1-3, which receives, to be understood to above-mentioned analysis of experimental data Rice glass fibre is uniformly dispersed, and good with the compatibility of polyethylene terephthalate, composite material tensile strength is good, extension at break Rate is high, and processability is good；And in comparative example 1, modifying agent is not used processing is modified to nanometer glass fiber, although adding point Powder, but nanometer glass fiber dispersion effect is poor, the poor compatibility with polyethylene terephthalate, and the stretching of composite material is strong Degree and elongation at break significantly reduce；Not processing for composite in the electric field, nanometer glass fiber dispersion effect in comparative example 2 Difference, the tensile strength and elongation at break of composite material significantly reduce；Modifying agent is not the application defined in comparative example 3, Nanometer glass fiber dispersion effect is poor, and the tensile strength and elongation at break of composite material significantly reduce；It is crosslinked in comparative example 4 anti- Should equally carry out in the electric field, electric field has a negative impact cross-linking reaction, so as to get the tensile strength of composite material and disconnected Split elongation reduction；The polyethylene terephthalate and the butadiene rubber degree of polymerization used in comparative example 5 is too small, although after compound Tensile strength increased, but its elongation at break and processability significantly reduce, and be unfavorable for the application of composite material.

Claims (10)

1. a kind of toughening modifying composite material, it is characterised in that be prepared including following parts by weight raw material：10-20 parts Nanometer glass fiber, 5-10 parts of modifying agent, 5-10 parts of polyurethane, 10-15 parts of butadiene rubber, 40-50 parts poly- to benzene Dioctyl phthalate second diester, 1-3 parts of coupling agent, 0.3-0.5 parts of crosslinking agent；The modifying agent is hydroxyethyl methacrylate and second The mixture of acyl tributyl citrate composition；The coupling agent is 3-aminopropyltriethoxysilane, and the crosslinking agent is two Methacrylic acid glycol ester；The degree of polymerization of the butadiene rubber is 200-300；The polyethylene terephthalate degree of polymerization For 1000-1600.
2. composite material according to claim 1, it is characterised in that hydroxyethyl methacrylate and second in the modifying agent The ratio between amount of material of acyl tributyl citrate is 1 ︰ 1.
3. composite material according to claim 1, it is characterised in that the degree of polymerization of the butadiene rubber is 230-270.
4. composite material according to claim 3, it is characterised in that the degree of polymerization of the butadiene rubber is 250.
5. composite material according to claim 1, it is characterised in that the polyethylene terephthalate degree of polymerization is 1200-1400。
6. composite material according to claim 5, it is characterised in that the polyethylene terephthalate degree of polymerization is 1300。
7. a kind of preparation method of the composite material as described in claim any one of 1-6, it is characterised in that comprise the following steps：
（1）Nanometer glass fiber is handled with coupling agent；
（2）Nanometer glass fiber Jing Guo coupling agent treatment is subjected to cladding processing with modifying agent；
（3）The place for composite in the electric field after mixing by the nanometer glass fiber after cladding and polyethylene terephthalate Reason, obtains mixture；
（4）By mixture and butadiene rubber, polyurethane, crosslinking agent after mixing in processing for composite, toughening modifying is obtained Composite material.
8. preparation method according to claim 7, it is characterised in that step（3）Middle electric field strength is 1.5-3.2kv/m.
9. preparation method according to claim 8, it is characterised in that step（3）Middle electric field strength is 2.0-2.5kv/m.
10. preparation method according to claim 7, it is characterised in that step（3）Middle electric field is put down for direction of an electric field is constant Row electric field.
CN201711269739.2A 2017-12-05 2017-12-05 A kind of toughening modifying composite material and preparation method thereof Withdrawn CN107915964A (en)

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Application Number Priority Date Filing Date Title
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Application publication date: 20180417