CN107964237A - A kind of preparation method of modified glass-fiber polycarbafil type aqueous polyurethane anti-static material - Google Patents

A kind of preparation method of modified glass-fiber polycarbafil type aqueous polyurethane anti-static material Download PDF

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Publication number
CN107964237A
CN107964237A CN201711427221.7A CN201711427221A CN107964237A CN 107964237 A CN107964237 A CN 107964237A CN 201711427221 A CN201711427221 A CN 201711427221A CN 107964237 A CN107964237 A CN 107964237A
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fiber
weight
parts
modified glass
polycarbafil
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苗则波
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WUHU CHANGJIANG JACK-UP EQUIPMENT Co Ltd
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WUHU CHANGJIANG JACK-UP EQUIPMENT Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
    • C08J5/06—Reinforcing macromolecular compounds with loose or coherent fibrous material using pretreated fibrous materials
    • C08J5/08—Reinforcing macromolecular compounds with loose or coherent fibrous material using pretreated fibrous materials glass fibres
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/30—Low-molecular-weight compounds
    • C08G18/32—Polyhydroxy compounds; Polyamines; Hydroxyamines
    • C08G18/3203—Polyhydroxy compounds
    • C08G18/3206—Polyhydroxy compounds aliphatic
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/30—Low-molecular-weight compounds
    • C08G18/34—Carboxylic acids; Esters thereof with monohydroxyl compounds
    • C08G18/348—Hydroxycarboxylic acids
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40—High-molecular-weight compounds
    • C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
    • C08G18/44—Polycarbonates
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
    • C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
    • C08G18/6633—Compounds of group C08G18/42
    • C08G18/6637—Compounds of group C08G18/42 with compounds of group C08G18/32 or polyamines of C08G18/38
    • C08G18/664—Compounds of group C08G18/42 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/3203
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
    • C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
    • C08G18/6633—Compounds of group C08G18/42
    • C08G18/6659—Compounds of group C08G18/42 with compounds of group C08G18/34
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2375/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
    • C08J2375/04—Polyurethanes
    • C08J2375/06—Polyurethanes from polyesters
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2429/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
    • C08J2429/02—Homopolymers or copolymers of unsaturated alcohols
    • 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
    • C08K2201/00—Specific properties of additives
    • C08K2201/017—Additives being an antistatic agent
    • 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
    • C08K3/04—Carbon
    • 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
    • C08K7/00—Use of ingredients characterised by shape
    • C08K7/02—Fibres or whiskers
    • C08K7/04—Fibres or whiskers inorganic
    • C08K7/14—Glass
    • 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
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00—Use of pretreated ingredients
    • C08K9/10—Encapsulated ingredients

Abstract

The invention discloses a kind of preparation method of modified glass-fiber polycarbafil type aqueous polyurethane anti-static material, by konjaku flour carry out pyrohydrolysis after with hydrolyzate cladding graphite oxide it is for composite after, with polycarbonate glycol, different methyl diphenylene diisocyanate is main synthesis material, synthesize with hydrolysis konjaku flour oxidized graphite composite material after cross-linked polycarbonate type Water-based polyurethane elastomer is mixed with modified glass-fiber and be granulated, hydrolysis konjaku flour oxidized graphite composite material prepared by the present invention is as Polymeric anti-static agent, compatibility improves after glass fibre carries out coupling modifier, POLYPROPYLENE GLYCOL and modified glass-fiber, synergistic effect is produced between antioxidant, the antistatic and wearability of the material of preparation is good, mechanical performance is homogeneous.

Description

A kind of modified glass-fiber polycarbafil type aqueous polyurethane anti-static material Preparation method
Technical field
The present invention relates to polyurethane material field, is exactly that a kind of modified glass-fiber polycarbafil type is water-based The preparation method of polyurethane electrostatic resistance material.
Background technology
Makrolon can simply be divided into several classes such as aliphatic, aromatic series, in automobile, build as a kind of thermoplastic polymer Build, have a wide range of applications in the industry such as electric appliance.Because its is nontoxic, transparent, corrosion resistant candle property is good, it is also applied in daily life, than Such as safety glass, CD material.
Aqueous polyurethane is a kind of special polyurethane material, dissolved in water by polyurethane it is scattered formed, Ke Yizuo It is increasingly deep with people's environmental consciousness for a variety of base resins using form, such as aqueous polyurethane coating, adhesive etc. Change and receive the extensive favor of people, this requires aqueous polyurethane must be from raw material selection to the ring of each preparation process Section is all green, environmental-friendly.The researcher of polyurethane has done substantial amounts of polyurethane-modified work for this：Such as acrylic acid The methods of ester modified, epoxy resin modification and use physical blending, is modified.But in these method of modifying, still or More or less there is the material being harmful to environment and people, do not solved the problems, such as from source.Therefore, environment-friendly type is researched and developed Polyurethane material is by as the Main way of modified aqueous polyurethane from now on.
Zhang Yunran exists《The preparation of glucose-acrylate modified polycarbonate waterborne polyurethane lotion and performance study》 By polycarbonate glycol, isophorone diisocyanate it is main synthesis material in one text, dihydromethyl propionic acid is hydrophilic expansion Chain agent, 1,4-butanediol are small molecule chain extender, synthesize polycarbonate waterborne polyurethane lotion, with glucose to poly- carbonic acid Ester type polyurethane is modified, and they are characterized, and show that the material comprehensive performance prepared is preferable, but with to material The requirement of material improves, and the performance of polycarbonate waterborne polyurethane in itself has been unable to meet demand, and this requires the high property of material Energyization.
The content of the invention
The defects of the object of the invention is exactly to make up prior art, improves antistatic and the shortcomings that wear no resistance, and carries For a kind of preparation method of modified glass-fiber polycarbafil type aqueous polyurethane anti-static material.
The present invention is achieved by the following technical solutions：
A kind of preparation method of modified glass-fiber polycarbafil type aqueous polyurethane anti-static material, including following step Suddenly：
（1）4-5 parts by weight konjaku flours are dissolved in 100-110 parts by weight water and are placed on closed container, are sealed, heat most 150- After being cooled down after when 180 DEG C of holding reaction 2-4 are small, and 1-2 parts by weight graphite oxides are added, ultrasonic disperse 30-40 minutes, adds When most 150-180 DEG C of heat keeps reaction 3-4 small, after cooling, hydrolysis konjaku flour-oxidized graphite composite material is obtained；
（2）By 25-30 weight part polycarbonate dihydric alcohol drying and dehydratings 12-24 it is small when after, be slowly added to 20-25 diphenyl methanes Diisocyanate, and 0.02-1 parts by weight dibutyl tin laurates, in nitrogen atmosphere after 80-85 DEG C of reaction 15-20 minutes, When reaction 3-4 is small after addition proper amount of acetone dilution, 60-70 DEG C is cooled to, adds 10-20 parts by weight dihydromethyl propionic acid and N- first It is compound that mixture, 1,4 butanediol of 5-7 parts by weight and the 4-5.5 parts by weight of base -2-Pyrrolidone hydrolyze konjaku flour-graphite oxide When material reaction 1-12 is small, it is stand-by to obtain cross-linked polycarbonate type Water-based polyurethane elastomer；
（3）2-3 parts by weight silane coupling agents are dissolved in appropriate absolute ethyl alcohol, the glass of 5-8 parts by weight is added in 50-70 DEG C of water-bath Glass fiber, uniform stirring 2-6h, is dried in vacuo 8-16h, obtains modified glass-fiber；
（4）By cross-linked polycarbonate type Water-based polyurethane elastomer, 2-5 parts by weight of polypropylene alcohol, modified glass-fiber, 1-2 weights Part antioxidant mixing high-speed stirred is measured until after uniformly, extruding pelletization, it is water-based to obtain modified glass-fiber polycarbafil type Polyurethane electrostatic resistance material.
Step（1）Described is cooled to be cooled down with cold water.
Step（2）The dihydromethyl propionic acid and the mixture of n-methyl-2-pyrrolidone for dihydromethyl propionic acid with N-methyl-2-pyrrolidone（0.8-1）:1 mixing.
Step（4）The antioxidant is antioxidant 1010, one kind in irgasfos 168.
It is an advantage of the invention that：
The present invention by konjaku flour carry out pyrohydrolysis after with hydrolyzate cladding graphite oxide it is for composite after, with makrolon two Alcohol, different methyl diphenylene diisocyanate are main synthesis material, and dibutyl tin laurate is catalyst, dihydromethyl propionic acid For hydrophilic monomer, 1,4-butanediol is small molecule chain extender, and n-methyl-2-pyrrolidone and acetone are thinner, with hydrolysis Konjaku flour-oxidized graphite composite material synthesizes cross-linked polycarbonate type Water-based polyurethane elastomer and is mixed with modified glass-fiber After be granulated, hydrolysis konjaku flour-oxidized graphite composite material for preparing of the present invention hydrolyzes at the same time as Polymeric anti-static agent Konjaku flour can reduce the influence to material mechanical performance, after glass fibre carries out coupling modifier as the crosslinking agent of polymer Compatibility improves, and produces synergistic effect between POLYPROPYLENE GLYCOL and modified glass-fiber, antioxidant, the material of preparation antistatic and Wearability is good, and mechanical performance is homogeneous.
Embodiment
A kind of preparation method of modified glass-fiber polycarbafil type aqueous polyurethane anti-static material, including it is following Step：
（1）4.5 parts by weight konjaku flours are dissolved in 105 parts by weight water and are placed on closed container, are sealed, heat most 165 DEG C holdings React 3 it is small when after cooled down after, and add 1.5 parts by weight graphite oxides, ultrasonic disperse 35 minutes, heat most 165 DEG C guarantor Hold reaction 3.5 it is small when, after cooling, obtain hydrolysis konjaku flour-oxidized graphite composite material；
（2）By 28 weight part polycarbonate dihydric alcohol drying and dehydratings 18 it is small when after, be slowly added to 22 diphenylmethane diisocyanates Ester, and 0.08 parts by weight dibutyl tin laurate, in nitrogen atmosphere after 83 DEG C of reactions 18 minutes, adds proper amount of acetone dilution When reaction 3.5 is small afterwards, be cooled to 65 DEG C, add 18 parts by weight dihydromethyl propionic acids and n-methyl-2-pyrrolidone mixture, When 6 parts by weight Isosorbide-5-Nitrae butanediols and small 4.5 parts by weight hydrolysis konjaku flour-oxidized graphite composite material reaction 8, poly- carbonic acid must be crosslinked Ester type Water-based polyurethane elastomer is stand-by；
（3）2.5 parts by weight silane coupling agents are dissolved in appropriate absolute ethyl alcohol, the glass fibers of 7 parts by weight are added in 60 DEG C of water-baths Dimension, when uniform stirring 4 is small, when vacuum drying 12 is small, obtains modified glass-fiber, stand-by；
（4）By cross-linked polycarbonate type Water-based polyurethane elastomer, 3 parts by weight of polypropylene alcohol, modified glass-fiber, 1.5 weight For part antioxidant mixing high-speed stirred until after uniformly, extruding pelletization, it is water-based poly- to obtain modified glass-fiber polycarbafil type Urethane anti-static material.
Step（1）Described is cooled to be cooled down with cold water.
Step（2）The dihydromethyl propionic acid and the mixture of n-methyl-2-pyrrolidone for dihydromethyl propionic acid with N-methyl-2-pyrrolidone（1:1 mixing.
Step（4）The antioxidant is antioxidant 1010.

Claims (4)

1. a kind of preparation method of modified glass-fiber polycarbafil type aqueous polyurethane anti-static material, its feature exist In comprising the following steps：
（1）4-5 parts by weight konjaku flours are dissolved in 100-110 parts by weight water and are placed on closed container, are sealed, heat most 150- After being cooled down after when 180 DEG C of holding reaction 2-4 are small, and 1-2 parts by weight graphite oxides are added, ultrasonic disperse 30-40 minutes, adds When most 150-180 DEG C of heat keeps reaction 3-4 small, after cooling, hydrolysis konjaku flour-oxidized graphite composite material is obtained；
（2）By 25-30 weight part polycarbonate dihydric alcohol drying and dehydratings 12-24 it is small when after, be slowly added to 20-25 diphenyl methanes Diisocyanate, and 0.02-1 parts by weight dibutyl tin laurates, in nitrogen atmosphere after 80-85 DEG C of reaction 15-20 minutes, When reaction 3-4 is small after addition proper amount of acetone dilution, 60-70 DEG C is cooled to, adds 10-20 parts by weight dihydromethyl propionic acid and N- first It is compound that mixture, 1,4 butanediol of 5-7 parts by weight and the 4-5.5 parts by weight of base -2-Pyrrolidone hydrolyze konjaku flour-graphite oxide When material reaction 1-12 is small, it is stand-by to obtain cross-linked polycarbonate type Water-based polyurethane elastomer；
（3）2-3 parts by weight silane coupling agents are dissolved in appropriate absolute ethyl alcohol, the glass of 5-8 parts by weight is added in 50-70 DEG C of water-bath Glass fiber, uniform stirring 2-6h, is dried in vacuo 8-16h, obtains modified glass-fiber；
（4）By cross-linked polycarbonate type Water-based polyurethane elastomer, 2-5 parts by weight of polypropylene alcohol, modified glass-fiber, 1-2 weights Part antioxidant mixing high-speed stirred is measured until after uniformly, extruding pelletization, it is water-based to obtain modified glass-fiber polycarbafil type Polyurethane electrostatic resistance material.
2. according to a kind of preparation side of modified glass-fiber polycarbafil type aqueous polyurethane anti-static material of claim 1 Method, it is characterised in that step（1）Described is cooled to be cooled down with cold water.
3. according to a kind of preparation side of modified glass-fiber polycarbafil type aqueous polyurethane anti-static material of claim 1 Method, it is characterised in that step（2）The dihydromethyl propionic acid and the mixture of n-methyl-2-pyrrolidone are dihydroxymethyl Propionic acid and n-methyl-2-pyrrolidone（0.8-1）:1 mixing.
4. according to a kind of preparation side of modified glass-fiber polycarbafil type aqueous polyurethane anti-static material of claim 1 Method, it is characterised in that step（4）The antioxidant is antioxidant 1010, one kind in irgasfos 168.
CN201711427221.7A 2017-12-26 2017-12-26 A kind of preparation method of modified glass-fiber polycarbafil type aqueous polyurethane anti-static material Pending CN107964237A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110078883A (en) * 2019-05-22 2019-08-02 西华大学 A kind of water paint resin, preparation method and composition based on konjaku flour

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103483802A (en) * 2013-09-17 2014-01-01 安徽科聚新材料有限公司 Method for preparing high-performance glass fiber-reinforced thermoplastic polyurethane elastomer
CN104277198A (en) * 2014-10-25 2015-01-14 朱蕾 Preparation method of graphene-based conductive flame-retardant water-based polyurethane coating and adhesive
CN106117631A (en) * 2016-07-02 2016-11-16 郭迎庆 A kind of preparation method of Rhizoma amorphophalli fiber/graphene aerogel

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103483802A (en) * 2013-09-17 2014-01-01 安徽科聚新材料有限公司 Method for preparing high-performance glass fiber-reinforced thermoplastic polyurethane elastomer
CN104277198A (en) * 2014-10-25 2015-01-14 朱蕾 Preparation method of graphene-based conductive flame-retardant water-based polyurethane coating and adhesive
CN106117631A (en) * 2016-07-02 2016-11-16 郭迎庆 A kind of preparation method of Rhizoma amorphophalli fiber/graphene aerogel

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110078883A (en) * 2019-05-22 2019-08-02 西华大学 A kind of water paint resin, preparation method and composition based on konjaku flour

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Application publication date: 20180427