CN107129678A - A kind of water-resistant type gypsum polyamide 6 composite material of polyvinyl alcohol modification and preparation method thereof - Google Patents

A kind of water-resistant type gypsum polyamide 6 composite material of polyvinyl alcohol modification and preparation method thereof Download PDF

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Publication number
CN107129678A
CN107129678A CN201710328376.9A CN201710328376A CN107129678A CN 107129678 A CN107129678 A CN 107129678A CN 201710328376 A CN201710328376 A CN 201710328376A CN 107129678 A CN107129678 A CN 107129678A
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CN
China
Prior art keywords
water
resistant type
polyamide
composite
solution
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Pending
Application number
CN201710328376.9A
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Chinese (zh)
Inventor
陈阳振
李久军
李春来
王洪山
黄利侠
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Fuyang Sanhuan Cement Product Co Ltd
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Fuyang Sanhuan Cement Product Co Ltd
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Priority to CN201710328376.9A priority Critical patent/CN107129678A/en
Publication of CN107129678A publication Critical patent/CN107129678A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L77/00Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
    • C08L77/02Polyamides derived from omega-amino carboxylic acids or from lactams thereof
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/30Sulfur-, selenium- or tellurium-containing compounds
    • C08K2003/3045Sulfates
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/011Nanostructured additives
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/08Stabilised against heat, light or radiation or oxydation

Abstract

The invention discloses a kind of water-resistant type gypsum polyamide 6 composite material of polyvinyl alcohol modification, and its preparation technology, it is characterised in that poly-vinyl alcohol solution, barium chloride solution, methyl silanol sodium solution are mixed to obtain into composite glue solution;It is added into land plaster, stir to obtain water-resistant type gypsum;Add ethanol dilution into coupling agent, water-resistant type gypsum is put into high-speed mixer, the coupling agent after dilution is sprayed in gypsum using atomization method, coupling modifier water-resistant type gypsum is dried in vacuo to obtain;Add distilled water into polyvinylpyrrolidone, obtain surfactant solution;Wall carbon nano tube is added, after stirring, ultrasonic, centrifugation is placed in ultrasonic cell disintegration instrument, obtains carbon nano tube dispersion liquid;Put into after polyamide is dried from fast mixer, white oil is sprayed onto polyamide 6 surface, mixed at high speed under spray condition;Put into after above resulting material, mixed at high speed, be added in double screw extruder and granulate, dry, obtain composite.

Description

A kind of water-resistant type gypsum-polyamide 6 composite material of polyvinyl alcohol modification and its preparation Method
Technical field
The present invention relates to field of compound material, and in particular to a kind of water-resistant type gypsum-polyamide 6 of polyvinyl alcohol modification is multiple Condensation material, and its preparation technology.
Background technology
Novel super-high strength cement-based material composite is super with its excellent resistance to compression, bending resistance, tension, wear-resisting, corrosion-resistant etc. Strong durability performance, is the key technology for realizing Sustainable Construction Industry.For the performance of high-strength and ultra-high-strength cement-based composites Go out that fragility is big, shrink big, a series of outstanding problems such as early-age crack is serious.
Zhang Yu is in its master thesis《Ultrastrength cement based composites and its product research》In, utilize natural river The mineral admixtures such as sand, flyash, miberal powder, silicon ash, and different addition quantity steel fibre prepare serial Ultrastrength cement base composite wood Material, can be obviously improved its workability, its workability can also be improved by mixing high efficiency water reducing agent when single fly ash or miberal powder.But deposit It is not enough in intensity, mechanical property.
The content of the invention
The present invention solves the technical problem of providing, a kind of water-resistant type gypsum-polyamide 6 of polyvinyl alcohol modification is multiple Condensation material and its preparation technology, the composite prepared according to the technique have good mechanical property, heat endurance and water-fast Property.
The technical problems to be solved by the invention are realized using following technical scheme:
The preparation method of water-resistant type gypsum-polyamide 6 composite material of a kind of polyvinyl alcohol modification, it is characterised in that by following Step is carried out:
A. while stirring by 1-2 weight account polyethylene alcohol powder 1:5-10 is added in distilled water, it is fully infiltrated, is swelled, dividing Dissipate, be then placed in 85-95 DEG C of hot bath and heat, be stirred continuously with glass bar to being completely dissolved, obtain poly-vinyl alcohol solution;
B. while stirring by 3-4 parts by weight barium chloride 1:5-10 is poured into distilled water, is sufficiently stirred for dissolving, is obtained barium chloride solution; By 2-3 parts by weight methyl silicon sodium alcoholate 1:5-10 is dissolved in distilled water, obtains methyl silanol sodium solution;Gained polyvinyl alcohol in a is molten Liquid is mixed with barium chloride solution, methyl silanol sodium solution, and stir to obtain composite glue solution;It is added into 10-20 parts by weight gypsum In powder, stir, obtain water-resistant type gypsum;
C. into 1-2 parts by weight coupling agents KH560 1:40-50 adds ethanol, and agitation and dilution is uniform, by gained water-resistant type stone in b In cream input high-speed mixer, 80-90 DEG C is warming up to, the coupling agent after dilution is sprayed in gypsum using atomization method, is mixed Close after 20-40min, be placed in 60-70 DEG C of vacuum drying oven and dry 2-3h, obtain coupling modifier water-resistant type gypsum;
D. ultrasonic disperse technique:Into 4-6 weight account polyethylene pyrrolidones 1:5-10 adds distilled water, is stirred with magnetic stirring apparatus Mix to being completely dissolved, obtain surfactant solution;1-2 parts by weight multi-walled carbon nanotubes are added, continue to use magnetic stirrer After 10-20min, ultrasound 30-40min in ultrasonic cell disintegration instrument is placed in, 20-30min is centrifuged, multi-walled carbon nanotube is obtained and disperses Liquid;
E. 60-80 weight parts of polyamide 6 is dried into 6-8h at 90-100 DEG C, put into from fast mixer, by 0.5-1 weight Part white oil is sprayed onto polyamide 6 surface, mixed at high speed 10-20min under spray condition;Resulting material in c, d is put into, it is mixed at a high speed Close after 20-30min, be added in double screw extruder and granulate, obtain composite.
Wherein, centrifugal speed described in step d is 2000-3000rpm.The extrusion temperature of double screw extruder described in step e Spend for 200-230 DEG C, screw speed is 180-200r/min.
The reaction mechanism of the present invention is as follows:
Multi-walled carbon nanotube (MWCNT) has high length-diameter ratio, is added in gypsum with fiber reinforced and nano-filled Characteristic, gained composite has high intensity, high volume stability and high permeability resistance;With the poly- second of nonionic surface active agent Alkene pyrrolidone (PVP) is modifying agent, good to MWCNT dispersion effect with reference to ultrasonic disperse technique, significantly improves composite wood The mechanical property of material.
Barium chloride and polyvinyl alcohol are filled in land plaster can reduce its porosity, and admixture methyl silicon sodium alcoholate can be in stone Non-crystalline material is generated between cream powder crystal body, plays a part of protecting crystal contact point;Compounding use can become crystal structure It is closely knit, significantly reduce the water absorption rate of plastering.Surface modification is carried out to land plaster using coupling agent KH560, by it with gathering The melt blending of acid amides 6, is made composite;The addition of land plaster serves the effect of heterogeneous nucleation, improves the knot of polyamide 6 Brilliant temperature and crystallinity;Modified gypsum can be dispersed in polyamide 6, and both interfacial adhesion effects are preferable;Carry The high tensile strength of composite, bending strength and impact strength, are more beneficial for improving the heat endurance of polyamide 6.
Embodiment
In order that the technical means, the inventive features, the objects and the advantages of the present invention are easy to understand, tie below Specific embodiment is closed, the present invention is expanded on further.
Embodiment
The preparation method of water-resistant type gypsum-polyamide 6 composite material of a kind of polyvinyl alcohol modification, it is characterised in that press Following steps are carried out:
A. while stirring by 1kg pva powders 1:5 add in distilled water, it is fully infiltrated, be swelled, disperse, Ran Houfang Enter in 85-95 DEG C of hot bath and heat, be stirred continuously with glass bar to being completely dissolved, obtain poly-vinyl alcohol solution;
B. while stirring by 3kg barium chlorides 1:5 pour into distilled water, are sufficiently stirred for dissolving, obtain barium chloride solution;By 2kg methyl Sodium silanolate 1:5 are dissolved in distilled water, obtain methyl silanol sodium solution;By gained poly-vinyl alcohol solution in a and barium chloride solution, methyl Silanol sodium solution is mixed, and stir to obtain composite glue solution;It is added into 20kg land plasters, stirs, obtains water-resistant type gypsum;
C. into 1kg coupling agents KH560 1:45 add ethanol, and agitation and dilution is uniform, gained water-resistant type gypsum in b are put into high In fast mixer, 80-90 DEG C is warming up to, the coupling agent after dilution is sprayed in gypsum using atomization method, 30min is mixed Afterwards, it is placed in 60-70 DEG C of vacuum drying oven and dries 3h, obtains coupling modifier water-resistant type gypsum;
D. ultrasonic disperse technique:Into 4kg polyvinylpyrrolidones 1:5 plus distilled water, with magnetic stirrer to completely molten Solution, obtains surfactant solution;1kg multi-walled carbon nanotubes are added, continue, with after magnetic stirrer 15min, to be placed in ultrasound Ultrasound 35min in cell crushing instrument, centrifuges 25min, obtains multi-walled carbon nanotube dispersion liquid;
E. 80kg polyamide 6s are dried into 6h at 90-100 DEG C, put into from fast mixer, by 0.5kg white oils in spray condition Under be sprayed onto polyamide 6 surface, mixed at high speed 15min;Put into after resulting material in c, d, mixed at high speed 25min, be added to double Granulated in screw extruder, obtain composite.
Wherein, centrifugal speed described in step d is 2500rpm.Double screw extruder extrusion temperature is described in step e 220 DEG C, screw speed is 200r/min.

Claims (4)

1. a kind of water-resistant type gypsum-polyamide 6 composite material of polyvinyl alcohol modification, it is characterised in that:
Poly-vinyl alcohol solution, barium chloride solution, methyl silanol sodium solution are mixed into obtain composite glue solution;It is added into land plaster, Stir to obtain water-resistant type gypsum;Add ethanol dilution into coupling agent, water-resistant type gypsum is put into high-speed mixer, using mist Coupling agent after dilution is sprayed in gypsum by change method, is dried in vacuo to obtain coupling modifier water-resistant type gypsum;To polyvinyl pyrrole Add distilled water in alkanone, obtain surfactant solution;Wall carbon nano tube is added, after stirring, is placed in ultrasonic cell disintegration instrument and surpasses Sound, centrifugation, obtains carbon nano tube dispersion liquid;Put into after polyamide is dried from fast mixer, white oil is sprayed under spray condition It is spread across polyamide 6 surface, mixed at high speed;Put into after above resulting material, mixed at high speed, be added in double screw extruder and make Grain, dries, obtains composite.
2. a kind of preparation side of water-resistant type gypsum-polyamide 6 composite material of polyvinyl alcohol modification according to claim 1 Method, it is characterised in that carry out according to the following steps:
While stirring by 1-2 weight account polyethylene alcohol powder 1:5-10 is added in distilled water, it is fully infiltrated, be swelled, disperseed, It is then placed in 85-95 DEG C of hot bath and heats, is stirred continuously with glass bar to being completely dissolved, obtains poly-vinyl alcohol solution;
B. while stirring by 3-4 parts by weight barium chloride 1:5-10 is poured into distilled water, is sufficiently stirred for dissolving, is obtained barium chloride solution; By 2-3 parts by weight methyl silicon sodium alcoholate 1:5-10 is dissolved in distilled water, obtains methyl silanol sodium solution;Gained polyvinyl alcohol in a is molten Liquid is mixed with barium chloride solution, methyl silanol sodium solution, and stir to obtain composite glue solution;It is added into 10-20 parts by weight gypsum In powder, stir, obtain water-resistant type gypsum;
C. into 1-2 parts by weight coupling agents KH560 1:40-50 adds ethanol, and agitation and dilution is uniform, by gained water-resistant type stone in b In cream input high-speed mixer, 80-90 DEG C is warming up to, the coupling agent after dilution is sprayed in gypsum using atomization method, is mixed Close after 20-40min, be placed in 60-70 DEG C of vacuum drying oven and dry 2-3h, obtain coupling modifier water-resistant type gypsum;
D. ultrasonic disperse technique:Into 4-6 weight account polyethylene pyrrolidones 1:5-10 adds distilled water, is stirred with magnetic stirring apparatus Mix to being completely dissolved, obtain surfactant solution;1-2 parts by weight multi-walled carbon nanotubes are added, continue to use magnetic stirrer After 10-20min, ultrasound 30-40min in ultrasonic cell disintegration instrument is placed in, 20-30min is centrifuged, multi-walled carbon nanotube is obtained and disperses Liquid;
E. 60-80 weight parts of polyamide 6 is dried into 6-8h at 90-100 DEG C, put into from fast mixer, by 0.5-1 weight Part white oil is sprayed onto polyamide 6 surface, mixed at high speed 10-20min under spray condition;Resulting material in c, d is put into, it is mixed at a high speed Close after 20-30min, be added in double screw extruder and granulate, obtain composite.
3. a kind of preparation side of water-resistant type gypsum-polyamide 6 composite material of polyvinyl alcohol modification according to claim 2 Method, it is characterised in that centrifugal speed described in step d is 2000-3000rpm.
4. a kind of preparation side of water-resistant type gypsum-polyamide 6 composite material of polyvinyl alcohol modification according to claim 2 Method, it is characterised in that double screw extruder extrusion temperature described in step e is 200-230 DEG C, and screw speed is 180-200r/ min。
CN201710328376.9A 2017-05-11 2017-05-11 A kind of water-resistant type gypsum polyamide 6 composite material of polyvinyl alcohol modification and preparation method thereof Pending CN107129678A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108004782A (en) * 2017-12-27 2018-05-08 成都新柯力化工科技有限公司 A kind of thermoplasticity inorfil and preparation method for plastics

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
M.J.埃克诺米德斯 等: "《油井建井工程》", 30 April 2001, 石油工业出版社 *
刘帅: "碳纳米管的分散性及其水泥基复合材料耐久性能", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 *
杜亚平 等: "不同偶联剂对PA6/硬石膏粉复合材料性能的影响", 《塑料科技》 *
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108004782A (en) * 2017-12-27 2018-05-08 成都新柯力化工科技有限公司 A kind of thermoplasticity inorfil and preparation method for plastics

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