CN109251432A - A kind of quaternary phosphonium insulation board material and preparation method thereof - Google Patents

A kind of quaternary phosphonium insulation board material and preparation method thereof Download PDF

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Publication number
CN109251432A
CN109251432A CN201810865082.4A CN201810865082A CN109251432A CN 109251432 A CN109251432 A CN 109251432A CN 201810865082 A CN201810865082 A CN 201810865082A CN 109251432 A CN109251432 A CN 109251432A
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insulation board
board material
hours
quaternary phosphonium
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CN201810865082.4A
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Inventor
胡俊凯
章荣春
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Anhui Jixi Huayu Fireproof Filter Material Co Ltd
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Anhui Jixi Huayu Fireproof Filter Material Co Ltd
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Priority to CN201810865082.4A priority Critical patent/CN109251432A/en
Publication of CN109251432A publication Critical patent/CN109251432A/en
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F112/00Homopolymers 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 aromatic carbocyclic ring
    • C08F112/02Monomers containing only one unsaturated aliphatic radical
    • C08F112/04Monomers containing only one unsaturated aliphatic radical containing one ring
    • C08F112/06Hydrocarbons
    • C08F112/08Styrene
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F251/00Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof
    • C08F251/02Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof on to cellulose or derivatives thereof
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/0061Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof characterized by the use of several polymeric components
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/009Use of pretreated compounding ingredients
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/04Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
    • C08J9/06Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent
    • C08J9/10Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent developing nitrogen, the blowing agent being a compound containing a nitrogen-to-nitrogen bond
    • C08J9/102Azo-compounds
    • C08J9/103Azodicarbonamide
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2203/00Foams characterized by the expanding agent
    • C08J2203/04N2 releasing, ex azodicarbonamide or nitroso compound
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2325/00Characterised 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 aromatic carbocyclic ring; Derivatives of such polymers
    • C08J2325/02Homopolymers or copolymers of hydrocarbons
    • C08J2325/04Homopolymers or copolymers of styrene
    • C08J2325/06Polystyrene
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2451/00Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers
    • C08J2451/02Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers grafted on to polysaccharides

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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)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)

Abstract

The invention discloses a kind of quaternary phosphonium insulation board materials, it is composed of the following raw materials by weight: hollow glass micropearl 10-13, methylcellulose 10-15, 2-mercaptobenzothiazole 7-8, allyl triphenylphosphinebromide 10-14, initiator 0.01-0.012, styrene 180-220, ammonium persulfate 5-7, butyl titanate 30-40, sp-80 0.7-1, ac foaming agent 7-12, present invention introduces titanium colloidal sol not only can effectively improve the mechanical property of finished product plate, and have the effect of cooperateing with well with quaternary phosphine salt blend antibacterial, to improve the integrated quality of finished-product material.

Description

A kind of quaternary phosphonium insulation board material and preparation method thereof
Technical field
The invention belongs to Material Fields, and in particular to a kind of quaternary phosphonium insulation board material and preparation method thereof.
Background technique
The purposes of foamed polystyrene resin is very extensive, since it has high intensity, light weight, splendid heat preservation insulation Performance and high-selenium corn energy ability, may be used as various instrument, valuables, precision instrument, vegetable and fruit and aquatic products etc. Packaging material;And because it is low with pyroconductivity, water imbibition is small, electrical insulating property is good, sound insulation, moisture-proof and moulding process are simple Equal good characteristics, and the roadbed for being widely used in road and bridge is laid with and catches and refrigerate industry with building construction and fishery Thermal insulation material etc..Wherein, as a kind of excellent construction material, foamed polystyrene resin is mainly used for the room of building Face and wall have very good energy-saving effect as external heat insulating composite wall;And as heat insulation house surface be suitable for house, Factory, flat and pitch roofing, the effects of sound insulation, water blocking steam, sealing and insulation can be played.
However, the mechanical property and biocidal property of traditional polystyrene are poor, therefore, seem if improving its comprehensive performance It is very necessary.
Summary of the invention
In view of the defects and deficiencies of the prior art, the present invention intends to provide a kind of quaternary phosphonium insulation board material and its Preparation method.
To achieve the above object, the invention adopts the following technical scheme:
A kind of quaternary phosphonium insulation board material, it is composed of the following raw materials by weight:
Hollow glass micropearl 10-13, methylcellulose 10-15,2-mercaptobenzothiazole 7-8, allyl triphenyl phosphonium bromide Phosphine 10-14, initiator 0.01-0.012, styrene 180-220, ammonium persulfate 5-7, butyl titanate 30-40, sp-80 0.7- 1, ac foaming agent 7-12.
The degree of substitution of the methylcellulose is 2.5-2.7.
The initiator is azodiisobutyronitrile.
A kind of preparation method of quaternary phosphonium insulation board material, comprising the following steps:
(1) methylcellulose is taken, is added in the chloroform of 10-17 times of its weight, stirring and dissolving, 2- sulfydryl benzo thiophene is added Azoles, increasing temperature is 50-55 DEG C, insulated and stirred 1-2 hours, obtains fiber dispersion;
(2) allyl triphenylphosphinebromide is taken, is added in above-mentioned fiber dispersion, stirs evenly, is passed through nitrogen deoxygenation, Initiator is added, ultraviolet irradiation 1-2 hours, revolving removed chloroform, air drying, get quaternary alkylphosphonium salt modified fibre;
(3) above-mentioned quaternary alkylphosphonium salt modified fibre is taken, is mixed with butyl titanate, going for 10-17 times of mixture weight is added to In ionized water, hollow glass micropearl, sp-80 is added, is stirred to react 4-6 hours, get quaternary alkylphosphonium salt sol solution;
(4) ammonium persulfate is taken, is added in the deionized water of 20-30 times of its weight, stirs evenly;
(5) styrene is taken, is added in above-mentioned quaternary alkylphosphonium salt sol solution, is stirred evenly, be sent in reaction kettle, be passed through nitrogen Gas, adjusting temperature of reaction kettle is 60-75 DEG C, above-mentioned ammonium persulfate aqueous solution is added, insulated and stirred 3-5 hours, ac was added in discharging Foaming agent, 2-3 hours dry under 110-120 DEG C of steam, discharging is cooling to get the quaternary phosphonium insulation board material.
Advantages of the present invention:
The present invention uses 2-mercaptobenzothiazole to handle methylcellulose first, then total with allyl triphenylphosphinebromide It is mixed, it is reacted under ultraviolet photoinitiation, obtains quaternary alkylphosphonium salt modified fibre, improve the methylcellulose of high substituted degree in water Dispersion performance, while imparting the good biocidal property of fiber, hydrolysis be blended with butyl titanate later, introduced in hydrolysis empty Heart glass microballoon realizes the cladding to hollow glass micropearl, later using styrene as monomer, with the season by the deposition of colloidal sol Phosphonium salt sol solution is reaction dissolvent, polymerize under initiator effect, obtains finished product, present invention introduces titanium colloidal sol not only can be with The effective mechanical property for improving finished product plate, and with quaternary phosphine salt blend have the effect of cooperateing with well it is antibacterial, to mention The high integrated quality of finished-product material.
Specific embodiment
Embodiment 1
A kind of quaternary phosphonium insulation board material, it is composed of the following raw materials by weight:
Hollow glass micropearl 13,2-mercaptobenzothiazole 8, allyl triphenylphosphinebromide 14, causes methylcellulose 15 Agent 0.012, styrene 220, ammonium persulfate 7, butyl titanate 40, sp-80 1, ac foaming agent 12.
The degree of substitution of the methylcellulose is 2.7.
The initiator is azodiisobutyronitrile.
A kind of preparation method of quaternary phosphonium insulation board material, comprising the following steps:
(1) methylcellulose is taken, is added in the chloroform of 17 times of its weight, stirring and dissolving, 2-mercaptobenzothiazole is added, Increasing temperature is 55 DEG C, insulated and stirred 2 hours, obtains fiber dispersion;
(2) allyl triphenylphosphinebromide is taken, is added in above-mentioned fiber dispersion, stirs evenly, is passed through nitrogen deoxygenation, Initiator is added, ultraviolet irradiation 2 hours, revolving removed chloroform, air drying, get quaternary alkylphosphonium salt modified fibre;
(3) above-mentioned quaternary alkylphosphonium salt modified fibre is taken, is mixed with butyl titanate, 17 times of mixture weight of deionization is added to In water, hollow glass micropearl, sp-80 is added, is stirred to react 6 hours, get quaternary alkylphosphonium salt sol solution;
(4) ammonium persulfate is taken, is added in the deionized water of 30 times of its weight, stirs evenly;
(5) styrene is taken, is added in above-mentioned quaternary alkylphosphonium salt sol solution, is stirred evenly, be sent in reaction kettle, be passed through nitrogen Gas, adjusting temperature of reaction kettle is 75 DEG C, above-mentioned ammonium persulfate aqueous solution is added, insulated and stirred 5 hours, ac foaming was added in discharging Agent, 3 hours dry under 120 DEG C of steam, discharging is cooling to get the quaternary phosphonium insulation board material.
Embodiment 2
A kind of quaternary phosphonium insulation board material, it is composed of the following raw materials by weight:
Hollow glass micropearl 10,2-mercaptobenzothiazole 7, allyl triphenylphosphinebromide 10, causes methylcellulose 10 Agent 0.01, styrene 180, ammonium persulfate 5, butyl titanate 30, sp-80 0.7, ac foaming agent 7.
The degree of substitution of the methylcellulose is 2.5.
The initiator is azodiisobutyronitrile.
A kind of preparation method of quaternary phosphonium insulation board material, comprising the following steps:
(1) methylcellulose is taken, is added in the chloroform of 10 times of its weight, stirring and dissolving, 2-mercaptobenzothiazole is added, Increasing temperature is 50 DEG C, insulated and stirred 1 hour, obtains fiber dispersion;
(2) allyl triphenylphosphinebromide is taken, is added in above-mentioned fiber dispersion, stirs evenly, is passed through nitrogen deoxygenation, Initiator is added, ultraviolet irradiation 1 hour, revolving removed chloroform, air drying, get quaternary alkylphosphonium salt modified fibre;
(3) above-mentioned quaternary alkylphosphonium salt modified fibre is taken, is mixed with butyl titanate, 10 times of mixture weight of deionization is added to In water, hollow glass micropearl, sp-80 is added, is stirred to react 4 hours, get quaternary alkylphosphonium salt sol solution;
(4) ammonium persulfate is taken, is added in the deionized water of 20 times of its weight, stirs evenly;
(5) styrene is taken, is added in above-mentioned quaternary alkylphosphonium salt sol solution, is stirred evenly, be sent in reaction kettle, be passed through nitrogen Gas, adjusting temperature of reaction kettle is 60 DEG C, above-mentioned ammonium persulfate aqueous solution is added, insulated and stirred 3 hours, ac foaming was added in discharging Agent, 2 hours dry under 110 DEG C of steam, discharging is cooling to get the quaternary phosphonium insulation board material.
Performance test:
The quaternary phosphonium insulation board material of the embodiment of the present invention 1:
Tensile strength (MPa): 15.1;
Elongation at break (%): 76;
Simply supported beam notch impact strength (J/m2):22.3;
The quaternary phosphonium insulation board material of the embodiment of the present invention 2:
Tensile strength (MPa): 16.2;
Elongation at break (%): 85;
Simply supported beam notch impact strength (J/m2):23.5;
Tensile strength≤10Mpa of commercial polysterol material, elongation at break≤50%, simply supported beam notch impact strength ≤15J/m2
Bacteriostasis property test:
Escherichia coli+the staphylococcus aureus for using this field common for observe object, testing time point be 20 hours, 30 hours;
Quaternary phosphonium insulation board material obtained in the embodiment of the present invention 1 measured at 24 hours bacteriostasis rate be 98.7%, It is 99.1% that bacteriostasis rate was measured at 48 hours;
Quaternary phosphonium insulation board material obtained in the embodiment of the present invention 2 measured at 24 hours bacteriostasis rate be 98.3%, It is 99.0% that bacteriostasis rate was measured at 48 hours;
Commercial polysterol material measured bacteriostasis rate at 24 hours and is 47.1%, measured bacteriostasis rate at 48 hours and be 47.2%.

Claims (4)

1. a kind of quaternary phosphonium insulation board material, which is characterized in that it is composed of the following raw materials by weight:
Hollow glass micropearl 10-13, methylcellulose 10-15,2-mercaptobenzothiazole 7-8, allyl triphenylphosphinebromide 10- 14, initiator 0.01-0.012, styrene 180-220, ammonium persulfate 5-7, butyl titanate 30-40, sp-80 0.7-1, ac Foaming agent 7-12.
2. a kind of quaternary phosphonium insulation board material according to claim 1, which is characterized in that the methylcellulose takes Dai Du is 2.5-2.7.
3. a kind of quaternary phosphonium insulation board material according to claim 1, which is characterized in that the initiator is azo two Isobutyronitrile.
4. a kind of preparation method of quaternary phosphonium insulation board material as described in claim 1, which comprises the following steps:
(1) methylcellulose is taken, is added in the chloroform of 10-17 times of its weight, stirring and dissolving, 2-mercaptobenzothiazole is added, Increasing temperature is 50-55 DEG C, insulated and stirred 1-2 hours, obtains fiber dispersion;
(2) allyl triphenylphosphinebromide is taken, is added in above-mentioned fiber dispersion, stirs evenly, is passed through nitrogen deoxygenation, is added Initiator, ultraviolet irradiation 1-2 hours, revolving removed chloroform, air drying, get quaternary alkylphosphonium salt modified fibre;
(3) above-mentioned quaternary alkylphosphonium salt modified fibre is taken, is mixed with butyl titanate, the deionization of 10-17 times of mixture weight is added to In water, hollow glass micropearl, sp-80 is added, is stirred to react 4-6 hours, get quaternary alkylphosphonium salt sol solution;
(4) ammonium persulfate is taken, is added in the deionized water of 20-30 times of its weight, stirs evenly;
(5) styrene is taken, is added in above-mentioned quaternary alkylphosphonium salt sol solution, is stirred evenly, be sent in reaction kettle, be passed through nitrogen, Adjusting temperature of reaction kettle is 60-75 DEG C, above-mentioned ammonium persulfate aqueous solution is added, insulated and stirred 3-5 hours, ac hair was added in discharging Infusion, 2-3 hours dry under 110-120 DEG C of steam, discharging is cooling to get the quaternary phosphonium insulation board material.
CN201810865082.4A 2018-08-01 2018-08-01 A kind of quaternary phosphonium insulation board material and preparation method thereof Withdrawn CN109251432A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111440278A (en) * 2020-05-12 2020-07-24 北京福田戴姆勒汽车有限公司 Activated carbon material and preparation method and application thereof
CN111635607A (en) * 2020-06-28 2020-09-08 宣城市创道智能技术开发有限责任公司 Polyester fireproof board material and preparation method thereof

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111440278A (en) * 2020-05-12 2020-07-24 北京福田戴姆勒汽车有限公司 Activated carbon material and preparation method and application thereof
CN111440278B (en) * 2020-05-12 2022-09-27 北京福田戴姆勒汽车有限公司 Activated carbon material and preparation method and application thereof
CN111635607A (en) * 2020-06-28 2020-09-08 宣城市创道智能技术开发有限责任公司 Polyester fireproof board material and preparation method thereof

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