CN105482314A - Saponified anti-corrosion floor and preparation method thereof - Google Patents
Saponified anti-corrosion floor and preparation method thereof Download PDFInfo
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- CN105482314A CN105482314A CN201610009139.1A CN201610009139A CN105482314A CN 105482314 A CN105482314 A CN 105482314A CN 201610009139 A CN201610009139 A CN 201610009139A CN 105482314 A CN105482314 A CN 105482314A
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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
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
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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
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/06—Working-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
- C08J9/10—Working-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
- C08J9/102—Azo-compounds
- C08J9/103—Azodicarbonamide
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-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
- C08K9/08—Ingredients agglomerated by treatment with a binding agent
-
- 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
- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/04—N2 releasing, ex azodicarbonamide or nitroso compound
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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
- C08J2205/00—Foams characterised by their properties
- C08J2205/04—Foams characterised by their properties characterised by the foam pores
- C08J2205/052—Closed cells, i.e. more than 50% of the pores are closed
-
- 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
- C08J2327/00—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 a halogen; Derivatives of such polymers
- C08J2327/02—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 a halogen; Derivatives of such polymers not modified by chemical after-treatment
- C08J2327/04—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 a halogen; Derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
- C08J2327/06—Homopolymers or copolymers of vinyl chloride
-
- 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
- C08K3/32—Phosphorus-containing compounds
- C08K2003/321—Phosphates
- C08K2003/328—Phosphates of heavy metals
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/14—Applications used for foams
Abstract
The invention discloses a saponified anti-corrosion floor. The saponified anti-corrosion floor is prepared from, by weight, 3-4 parts of isobutyl oleate, 1-2 parts of triethanolamine oleic soap, 3-4 parts of sodium potassium silicate, 0.6-1 part of ammonium ferrous sulfate, 17-20 parts of zirconium oxychloride octahydrate, 10-15 parts of 40-47% hydrochloric acid, 90-100 parts of 80-85% of phosphoric acid, 3-4 parts of tetrakis hydroxymethyl phosphonium sulfate, 4-7 parts of 25-30% methylamine water solution, 5-7 parts of trifluoroethyl methacrylate, 0.2-0.4 part of 2-octyl-3(2H)-isothiazolone, 0.06-0.1 part of ammonium persulfate, 0.01-0.02 part of divinyl benzene, 1-2 parts of azodicarbonamide, 140-200 parts of polyvinyl chloride, 6-10 parts of trimellitate, 0.5-1 part of trichloroisocyanuric acid and 3-4 parts of lanolin magnesium soap. Triethanolamine oleic soap, lanolin magnesium soap and the like are adopted so that compatibility of the raw materials and polyvinyl chloride can be effectively improved, and stability of finished products is improved.
Description
Technical field
The present invention relates to technical field of floor, particularly relate to a kind of saponification anticorrosive floor board and preparation method thereof.
Background technology
PVC, as world's second largest general-purpose plastics, has good over-all properties, and cheap, raw material sources are extensive etc., and advantage has given play to vital role in all trades and professions.PVC foam material not only inherits above all advantages, and there is defect or the deficiency of some performances, as intensity, rigidity and thermomechanical property etc. do not reach the expectation of people, especially PVC foam material can discharge poisonous dense smoke when burning, and these all seriously hinder development and the application of PVC foam materials.Along with nanometer in recent years in the material shown by the great potential that goes out, make to form by modifications such as laminated inorganic matters the focus that over-all properties that nano composite material improves material becomes Recent study.Laminated inorganic matter makes the thermal stability of polymer composites after organically-modified, mechanical property significantly improves, particularly alpha zirconium phosphate is as a kind of novel nano particle with unique texture and character, there is purity high, loading capacity greatly easily realizes intercalation or lift-off structure, easily form nanostructure with polymkeric substance compound, this not only gives the excellent mechanical property of polymer materials, barrier property but also laminar nano particle is applied to the effect that can also play foaming nucleation agent in foam material to such an extent as to reaches the object optimizing foaming quality.On the other hand, PVC foam material, in inferior position that is fire-retardant and that press down in cigarette, also counteracts that it is further applied.And add anti-flaming smoke-inhibiting agent and just can well address this problem, the research of forefathers is for we have laid a good foundation, organic tin anti-flaming smoke-inhibiting agent and molybdenum class anti-flaming smoke-inhibiting agent have all shown outstanding flame-retardant smoke inhibition effect, the anti-flaming smoke-inhibiting agent of special organic is that same polymkeric substance has good consistency, this is that other fire retardants are unapproachable, therefore for other fire retardants, have suitable DEVELOPMENT PROSPECT, both conbined usage has no report in the flame-retardant smoke inhibition research of PVC at present.So this paper is intended to introduce organically-modified alpha zirconium phosphate Nano filling, improve foaming quality and mechanical property, the thermal stability etc. of PVC foam material.
Summary of the invention
The object of the invention is exactly the defect in order to make up prior art, provides a kind of saponification anticorrosive floor board and preparation method thereof.
The present invention is achieved by the following technical solutions:
A kind of saponification anticorrosive floor board, it is made up of the raw material of following weight parts:
Tebelon 3-4, trihydroxy ethylamine oleate soap 1-2, sodium-potassium silicate 3-4, ferrous ammonium sulphate 0.6-1, eight water zirconium oxychloride 17-20, the hydrochloric acid 10-15 of 40-47%, the phosphatase 79 0-100 of 80-85%, tetrakis hydroxymetyl phosphonium sulfuric 3-4, 25-30% aqueous methylamine solution 4-7, trifluoroethyl methacrylate 5-7, octylisothiazolinone 0.2-0.4, ammonium persulphate 0.06-0.1, Vinylstyrene 0.01-0.02, Cellmic C 121 1-2, polyvinyl chloride 140-200, trimellitate 6-10, trichloroisocyanuric acid 0.5-1, lanolin magnesium soap 3-4.
A preparation method for described saponification anticorrosive floor board, comprises the following steps:
(1) eight water zirconium oxychlorides are joined in 15-18 times of distilled water, stir, add the hydrochloric acid of above-mentioned 40-47%, the phosphoric acid of 80-85% successively, induction stirring 3-4 days under room temperature, filters, and is 5 with deionized water wash to PH, vacuum-drying at 60-65 DEG C, grinding, obtains alpha zirconium phosphate;
(2) above-mentioned trihydroxy ethylamine oleate soap is joined in 4-7 times of dehydrated alcohol, stir, add tebelon, insulated and stirred 3-5 minute at 60-70 DEG C, adds soda, and adjustment PH is 10-12, add octylisothiazolinone, 100-200 rev/min is stirred 10-20 minute, obtains anticorrosion soap lye;
(3) joined by above-mentioned lanolin magnesium soap in the ethanolic soln of 3-4 times of 20-30%, stir, add trifluoroethyl methacrylate, anticorrosion soap lye, raised temperature is 70-75 DEG C, adds Vinylstyrene, insulation reaction 3-4 hour, obtains anticorrosion saponification monomer;
(4) above-mentioned sodium-potassium silicate is joined in 3-5 times of deionized water, stir, add ferrous ammonium sulphate, insulated and stirred 10-15 minute at 70-75 DEG C, drip the sulfuric acid of 96-98%, adjustment PH is 1-2, continue insulated and stirred 20-30 minute, mix with above-mentioned alpha zirconium phosphate, suction filtration, dry 10-20 minute at 100-110 DEG C, obtains compound alpha zirconium phosphate;
(5) above-mentioned compound alpha zirconium phosphate is joined in 90-100 times of deionized water, stir, add aqueous methylamine solution, ultrasonic 30-35 minute, add tetrakis hydroxymetyl phosphonium sulfuric, dispersed with stirring 10-16 minute, add above-mentioned anticorrosion monomer, ultrasonic 3-5 minute, add ammonium persulphate, insulation reaction 6-10 hour at 75-80 DEG C, centrifugation, throw out is washed, dries, obtain organically-modified zirconium phosphate;
(6) above-mentioned organically-modified zirconium phosphate is mixed with polyvinyl chloride, send in homogenizer, 1000-1200r/min stirs 20-30 minute, and slow raised temperature is 120-130 DEG C, reduction rotating speed is 300-400r/min, be stirred to 46-50 DEG C, then raised temperature is 130-140 DEG C, adds each raw material of residue, heat-insulation preheating 50-60 minute, melt extruded by forcing machine, through traction cutting, plucking, to obtain final product.
Advantage of the present invention is:
(1) floor of the present invention has good heat-resistant stability:
Adopt tetrakis hydroxymetyl phosphonium sulfuric as properties-correcting agent, interlayer do not have can catalysis polyvinyl chloride decompose the factor, obtain the laminate structure of organically-modified zirconium phosphate, effectively can play the iris action of energy and material; On the other hand, organically-modified alpha zirconium phosphate add the foaming quality improving polyvinyl-chloride foam material, make uniform foam cell, obvious boundary has been there is between abscess, namely closed pore quantity is increasing, open-celled structure reduces, and this unicellular structure absorbs a large amount of heat in the process of heat transmission, stops the propagation of heat; In addition, adding organically-modified alpha zirconium phosphate can make polyvinyl chloride composite foam material be can be good at keeping the shape of abscess when impacting, abscess is made to keep original rigidity and toughness, therefore improve the thickness of polyvinyl chloride walls, enhance the outer position of its opposing and the ability destroyed is produced to it;
(2) floor of the present invention has good water resisting property:
Through organically-modified alpha zirconium phosphate, due to the H+ between organic cation substituted layer or organic anion the adsorption at alpha zirconium phosphate interlayer and modified hydrophobicity is improved comparatively significantly;
(3) floor of the present invention has good shock resistance:
The present invention adopts tetrakis hydroxymetyl phosphonium sulfuric to significantly improve the foaming quality of polyvinyl-chloride foam material as properties-correcting agent, and abscess is comparatively even, and cell wall presents spherical, and complete cell wall absorbs energy by there is deformation, then toughness increases;
(4) floor of the present invention has good flame retardant properties:
Alpha zirconium phosphate self is laminate structure, and through the lift-off structure that modified formation is certain, no matter be laminate structure or lift-off structure, the existence of these structures, matter and energy iris action can be played when polymer combustion, and can HCl be discharged during polyvinyl chloride burning, HCL gas self has obvious flame retardant resistance;
(5) first the present invention makes alpha zirconium phosphate gelatinizing with methylamine, then using trifluoroethyl methacrylate as anticorrosion monomer, embed in the course of the polymerization process and stable existence between modified alpha-zirconium phosphate layer, ensure heat-resisting, the water resistant of modification alpha zirconium phosphate, shock resistance, fire-retardant while improve antiseptic property;
The present invention adopts trihydroxy ethylamine oleate soap, lanolin magnesium soap etc. effectively can improve consistency between each raw material and polyvinyl chloride, improves the stability of finished product.
Embodiment
A kind of saponification anticorrosive floor board, it is made up of the raw material of following weight parts:
The phosphatase 79 0 of the hydrochloric acid 10,80% of tebelon 3, trihydroxy ethylamine oleate soap 1, sodium-potassium silicate 3, ferrous ammonium sulphate 0.6, eight water zirconium oxychloride 17,40%, tetrakis hydroxymetyl phosphonium sulfuric 3,25% aqueous methylamine solution 4, trifluoroethyl methacrylate 5, octylisothiazolinone 0.2, ammonium persulphate 0.06, Vinylstyrene 0.01, Cellmic C 121 1, polyvinyl chloride 140, trimellitate 6, trichloroisocyanuric acid 0.5, lanolin magnesium soap 3.
A preparation method for described saponification anticorrosive floor board, comprises the following steps:
(1) being joined in 15 times of distilled water by eight water zirconium oxychlorides, stir, add the hydrochloric acid of above-mentioned 40%, the phosphoric acid of 80% successively, induction stirring 3 days under room temperature, filter, is 5 with deionized water wash to PH, vacuum-drying at 60 DEG C, and grinding, obtains α zirconium phosphate;
(2) above-mentioned trihydroxy ethylamine oleate soap is joined in 4 times of dehydrated alcohols, stir, add tebelon, at 60 DEG C, insulated and stirred 3 minutes, adds soda, regulates PH to be 10, add octylisothiazolinone, 100 revs/min are stirred 10 minutes, obtain anticorrosion soap lye;
(3) joined in the ethanolic soln of 3 times 20% by above-mentioned lanolin magnesium soap, stir, add trifluoroethyl methacrylate, anticorrosion soap lye, raised temperature is 70 DEG C, adds Vinylstyrene, and insulation reaction 3 hours obtains anticorrosion saponification monomer;
(4) above-mentioned sodium-potassium silicate is joined in 3 times of deionized waters, stir, add ferrous ammonium sulphate, insulated and stirred 10 minutes at 70 DEG C, drip the sulfuric acid of 96%, PH is regulated to be 1, continue insulated and stirred 20 minutes, mix with above-mentioned α zirconium phosphate, suction filtration, at 100 DEG C, drying 10 minutes, obtains compound α zirconium phosphate;
(5) above-mentioned compound α zirconium phosphate is joined in 90 times of deionized waters, stir, add aqueous methylamine solution, ultrasonic 30 minutes, add tetrakis hydroxymetyl phosphonium sulfuric, dispersed with stirring 10 minutes, add above-mentioned anticorrosion monomer, ultrasonic 3 minutes, add ammonium persulphate, insulation reaction 6 hours at 75 DEG C, centrifugation, throw out is washed, dries, obtain organically-modified zirconium phosphate;
(6) above-mentioned organically-modified zirconium phosphate is mixed with polyvinyl chloride, send in homogenizer, 1000r/min stirs 20 minutes, and slow raised temperature is 120 DEG C, reduction rotating speed is 300r/min, be stirred to 46 DEG C, then raised temperature is 130 DEG C, adds each raw material of residue, heat-insulation preheating 50 minutes, melt extruded by forcing machine, through traction cutting, plucking, to obtain final product.
Performance test:
Shore D hardness: 68 degree;
Camber intensity: 24.9MPa;
Unnotched impact strength: 73kJ/m2;
Water-intake rate: 0.403%;
Shock resistance: flawless;
Oxygen index: 37.0%;
Miter angle burns: difficult combustion;
Nail-holding ability: 2.3kN;
Environmental-protecting performance (methyl alcohol burst size, condensed steam water 9-11L): 0.18mg/L.
Claims (2)
1. a saponification anticorrosive floor board, is characterized in that, it is made up of the raw material of following weight parts:
Tebelon 3-4, trihydroxy ethylamine oleate soap 1-2, sodium-potassium silicate 3-4, ferrous ammonium sulphate 0.6-1, eight water zirconium oxychloride 17-20, the hydrochloric acid 10-15 of 40-47%, the phosphatase 79 0-100 of 80-85%, tetrakis hydroxymetyl phosphonium sulfuric 3-4, 25-30% aqueous methylamine solution 4-7, trifluoroethyl methacrylate 5-7, octylisothiazolinone 0.2-0.4, ammonium persulphate 0.06-0.1, Vinylstyrene 0.01-0.02, Cellmic C 121 1-2, polyvinyl chloride 140-200, trimellitate 6-10, trichloroisocyanuric acid 0.5-1, lanolin magnesium soap 3-4.
2. a preparation method for saponification anticorrosive floor board as claimed in claim 1, is characterized in that, comprise the following steps:
(1) eight water zirconium oxychlorides are joined in 15-18 times of distilled water, stir, add the hydrochloric acid of above-mentioned 40-47%, the phosphoric acid of 80-85% successively, induction stirring 3-4 days under room temperature, filters, and is 5 with deionized water wash to PH, vacuum-drying at 60-65 DEG C, grinding, obtains alpha zirconium phosphate;
(2) above-mentioned trihydroxy ethylamine oleate soap is joined in 4-7 times of dehydrated alcohol, stir, add tebelon, insulated and stirred 3-5 minute at 60-70 DEG C, adds soda, and adjustment PH is 10-12, add octylisothiazolinone, 100-200 rev/min is stirred 10-20 minute, obtains anticorrosion soap lye;
(3) joined by above-mentioned lanolin magnesium soap in the ethanolic soln of 3-4 times of 20-30%, stir, add trifluoroethyl methacrylate, anticorrosion soap lye, raised temperature is 70-75 DEG C, adds Vinylstyrene, insulation reaction 3-4 hour, obtains anticorrosion saponification monomer;
(4) above-mentioned sodium-potassium silicate is joined in 3-5 times of deionized water, stir, add ferrous ammonium sulphate, insulated and stirred 10-15 minute at 70-75 DEG C, drip the sulfuric acid of 96-98%, adjustment PH is 1-2, continue insulated and stirred 20-30 minute, mix with above-mentioned alpha zirconium phosphate, suction filtration, dry 10-20 minute at 100-110 DEG C, obtains compound alpha zirconium phosphate;
(5) above-mentioned compound alpha zirconium phosphate is joined in 90-100 times of deionized water, stir, add aqueous methylamine solution, ultrasonic 30-35 minute, add tetrakis hydroxymetyl phosphonium sulfuric, dispersed with stirring 10-16 minute, add above-mentioned anticorrosion monomer, ultrasonic 3-5 minute, add ammonium persulphate, insulation reaction 6-10 hour at 75-80 DEG C, centrifugation, throw out is washed, dries, obtain organically-modified zirconium phosphate;
(6) above-mentioned organically-modified zirconium phosphate is mixed with polyvinyl chloride, send in homogenizer, 1000-1200r/min stirs 20-30 minute, and slow raised temperature is 120-130 DEG C, reduction rotating speed is 300-400r/min, be stirred to 46-50 DEG C, then raised temperature is 130-140 DEG C, adds each raw material of residue, heat-insulation preheating 50-60 minute, melt extruded by forcing machine, through traction cutting, plucking, to obtain final product.
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| CN201610009139.1A CN105482314A (en) | 2016-01-04 | 2016-01-04 | Saponified anti-corrosion floor and preparation method thereof |
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| CN201610009139.1A CN105482314A (en) | 2016-01-04 | 2016-01-04 | Saponified anti-corrosion floor and preparation method thereof |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102558758A (en) * | 2012-01-04 | 2012-07-11 | 上海柯瑞冶金炉料有限公司 | Phenolic resin foam material and preparing method thereof |
| CN104631775A (en) * | 2013-11-12 | 2015-05-20 | 江阴华诚汽车内饰件有限公司 | Coiled material floor having bacteria resistant function |
-
2016
- 2016-01-04 CN CN201610009139.1A patent/CN105482314A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102558758A (en) * | 2012-01-04 | 2012-07-11 | 上海柯瑞冶金炉料有限公司 | Phenolic resin foam material and preparing method thereof |
| CN104631775A (en) * | 2013-11-12 | 2015-05-20 | 江阴华诚汽车内饰件有限公司 | Coiled material floor having bacteria resistant function |
Non-Patent Citations (2)
| Title |
|---|
| 施增楷: "施增楷", 《广东化工》 * |
| 李智: "聚氯乙烯/α-磷酸锆纳米复合发泡材料的制备及阻燃抑烟性能研究", 《中国优秀硕士论文全文数据库工程科技Ⅰ辑》 * |
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Application publication date: 20160413 |
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