KR20150031965A - Method For Measuring Plastisol Migration Rate Of Paste Vinyl Chloride Resins by Elusion Agent - Google Patents
Method For Measuring Plastisol Migration Rate Of Paste Vinyl Chloride Resins by Elusion Agent Download PDFInfo
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- KR20150031965A KR20150031965A KR20130111877A KR20130111877A KR20150031965A KR 20150031965 A KR20150031965 A KR 20150031965A KR 20130111877 A KR20130111877 A KR 20130111877A KR 20130111877 A KR20130111877 A KR 20130111877A KR 20150031965 A KR20150031965 A KR 20150031965A
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- South Korea
- Prior art keywords
- plasticizer
- vinyl chloride
- plastisol
- measuring
- resin
- Prior art date
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- 239000011347 resin Substances 0.000 title claims abstract description 64
- 229920005989 resin Polymers 0.000 title claims abstract description 64
- BZHJMEDXRYGGRV-UHFFFAOYSA-N Vinyl chloride Chemical compound ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 title claims abstract description 57
- 229920001944 Plastisol Polymers 0.000 title claims abstract description 38
- 239000004999 plastisol Substances 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 31
- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 11
- 238000013508 migration Methods 0.000 title claims description 48
- 230000005012 migration Effects 0.000 title claims description 48
- 239000004014 plasticizer Substances 0.000 claims abstract description 80
- 238000004519 manufacturing process Methods 0.000 claims abstract description 16
- 239000003480 eluent Substances 0.000 claims abstract description 9
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 23
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- 239000003995 emulsifying agent Substances 0.000 claims description 15
- 239000003638 chemical reducing agent Substances 0.000 claims description 13
- 238000000576 coating method Methods 0.000 claims description 13
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 claims description 12
- 238000010828 elution Methods 0.000 claims description 12
- 239000011248 coating agent Substances 0.000 claims description 11
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 10
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 8
- 239000004480 active ingredient Substances 0.000 claims description 8
- 239000005639 Lauric acid Substances 0.000 claims description 6
- 238000000605 extraction Methods 0.000 claims description 6
- 238000005187 foaming Methods 0.000 claims description 6
- 230000004580 weight loss Effects 0.000 claims description 6
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 239000012760 heat stabilizer Substances 0.000 claims description 5
- 238000007602 hot air drying Methods 0.000 claims description 5
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 4
- 150000001338 aliphatic hydrocarbons Chemical class 0.000 claims description 4
- 239000000945 filler Substances 0.000 claims description 4
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 4
- 239000004816 latex Substances 0.000 claims description 4
- 229920000126 latex Polymers 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 4
- 238000010907 mechanical stirring Methods 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- -1 polyoxyethylene Polymers 0.000 claims description 4
- 239000000654 additive Substances 0.000 claims description 3
- 239000004088 foaming agent Substances 0.000 claims description 3
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 3
- 230000000996 additive effect Effects 0.000 claims description 2
- 238000005259 measurement Methods 0.000 claims description 2
- 229920002554 vinyl polymer Polymers 0.000 claims description 2
- 238000013019 agitation Methods 0.000 claims 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims 1
- 125000003262 carboxylic acid ester group Chemical class [H]C([H])([*:2])OC(=O)C([H])([H])[*:1] 0.000 claims 1
- 150000001875 compounds Chemical class 0.000 claims 1
- 238000005461 lubrication Methods 0.000 claims 1
- 239000008029 phthalate plasticizer Substances 0.000 claims 1
- 239000002994 raw material Substances 0.000 claims 1
- 239000003017 thermal stabilizer Substances 0.000 claims 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 7
- 239000000178 monomer Substances 0.000 description 7
- 238000007720 emulsion polymerization reaction Methods 0.000 description 6
- 239000006260 foam Substances 0.000 description 5
- IRIAEXORFWYRCZ-UHFFFAOYSA-N Butylbenzyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCC1=CC=CC=C1 IRIAEXORFWYRCZ-UHFFFAOYSA-N 0.000 description 4
- BJQHLKABXJIVAM-UHFFFAOYSA-N bis(2-ethylhexyl) phthalate Chemical compound CCCCC(CC)COC(=O)C1=CC=CC=C1C(=O)OCC(CC)CCCC BJQHLKABXJIVAM-UHFFFAOYSA-N 0.000 description 4
- 235000010216 calcium carbonate Nutrition 0.000 description 4
- 150000001733 carboxylic acid esters Chemical class 0.000 description 4
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- MQIUGAXCHLFZKX-UHFFFAOYSA-N Di-n-octyl phthalate Natural products CCCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCC MQIUGAXCHLFZKX-UHFFFAOYSA-N 0.000 description 2
- ZVFDTKUVRCTHQE-UHFFFAOYSA-N Diisodecyl phthalate Chemical compound CC(C)CCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCC(C)C ZVFDTKUVRCTHQE-UHFFFAOYSA-N 0.000 description 2
- HBGGXOJOCNVPFY-UHFFFAOYSA-N diisononyl phthalate Chemical compound CC(C)CCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCC(C)C HBGGXOJOCNVPFY-UHFFFAOYSA-N 0.000 description 2
- 238000010790 dilution Methods 0.000 description 2
- 239000012895 dilution Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002386 leaching Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000011550 stock solution Substances 0.000 description 2
- 238000010557 suspension polymerization reaction Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 239000004604 Blowing Agent Substances 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 230000004520 agglutination Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000011437 continuous method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 229960002380 dibutyl phthalate Drugs 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- 230000005660 hydrophilic surface Effects 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 230000005661 hydrophobic surface Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 125000001424 substituent group Chemical group 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000005809 transesterification reaction Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F14/00—Homopolymers and 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
- C08F14/02—Monomers containing chlorine
- C08F14/04—Monomers containing two carbon atoms
- C08F14/06—Vinyl chloride
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/01—Processes of polymerisation characterised by special features of the polymerisation apparatus used
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/44—Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
-
- 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
-
- 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
- C08K3/01—Use of inorganic substances as compounding ingredients characterized by their specific function
- C08K3/014—Stabilisers against oxidation, heat, light or ozone
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L27/00—Compositions 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; Compositions of derivatives of such polymers
- C08L27/02—Compositions 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; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L27/04—Compositions 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; Compositions of derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
- C08L27/06—Homopolymers or copolymers of vinyl chloride
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/34—Paper
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/44—Resins; Plastics; Rubber; Leather
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/44—Resins; Plastics; Rubber; Leather
- G01N33/442—Resins; Plastics
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Polymers & Plastics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Physics & Mathematics (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- General Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
Description
The present invention relates to a method of measuring the plasticizer migration property of a paste vinyl chloride resin by an extraction agent, and more particularly, to a method of measuring the plasticizer migration property of a paste vinyl chloride resin by using a paste The present invention relates to a method for easily and easily measuring the plasticizer migration property of a plastisol produced using a vinyl chloride resin, and a method and apparatus for producing the plastisol using the same.
Paste A sheet coated with a plastisol produced by using a vinyl chloride resin is produced through a coating process by introducing various subsidiary materials when processing wallpaper products, for example. The plasticizer used to secure the fluidity of the vinyl resin is a problem of compatibility with vinyl chloride resin, so that the so-called plasticizer migration phenomenon in which the plasticizer seeps into paper (paper) during the foaming process is recognized as a problem.
The occurrence of plasticizer migration adversely affects the foaming process and the subsequent printing process, so quantitative analysis of the implementation of the plasticizer to prevent this in advance is essential.
On the other hand, the plasticizer migration phenomenon depends on the properties of the vinyl chloride resin, and in particular, the degree of hydrophilicity / hydrophobicity of the surface, and the type of the viscosity reducing agent added before the coating process are dominantly influenced. Is required.
In order to solve the problems of the prior art as described above, the present invention relates to a plasticizer for plastisol prepared by using a paste vinyl chloride resin, which is stable with respect to a vinyl chloride-based paste resin and is free from a free plasticizer, And a method and an apparatus for producing a plastisol using the same.
In order to achieve the above object, the present invention provides a method for producing a vinyl chloride resin, comprising the steps of: a) treating a vinyl chloride latex with an emulsifier and drying to obtain a surface-treated paste vinyl chloride resin; b) applying a plasticizer to the resin, coating and hot-air drying the plastisol obtained by mechanical stirring and defoaming; And c) measuring the plasticizer migration by injecting an extraction agent containing n-hexane as an active ingredient into the product of the step b) to determine the plasticizer migration property of the paste vinyl chloride resin. do.
The present invention also provides a method for producing a plastisol with a paste vinyl chloride resin, comprising the steps of: mixing a part of the prepared plastisol with an eluent containing n-hexane as an active ingredient; And measuring the plasticizer migration. The present invention also provides a method for producing a plastisol.
Further, the present invention relates to an apparatus for producing a plastisol, which comprises a plasticizer transitivity measuring device for a plastisol, wherein the plasticizer transitivity measuring instrument of the plastisol is a plasticizer transesterification measuring device for a plasticizer, And measuring transitivity of the plastisol.
According to the present invention, there is provided a method for easily and easily measuring the plasticizer migration property of a plastisol produced by using a paste vinyl chloride resin by an extraction agent which is stable to a vinyl chloride-based paste resin and elutes a free plasticizer And a method and an apparatus for producing the plastisol using the same. Concretely, it is possible to quantitatively calculate the plasticizer migration after the plastisol processing of the paste vinyl chloride resin in which the plasticizer is used, to quantitatively evaluate the plasticizer migration and mechanism, and to suggest the improvement direction.
Hereinafter, the present invention will be described in detail.
A method for measuring the plasticizer migration property of a paste vinyl chloride resin of the present invention comprises the steps of: a) treating a vinyl chloride latex with an emulsifier and drying the resulting paste to prepare a paste-finished vinyl chloride resin; b) applying a plasticizer to the resin, coating and hot-air drying the plastisol obtained by mechanical stirring and defoaming; And c) measuring the plasticizer migration by injecting an extraction agent containing n-hexane as an active ingredient into the product of b).
The plasticizer migration property of the paste vinyl chloride resin has a correlation with the content of the pre-plasticizer, the characteristics of the PVC resin surface, and the like.
The paste vinyl chloride resin may be one produced by suspension polymerization, micro suspension polymerization, emulsion polymerization or seed emulsion polymerization using an emulsifier, preferably emulsion polymerization or seed emulsion polymerization.
The seed used for the above-mentioned seed emulsion polymerization is not particularly limited in the case of a seed usually used in the production of a paste vinyl chloride resin.
The emulsifier is not particularly limited in the case of an emulsifier used in polymerization of a paste vinyl chloride resin.
Also, the paste vinyl chloride resin is a polymer latex comprising a vinyl chloride monomer, and the vinyl chloride monomer is at least one selected from the group consisting of vinyl chloride and a derivative thereof, and the vinyl chloride derivative is a hydrogen chloride Is a monomer substituted with another substituent.
The paste vinyl chloride resin may further comprise a monomer copolymerizable with the vinyl chloride monomer.
The step (a) is characterized in that, for example, lauric acid is treated with an emulsifier sensitized with NaOH to hydrophilize the resin surface, or an emulsifier of polyoxyethylene glycol is added to hydrophobicize the resin surface.
In the step (b), a filler, a foaming agent, a viscosity reducing agent and a heat stabilizer are added to the resin together with a plasticizer, and the mixture is foamed by mechanical stirring, defoaming coating and hot air drying to obtain a sheet.
The step b) may be carried out in the presence of a catalyst selected from the group consisting of dioctyl phthalate, di- (2-ethylhexyl) phthalate, dibutyl phthalate (DBP), benzyl butyl phthalate , BBP), di-isononyl phthalate (DINP), and di-isodecyl phthalate (DIDP).
The viscosity reducing agent may include, for example, a carboxylic acid ester and an aliphatic hydrocarbon.
For reference, the carboxylic acid ester (R-COO-R ') serves to keep the surface of the PVC particles hydrophilic, and the aliphatic hydrocarbon (CnH2n + 1) acts to lower the viscosity of the plasticizer and the liquid ingredient sub- , And a viscosity reducing agent having a desired property can be provided according to the blend ratio thereof.
In step c), the substrate is immersed for about 1 to 2 hours at a temperature of 30 to 65 ° C on the basis of 100 ml of the applied eluent, dried at room temperature for 12 to 24 hours, and then measured for plasticizer migration according to the following formula .
[Formula 1]
Plasticizer migration (%) = weight loss / addition x 100
(Wherein the weight loss is a value obtained by subtracting the total weight of the sample after elution from the total weight of the sample before elution, and the addition amount is a value obtained by multiplying the total weight of the sample before elution by the ratio of plasticizer in the sample)
The elution conditions correspond to the specific selection conditions of the present invention as described in the following examples.
The solvent is preferably applied to a paste vinyl chloride resin, and more preferably to a plasticizer migration test of a paste vinyl chloride resin. In this case, unlike other solvents, the main chain of the vinyl chloride polymer There is an effect of eluting a free plasticizer without directly damaging it.
As a specific example, the solvent may be a n-hexane stock solution or a dilution thereof, and it is preferable to use a stock solution of normal hexane for a small relative comparison of the plasticizer migration property between the paste and the vinyl chloride resin.
The normal hexane dilution solution may be a solution in which normal hexane is diluted with alcohol such as methanol. The n-hexane diluent preferably contains 30 to 50% by weight of n-hexane.
The method of measuring the plasticizer migration property of the paste vinyl chloride resin is simpler, quicker and more economical than the conventional measuring method.
The method for producing a plastisol of the present invention is a method for producing a plastisol with a paste vinyl chloride resin, comprising the steps of: mixing a part of the prepared plastisol with a leaching agent containing normal hexane as an active ingredient; And measuring the plasticizer migration.
The method for producing a paste vinyl chloride resin may further include changing an additive material condition when the agglutination time is less than a predetermined time.
The modified additives may include calcium carbonate, BYK-5120 and 5130 viscosity reducers, Ba-Zn and Ca-Zn series heat stabilizers, calcium carbonate fillers having an average particle size of 10 microns, and aliphatic hydrocarbons (CnH2n + 1) and a carboxylic acid ester (R-COO-R ').
It is preferable that the method for producing the plastisol is a continuous method.
The apparatus for producing a plastisol of the present invention includes a plasticizer transitivity measuring instrument of plastisol, wherein the plasticizer transitivity measuring instrument of the plastisol is a plasticizer transitivity measuring instrument for measuring the plasticizer transitivity by injecting a leaching agent containing normal hexane as an active ingredient .
The measurement of the plasticizer migration property of the above-mentioned paste vinyl chloride resin has an effect to prevent and check the plasticizer migration defect in advance during the coating, foaming or other processing of the plastisol made of paste vinyl chloride resin.
It will be apparent to those skilled in the art that various modifications and variations can be made in the present invention without departing from the spirit or scope of the present invention. Such variations and modifications are intended to be within the scope of the appended claims.
[Example]
Example 1: Coating Manufacturing 1
141 kg of deionized water, 185 ml of vinyl chloride monomer and 0.8 phm of vinyl chloride monomer, which is an emulsifier, were added to the 500 L high-pressure reactor, followed by seed emulsion polymerization at 61 ° C for 9 hours to prepare a paste Vinyl chloride resin was prepared.
To 100 parts by weight of the prepared paste vinyl chloride resin was added 0.25 part by weight of an emulsifier which was sensitized with NaOH to lauric acid, 60 parts by weight of dioctyl phthalate was added as a plasticizer to the dried paste vinyl chloride resin, and the mixture was stirred for 10 minutes by mechanical mixing Lt; / RTI >
The degummed plastisol was coated on paper paper and was gelled by a hot air dryer (about 200 ° C) to obtain a coating.
After that, plasticizer evaluation was carried out. Specifically, 100 ml of normal hexane was added, and the resultant was immersed at 50 ° C for 2 hours and dried at room temperature for 12 hours. The plasticizer migration was measured according to the following formula 1, and the results are summarized in Table 1 below.
[Formula 1]
Plasticizer migration (%) = weight loss / addition x 100
(Wherein the weight loss is a value obtained by subtracting the total weight of the sample after elution from the total weight of the sample before elution, and the addition amount is a value obtained by multiplying the total weight of the sample before elution by the ratio of plasticizer in the sample)
Example 2: Coating Manufacturing 2
Except that 0.25 parts by weight of an emulsifying agent lauric acid-saturated with NaOH was added in the same manner as in Example 1, and 0.7 part by weight of polyoxyethylene glycol instead of the dried paste vinyl chloride resin was added thereto to prepare a paste-made vinyl chloride resin. A coating was obtained in the same manner as in Example 1.
The plasticizer migration properties were measured in the same manner as in Example 1, and the results are summarized in Table 1 below.
Example 3: foam sheet Manufacturing 1
The procedure of Example 1 was repeated except that 0.25 part by weight of an emulsifier which had been immobilized with NaOH in lauric acid was added to the lauric acid in Example 1 to prepare a plastisol using the dried paste chlorinated vinyl resin as a product for foaming. The same method was repeated.
Specifically, 100 parts by weight of a vinyl chloride resin, 100 parts by weight of a plasticizer, 150 parts by weight of calcium carbonate (CaCO3, OMYA10), 3 parts by weight of a blowing agent (DWPX-03), a viscosity reducing agent (BYK5120 Or 5130) and 25 parts by weight of a heat stabilizer (BZ or CZ series heat stabilizer).
The plasticizer migration properties were measured in the same manner as in Example 1, and the results are summarized in Table 1 below.
Example 4: foam sheet Manufacturing 2
In Example 3, 0.25 parts by weight of an emulsifier immobilized with NaOH was added to the lauric acid of Example 1, and 0.7 part by weight of polyoxyethylene glycol of Example 2 was added to the dried paste-type vinyl chloride resin to prepare dried paste vinyl chloride Based resin was used instead of the above resin.
Then, the plasticizer migration properties were measured in the same manner as in Example 1, and the results are summarized together in Table 1 below.
Example 5: foam sheet Manufacturing 3
In Example 4, the same procedure as in Example 3 was repeated except that BYK-5120, which has a higher carboxylic acid ester content, was used in place of the viscosity reducing agent BYK-5130 in the subsidiary materials contained in the foamed product prescription.
Then, the plasticizer migration properties were measured in the same manner as in Example 1, and the results are summarized together in Table 1 below.
Comparative Example 1 : Example 1 under 12 hours of room temperature drying
The experiment was carried out in the same manner as in Example 1 except that the sample was not dried at room temperature for 12 hours after treatment at 50 ° C for 2 hours in Example 1.
Comparative Example 2 : Example 1 > C for 2 hours at 50 < 0 > C
The experiment was carried out in the same manner as in Example 1, except that the sample was dried at room temperature for 12 hours without treatment at 50 ° C for 2 hours.
Comparative Example 3 : Example 3 was treated at 50 캜 for 2 hours at a low temperature
The experiment was carried out in the same manner as in Example 3, except that the low temperature treatment at 30 占 폚 was used instead of 50 占 폚 in Example 3. [
Comparative Example 4 : Example 3 was treated at 50 ° C for 2 hours at a high temperature
The experiment was carried out in the same manner as in Example 3, except that the high-temperature treatment at 65 ° C was used instead of the 50 ° C in the above-mentioned Example 3.
[Test Example]
The plasticizer migration rates measured in Examples 1-5 and Comparative Examples 1-4 are shown in Table 1 below.
As shown in Table 1 above, the results of the comparison of Examples 1 to 5 and Comparative Examples 1 to 4 confirm the use of n-hexane as an eluent for the plasticizer migration and proper conditions.
In the plastisol coating of Examples 1 and 2, the results of plasticizer migration according to the surface characteristics of the PVC resin could be predicted. In particular, it was confirmed that the migration rate was high in the hydrophilic characteristics of Example 2. Specifically, the hydrophobic surface properties of Example 1 increase the compatibility between the PVC and the plasticizer and are effective in the plasticizer migration phenomenon. The hydrophilic surface properties of Example 2 lower the compatibility between the PVC and the plasticizer, thereby worsening the plasticizer migration phenomenon .
The results of plasticizer migration can be predicted according to the surface characteristics and the viscosity reducing agent of PVC resin in the production of the foam sheet of the plastisols of Examples 3 to 5. In particular, the migration rate was high in the hydrophilic characteristic of Example 4, Even when the hydrophobic property of Example 4 was used, it was found that the migration rate was somewhat higher when the viscosity reducing agent having hydrophilicity was used, depending on the kind of the viscosity reducing agent contained in the foam formulation.
It was also confirmed that even when the same eluent was used, improved plasticizer migration results were obtained compared to the elution conditions of Comparative Examples 1 to 4 under the elution conditions of Examples 1 to 5.
Claims (10)
Wherein the step a) is a step of treating the surface of the resin with an emulsifier which has been subjected to lubrication with lauric acid with NaOH, hydrophilizing the surface of the resin, or adding an emulsifying agent of polyoxyethylene glycol to hydrophobize the surface of the resin. Method of measuring transitivity.
Wherein the step (b) is a step of applying a filler, a foaming agent, a viscosity reducing agent and a heat stabilizer together with a plasticizer to the resin, and subjecting the resultant to a mechanical agitation, de-foaming coating and hot air drying and foaming to obtain a sheet. ≪ / RTI >
Wherein said step (b) is a step of introducing a phthalate plasticizer into said plasticized vinyl chloride resin.
Wherein the viscosity reducing agent comprises a carboxylic acid ester and an aliphatic hydrocarbon.
Wherein the step (c) is carried out by immersing the sample at a temperature of 30 to 65 ° C for 1 to 2 hours and drying at room temperature for 12 to 24 hours on the basis of 100 ml of the applied eluent, and then measuring the plasticizer migration according to the following formula Method of measuring plasticizer migration of vinyl based resin.
[Formula 1]
Plasticizer migration (%) = weight loss / addition x 100
(Wherein the weight loss is a value obtained by subtracting the total weight of the sample after elution from the total weight of the sample before elution, and the addition amount is a value obtained by multiplying the total weight of the sample before elution by the ratio of plasticizer in the sample)
Mixing a part of the prepared plastisol with an eluent containing normal hexane as an active ingredient; And measuring the plasticizer migration. ≪ RTI ID = 0.0 > 11. < / RTI >
The method of claim 1, further comprising the step of: if the plasticizer migration measurement is less than a predetermined value, changing the additive material condition.
Wherein the sub-raw material condition is at least one selected from a calcium carbonate-based filler, an AZO-based compound foaming agent, a viscosity reducing agent containing a carboxyl group, and a Ca-Zn or Ba-Zn thermal stabilizer.
A plasticizer transitivity meter of plastisols,
Wherein the plasticizer transitivity measuring device of the plastisol is a device for measuring the plasticizer migration property by injecting an extraction agent containing normal hexane as an active ingredient.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20190089133A (en) * | 2011-11-07 | 2019-07-30 | 스미또모 가가꾸 가부시키가이샤 | Curable resin composition |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| KR20190089133A (en) * | 2011-11-07 | 2019-07-30 | 스미또모 가가꾸 가부시키가이샤 | Curable resin composition |
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