JP6591038B2 - 高吸水性樹脂の単一粒子の破砕強度測定方法 - Google Patents
高吸水性樹脂の単一粒子の破砕強度測定方法 Download PDFInfo
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- 239000002245 particle Substances 0.000 title claims description 60
- 238000000034 method Methods 0.000 title claims description 25
- 229920000247 superabsorbent polymer Polymers 0.000 title description 6
- 229920005989 resin Polymers 0.000 claims description 107
- 239000011347 resin Substances 0.000 claims description 107
- 239000000843 powder Substances 0.000 claims description 26
- 239000000178 monomer Substances 0.000 claims description 19
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 18
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 11
- -1 2-hydroxypropyl Chemical group 0.000 claims description 9
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 7
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 7
- 238000003825 pressing Methods 0.000 claims description 7
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims description 6
- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Chemical compound OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 claims description 6
- 229920006037 cross link polymer Polymers 0.000 claims description 5
- 239000002202 Polyethylene glycol Substances 0.000 claims description 4
- 230000002378 acidificating effect Effects 0.000 claims description 4
- 125000004432 carbon atom Chemical group C* 0.000 claims description 4
- 150000002009 diols Chemical class 0.000 claims description 4
- 229920001223 polyethylene glycol Polymers 0.000 claims description 4
- 230000000379 polymerizing effect Effects 0.000 claims description 4
- JAHNSTQSQJOJLO-UHFFFAOYSA-N 2-(3-fluorophenyl)-1h-imidazole Chemical compound FC1=CC=CC(C=2NC=CN=2)=C1 JAHNSTQSQJOJLO-UHFFFAOYSA-N 0.000 claims description 3
- 125000000954 2-hydroxyethyl group Chemical group [H]C([*])([H])C([H])([H])O[H] 0.000 claims description 3
- AUZRCMMVHXRSGT-UHFFFAOYSA-N 2-methylpropane-1-sulfonic acid;prop-2-enamide Chemical compound NC(=O)C=C.CC(C)CS(O)(=O)=O AUZRCMMVHXRSGT-UHFFFAOYSA-N 0.000 claims description 3
- MJIFFWRTVONWNO-UHFFFAOYSA-N 3-oxopent-4-ene-1-sulfonic acid Chemical compound OS(=O)(=O)CCC(=O)C=C MJIFFWRTVONWNO-UHFFFAOYSA-N 0.000 claims description 3
- SVYPQURSUBDSIQ-UHFFFAOYSA-N 4-methyl-3-oxopent-4-ene-1-sulfonic acid Chemical compound CC(=C)C(=O)CCS(O)(=O)=O SVYPQURSUBDSIQ-UHFFFAOYSA-N 0.000 claims description 3
- AEYSASDBPHWTGR-UHFFFAOYSA-N 4-oxohex-5-ene-3-sulfonic acid Chemical compound CCC(S(O)(=O)=O)C(=O)C=C AEYSASDBPHWTGR-UHFFFAOYSA-N 0.000 claims description 3
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 3
- 229910000831 Steel Inorganic materials 0.000 claims description 3
- 125000003277 amino group Chemical group 0.000 claims description 3
- 125000000129 anionic group Chemical group 0.000 claims description 3
- 150000001875 compounds Chemical class 0.000 claims description 3
- LDHQCZJRKDOVOX-NSCUHMNNSA-N crotonic acid Chemical compound C\C=C\C(O)=O LDHQCZJRKDOVOX-NSCUHMNNSA-N 0.000 claims description 3
- 239000001530 fumaric acid Substances 0.000 claims description 3
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 3
- LVHBHZANLOWSRM-UHFFFAOYSA-N methylenebutanedioic acid Natural products OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 claims description 3
- 150000003839 salts Chemical class 0.000 claims description 3
- 239000010959 steel Substances 0.000 claims description 3
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 claims description 3
- LDHQCZJRKDOVOX-UHFFFAOYSA-N trans-crotonic acid Natural products CC=CC(O)=O LDHQCZJRKDOVOX-UHFFFAOYSA-N 0.000 claims description 3
- 229910010293 ceramic material Inorganic materials 0.000 claims 1
- 238000000691 measurement method Methods 0.000 claims 1
- 238000010298 pulverizing process Methods 0.000 claims 1
- 239000002250 absorbent Substances 0.000 description 22
- 238000004519 manufacturing process Methods 0.000 description 17
- 239000000463 material Substances 0.000 description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 12
- 238000010521 absorption reaction Methods 0.000 description 8
- 239000002504 physiological saline solution Substances 0.000 description 8
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 229920000642 polymer Polymers 0.000 description 6
- 238000006116 polymerization reaction Methods 0.000 description 6
- 239000000499 gel Substances 0.000 description 5
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- 230000000704 physical effect Effects 0.000 description 4
- 230000002745 absorbent Effects 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000004898 kneading Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 239000002952 polymeric resin Substances 0.000 description 2
- 235000011121 sodium hydroxide Nutrition 0.000 description 2
- 239000002689 soil Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000010557 suspension polymerization reaction Methods 0.000 description 2
- 229920001059 synthetic polymer Polymers 0.000 description 2
- 229920003002 synthetic resin Polymers 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical compound NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 description 1
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 1
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
- 229960005070 ascorbic acid Drugs 0.000 description 1
- 235000010323 ascorbic acid Nutrition 0.000 description 1
- 239000011668 ascorbic acid Substances 0.000 description 1
- 229920005601 base polymer Polymers 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 125000004386 diacrylate group Chemical group 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010528 free radical solution polymerization reaction Methods 0.000 description 1
- 238000010413 gardening Methods 0.000 description 1
- 239000000017 hydrogel Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N3/08—Investigating strength properties of solid materials by application of mechanical stress by applying steady tensile or compressive forces
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/10—Investigating individual particles
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/0014—Type of force applied
- G01N2203/0016—Tensile or compressive
- G01N2203/0019—Compressive
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/0058—Kind of property studied
- G01N2203/006—Crack, flaws, fracture or rupture
- G01N2203/0067—Fracture or rupture
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/02—Details not specific for a particular testing method
- G01N2203/026—Specifications of the specimen
- G01N2203/0286—Miniature specimen; Testing on microregions of a specimen
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- Chemical & Material Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- Physics & Mathematics (AREA)
- Pathology (AREA)
- General Health & Medical Sciences (AREA)
- Dispersion Chemistry (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
- Investigating Strength Of Materials By Application Of Mechanical Stress (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Description
本出願は、2015年10月7日付の韓国特許出願第10−2015−0140934号に基づく優先権の利益を主張し、当該韓国特許出願の文献に開示された全ての内容は本明細書の一部として含まれる。
Geometry Diameter:8mm
SAP粒子の大きさ:600−850μm
押圧する速度:0.01mm/s
本発明による高吸水性樹脂の破砕強度測定時に使用されるシリンダーは直径8mmの大きさを有するもので、スチールやセラミックなどの多様な材質で製造されることができる。また、前記シリンダーは高吸水性樹脂より強度が大きく、高吸水性樹脂と接する面とその反対面である両面いずれも平らな材質および形態を有することでありうる。
[計算式1]
CRC(g/g) = [[W2(g) - W1(g)]/W0(g)] - 1
前記計算式1において、
W0(g)は、吸水性樹脂の重量(g)であり、W1(g)は、吸水性樹脂を使用せず、遠心分離機を用いて250Gで3分間脱水した後に測定した装置重量であり、W2(g)は、常温で0.9質量%の生理食塩水に吸水性樹脂を30分間浸水した後、遠心分離機を用いて250Gで3分間脱水した後、吸水性樹脂を含んで測定した装置重量である。
[計算式2]
AUP(g/g) = [W4(g) - W3(g)]/ W0(g)
前記計算式2において、
W0(g)は、吸水性樹脂の重量(g)であり、W3(g)は、吸水性樹脂の重量および前記吸水性樹脂に荷重を付与できる装置重量の総和であり、W4(g)は、荷重(0.7psi)下に1時間にかけて前記吸水性樹脂に水分を供給した後、水分が吸収された吸水性樹脂の重量および前記吸水性樹脂に荷重を付与できる装置重量の総和である。
製造例1:高吸水性樹脂ベースレジンの製造
まず、高吸水性樹脂は次のような方法で製造した。アクリル酸100g、架橋剤としてポリエチレングリコールジアクリレート(Mw=523)0.25−0.5g、50%苛性ソーダ(NaOH)83.3gおよび水89.8gを混合して、単量体濃度が45重量%のモノマー水溶液組成比を有するように製造した。
以降、前記モノマー水溶液810gを、まず、0.18%アスコルビン酸溶液30.54gと、1%過硫酸ナトリウム溶液33gとを混合し、0.15%過酸化水素溶液30.45gと共に連続的に重合しながらニーディングできる重合機の供給部を通して投入して重合を実施した。この時、重合機の温度は80℃に維持し、重合の最高温度は110℃、重合時間は1分15秒である。以降、引き続き、ニーディングを実施して20分間重合とニーディングを実施した。以降生成された重合体の大きさは0.2cm以下に分布された。この時、最終形成された含水ゲル重合体の含水率は51重量%であった。
次に、前記含水ゲル重合体に対して180℃の熱風乾燥機で30分間乾燥し、乾燥された含水ゲル重合体をピンミル粉砕機で粉砕した。その後、ふるい(sieve)を利用して粒度(平均粒径)が150μm未満の重合体と粒度150μm乃至850μmの重合体を分級してCRCが34gのベースポリマーを得た。
前記製造例1により製造された高吸水性樹脂のベースレジン(base resin)を、以前の他の高分子樹脂の製造工程中に発生した微粉と混合して再組立する工程を通して高吸水性樹脂再組立体を製造した。
次のような方法で、製造例1の高吸水性樹脂ベースレジン(base resin)の単一粒子と製造例2の高吸水性樹脂再組立体の単一粒子に対する破砕強度を測定した。
Claims (6)
- 粒子の大きさ550ないし900μmの高吸水性樹脂の単一粒子を、直径8mmのシリンダーを使って0.005ないし0.05mm/sの速度で定速加圧して破砕される時点の力である破砕強度を測定する段階を含み、
前記高吸水性樹脂の単一粒子は酸性基を含み少なくとも一部が中和した水溶性エチレン系不飽和単量体を重合させた粉末形態のベース樹脂を炭素数2ないし8のジオールまたはグリコール系化合物で表面架橋させた架橋重合体を含み、乾燥状態のものである、高吸水性樹脂の単一粒子の破砕強度測定方法。 - 前記水溶性エチレン系不飽和単量体は、アクリル酸、メタクリル酸、無水マレイン酸、フマル酸、クロトン酸、イタコン酸、2−アクリロイルエタンスルホン酸、2−メタクリロイルエタンスルホン酸、2−(メタ)アクリロイルプロパンスルホン酸、または2−(メタ)アクリルアミド−2−メチルプロパンスルホン酸の陰イオン性単量体とその塩;(メタ)アクリルアミド、N−置換(メタ)アクリレート、2−ヒドロキシエチル(メタ)アクリレート、2−ヒドロキシプロピル(メタ)アクリレート、メトキシポリエチレングリコール(メタ)アクリレートまたはポリエチレングリコール(メタ)アクリレートの非イオン系親水性含有単量体;および(N,N)−ジメチルアミノエチル(メタ)アクリレートまたは(N,N)−ジメチルアミノプロピル(メタ)アクリルアミドのアミノ基含有不飽和単量体とその4級化物;からなる群より選択された1種以上を含む、請求項1に記載の高吸水性樹脂の単一粒子の破砕強度測定方法。
- 前記シリンダーはスチールまたはセラミック材質からなる、請求項1または2に記載の高吸水性樹脂の単一粒子の破砕強度測定方法。
- 前記高吸水性樹脂の粒子の大きさは600ないし850μmである、請求項1〜3のいずれかに記載の高吸水性樹脂の単一粒子の破砕強度測定方法。
- 前記シリンダーの定速加圧速度を0.01mm/sで行う、請求項1〜4のいずれかに記載の高吸水性樹脂の単一粒子の破砕強度測定方法。
- 前記高吸水性樹脂の単一粒子の破砕強度は、2kgf(19.6N)以上である、請求項1〜5のいずれかに記載の高吸水性樹脂の単一粒子の破砕強度測定方法。
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KR10-2015-0140934 | 2015-10-07 | ||
KR1020150140934A KR102009909B1 (ko) | 2015-10-07 | 2015-10-07 | 고흡수성 수지 단일 입자의 파쇄강도 측정 방법 |
PCT/KR2016/010025 WO2017061705A1 (ko) | 2015-10-07 | 2016-09-07 | 고흡수성 수지 단일 입자의 파쇄강도 측정 방법 |
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EP (1) | EP3312585A4 (ja) |
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KR101750013B1 (ko) * | 2016-02-19 | 2017-06-22 | 주식회사 엘지화학 | 고흡수성 수지 |
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WO2017061705A1 (ko) | 2017-04-13 |
US10634595B2 (en) | 2020-04-28 |
KR102009909B1 (ko) | 2019-08-21 |
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EP3312585A1 (en) | 2018-04-25 |
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