JP2010120241A - Production method for extrusion molding - Google Patents
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- JP2010120241A JP2010120241A JP2008295329A JP2008295329A JP2010120241A JP 2010120241 A JP2010120241 A JP 2010120241A JP 2008295329 A JP2008295329 A JP 2008295329A JP 2008295329 A JP2008295329 A JP 2008295329A JP 2010120241 A JP2010120241 A JP 2010120241A
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- 238000001125 extrusion Methods 0.000 title claims abstract description 78
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 14
- 239000012778 molding material Substances 0.000 claims abstract description 24
- 239000000843 powder Substances 0.000 claims abstract description 24
- 239000002994 raw material Substances 0.000 claims abstract description 17
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000011230 binding agent Substances 0.000 claims abstract description 8
- 239000002904 solvent Substances 0.000 claims abstract description 8
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 5
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 5
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910052787 antimony Inorganic materials 0.000 claims abstract description 5
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910052792 caesium Inorganic materials 0.000 claims abstract description 5
- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical compound [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910052802 copper Inorganic materials 0.000 claims abstract description 5
- 239000010949 copper Substances 0.000 claims abstract description 5
- 239000011964 heteropoly acid Substances 0.000 claims abstract description 5
- 229910052742 iron Inorganic materials 0.000 claims abstract description 5
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 5
- 239000011733 molybdenum Substances 0.000 claims abstract description 5
- 229910052720 vanadium Inorganic materials 0.000 claims abstract description 5
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims abstract description 5
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910052684 Cerium Inorganic materials 0.000 claims abstract description 4
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims abstract description 4
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910052785 arsenic Inorganic materials 0.000 claims abstract description 4
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910052797 bismuth Inorganic materials 0.000 claims abstract description 4
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910052796 boron Inorganic materials 0.000 claims abstract description 4
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 4
- 239000010941 cobalt Substances 0.000 claims abstract description 4
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910052746 lanthanum Inorganic materials 0.000 claims abstract description 4
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910052700 potassium Inorganic materials 0.000 claims abstract description 4
- 239000011591 potassium Substances 0.000 claims abstract description 4
- 229910052701 rubidium Inorganic materials 0.000 claims abstract description 4
- IGLNJRXAVVLDKE-UHFFFAOYSA-N rubidium atom Chemical compound [Rb] IGLNJRXAVVLDKE-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910052709 silver Inorganic materials 0.000 claims abstract description 4
- 239000004332 silver Substances 0.000 claims abstract description 4
- 229910052716 thallium Inorganic materials 0.000 claims abstract description 4
- BKVIYDNLLOSFOA-UHFFFAOYSA-N thallium Chemical compound [Tl] BKVIYDNLLOSFOA-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000012783 reinforcing fiber Substances 0.000 claims description 17
- 235000012438 extruded product Nutrition 0.000 claims description 15
- 229910052698 phosphorus Inorganic materials 0.000 claims description 4
- 239000011574 phosphorus Substances 0.000 claims description 4
- 239000000835 fiber Substances 0.000 abstract description 16
- 230000002787 reinforcement Effects 0.000 abstract description 3
- 239000003054 catalyst Substances 0.000 description 11
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 7
- 239000000463 material Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 230000002950 deficient Effects 0.000 description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 2
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 239000003463 adsorbent Substances 0.000 description 2
- 238000005452 bending Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- -1 hexane and heptane Chemical compound 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 235000019198 oils Nutrition 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 2
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 description 1
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- 241001391944 Commicarpus scandens Species 0.000 description 1
- STNJBCKSHOAVAJ-UHFFFAOYSA-N Methacrolein Chemical compound CC(=C)C=O STNJBCKSHOAVAJ-UHFFFAOYSA-N 0.000 description 1
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 239000004642 Polyimide Substances 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 239000001099 ammonium carbonate Substances 0.000 description 1
- 235000012501 ammonium carbonate Nutrition 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 1
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 1
- 235000011130 ammonium sulphate Nutrition 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000002274 desiccant Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 239000012784 inorganic fiber Substances 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 239000003350 kerosene Substances 0.000 description 1
- 229940057995 liquid paraffin Drugs 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229920002401 polyacrylamide Polymers 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 229920002379 silicone rubber Polymers 0.000 description 1
- 239000004945 silicone rubber Substances 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 235000002639 sodium chloride Nutrition 0.000 description 1
- 235000012424 soybean oil Nutrition 0.000 description 1
- 239000003549 soybean oil Substances 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 239000012209 synthetic fiber Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
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Abstract
Description
本発明は、押出成形体の製造方法に関し、より詳細には、機械的強度が向上した押出成形体の製造方法に関する。 The present invention relates to a method for manufacturing an extrusion-molded body, and more particularly to a method for manufacturing an extrusion-molded body having improved mechanical strength.
一般に、触媒、触媒担体、吸着材、乾燥材、調湿材等は、直径2〜10mm、長さ2〜20mm程度の円柱形または円筒形等の成形体に成形され、反応器に充填されて種々の化学反応プロセスに使用される。このような触媒等の成形体を製造するために、従来から押出成形法が採用されている。すなわち、所定の成形材料をダイの押出孔から押出し、押出された成形体を所定の長さに切断して押出成形体を得ている(例えば、特許文献1参照)。 In general, a catalyst, a catalyst carrier, an adsorbent, a drying material, a humidity control material, etc. are formed into a cylindrical or cylindrical shaped body having a diameter of about 2 to 10 mm and a length of about 2 to 20 mm, and filled into a reactor. Used in various chemical reaction processes. In order to produce such a molded body such as a catalyst, an extrusion molding method has been conventionally employed. That is, a predetermined molding material is extruded from an extrusion hole of a die, and the extruded molded body is cut into a predetermined length to obtain an extruded molded body (for example, see Patent Document 1).
前記成形材料は、原料粉末と溶媒とを含み、前記溶媒には、通常、バインダー成分が溶解されている。そして、成形体の強度を向上させる上で、成形材料に補強用繊維を混ぜ込み、分散させることが行なわれている。 The molding material includes a raw material powder and a solvent, and a binder component is usually dissolved in the solvent. And in order to improve the intensity | strength of a molded object, the fiber for a reinforcement is mixed and disperse | distributed to a molding material.
ところが、押出成形体は、たとえ補強用繊維が分散されていても、床に落とす等の衝撃や圧力で割れやすいという問題があった。特に、円柱形または円筒形の成形体の場合には、押出方向に沿って割れやすかった。
本発明の課題は、機械的強度が向上した押出成形体の製造方法を提供することである。 The subject of this invention is providing the manufacturing method of the extrusion molded object which mechanical strength improved.
本発明者らは、上記課題を解決すべく鋭意研究を重ねた結果、以下の知見を見出した。すなわち、押出成形法では、図2に示すように、成形材料をダイ100の押出孔101から矢印Aに示す押出方向へ押出す。このとき、成形体110内の補強用繊維の向きが、押出方向(軸方向)に配向されやすい。それゆえ成形体110は、押出方向に直交する矢印Bに示す方向(径方向)の強度が強くなって、押出方向の強度が弱くなり、衝撃や圧力で割れやすくなる。
As a result of intensive studies to solve the above problems, the present inventors have found the following findings. That is, in the extrusion molding method, as shown in FIG. 2, the molding material is extruded from the
通常、押出孔101の先端には、成形体110に曲がりや反りが発生するのを抑制する上で、直管部102が設けられている。この直管部102において、特に補強用繊維の向きが押出方向に配向されやすい。
Usually, a
本発明者らは、これらの知見に基づき、鋭意研究を重ねた。その結果、直管部102における内径と長さとの比が特定範囲であれば、成形体110内の補強用繊維の向きが押出方向に配向されるのを抑制することができるという新たな事実を見出し、本発明を完成させるに至った。
Based on these findings, the present inventors conducted extensive research. As a result, if the ratio between the inner diameter and the length in the
すなわち、本発明の押出成形体の製造方法は、原料粉末と、補強用繊維と、バインダー成分を溶解した溶媒とを含む成形材料をダイの押出孔から押出して押出成形体を製造する方法であって、前記押出孔の直管部は、内径Dと長さLとの比(D/L)が2〜6であることを特徴とする。 That is, the method for producing an extruded product of the present invention is a method for producing an extruded product by extruding a molding material containing raw material powder, reinforcing fibers, and a solvent in which a binder component is dissolved from an extrusion hole of a die. The straight tube portion of the extrusion hole has a ratio (D / L) of the inner diameter D to the length L of 2 to 6.
本発明の有用性がより向上する上で、前記押出成形体の形状が円柱形または円筒形であるのが好ましい。
前記直管部の長さLが3mm以下であるのが好ましい。
前記原料粉末は、リンおよびモリブテンを含み、かつバナジウム、カリウム、ルビジウム、セシウムおよびタリウムから選ばれる少なくとも1つの元素と、銅、ヒ素、アンチモン、ホウ素、銀、ビスマス、鉄、コバルト、ランタンおよびセリウムから選ばれる少なくとも1つの元素とを含むヘテロポリ酸であるのが好ましい。
In order to further improve the usefulness of the present invention, the shape of the extruded product is preferably a columnar shape or a cylindrical shape.
It is preferable that the length L of the straight pipe portion is 3 mm or less.
The raw material powder contains phosphorus and molybdenum, and includes at least one element selected from vanadium, potassium, rubidium, cesium and thallium, and copper, arsenic, antimony, boron, silver, bismuth, iron, cobalt, lanthanum and cerium. A heteropolyacid containing at least one selected element is preferred.
本発明によれば、所定の成形材料を、内径Dと長さLとの比(D/L)が2〜6である直管部を有する押出孔から押出すようにした。これにより、押出される成形体に曲がりや反りが発生するのを抑制しつつ、該成形体内の補強用繊維の向きが押出方向に配向されるのを抑制することができる。すなわち、成形体内の補強用繊維の向きがランダムに分散されるので、押出方向の強度が弱くなるのを抑制することができ、成形体の機械的強度が向上し、該成形体を割れ難くすることができる。 According to the present invention, a predetermined molding material is extruded from an extrusion hole having a straight pipe portion in which the ratio (D / L) of the inner diameter D to the length L is 2 to 6. Thereby, it is possible to suppress the orientation of the reinforcing fibers in the molded body from being oriented in the extrusion direction while suppressing the bending and warping of the molded body to be extruded. That is, since the directions of the reinforcing fibers in the molded body are randomly dispersed, it is possible to suppress the strength in the extrusion direction from being weakened, the mechanical strength of the molded body is improved, and the molded body is difficult to break. be able to.
本発明にかかる成形材料は、原料粉末と、補強用繊維と、バインダー成分を溶解した溶媒とを含む。前記原料粉末としては、リンおよびモリブテンを含み、かつバナジウム、カリウム、ルビジウム、セシウムおよびタリウムから選ばれる少なくとも1つの元素と、銅、ヒ素、アンチモン、ホウ素、銀、ビスマス、鉄、コバルト、ランタンおよびセリウムから選ばれる少なくとも1つの元素とを含むヘテロポリ酸が好ましい。 The molding material concerning this invention contains raw material powder, the fiber for reinforcement, and the solvent which melt | dissolved the binder component. The raw material powder includes phosphorus and molybdenum, and at least one element selected from vanadium, potassium, rubidium, cesium and thallium, and copper, arsenic, antimony, boron, silver, bismuth, iron, cobalt, lanthanum and cerium. A heteropolyacid containing at least one element selected from is preferred.
前記ヘテロポリ酸以外の成形材料としては、例えば特開2003−10700号公報に記載されているメタクロレインを気相接触酸化してメタクリル酸を製造するための触媒粉末やその前駆体粉末、特公昭59−15015号公報に記載されているアルミナからなる触媒担体を製造するためのアルミナやアルミナ前駆体の粉末等が挙げられる。なお、本発明にかかる原料粉末は、前記で例示したものに限定されるものではなく、所望の原料粉末を用いることができる。 Examples of the molding material other than the heteropolyacid include catalyst powder and precursor powder thereof for producing methacrylic acid by vapor phase catalytic oxidation of methacrolein described in JP-A-2003-10700. Examples include alumina and alumina precursor powder for producing a catalyst carrier made of alumina described in JP-A-151515. In addition, the raw material powder concerning this invention is not limited to what was illustrated above, A desired raw material powder can be used.
前記補強用繊維としては、例えばガラス繊維、炭素繊維、炭化ケイ素繊維、アルミナ繊維等の無機繊維、ポリエステル繊維、ポリアミド繊維(ナイロン繊維等)、ポリイミド繊維等の合成繊維等が挙げられる。 Examples of the reinforcing fibers include inorganic fibers such as glass fibers, carbon fibers, silicon carbide fibers, and alumina fibers, synthetic fibers such as polyester fibers, polyamide fibers (nylon fibers, etc.), polyimide fibers, and the like.
補強用繊維の繊維長は、成形体の大きさ等によって決定されるため、特に限定されるものではないが、平均繊維長としては0 .01〜1mm 、好ましくは0.1〜0.8mm、平均繊維径としては1〜10μm、好ましくは1.5〜5μmであるのがよい。補強用繊維の含有量としては、原料粉末(乾燥重量)100重量部に対して1〜30重量部、好ましくは2〜20重量部であるのがよい。 The fiber length of the reinforcing fiber is not particularly limited because it is determined by the size of the molded body, but the average fiber length is 0. 01 to 1 mm, preferably 0.1 to 0.8 mm, and the average fiber diameter is 1 to 10 μm, preferably 1.5 to 5 μm. The content of the reinforcing fiber is 1 to 30 parts by weight, preferably 2 to 20 parts by weight with respect to 100 parts by weight of the raw material powder (dry weight).
前記バインダー成分としては、例えば硝酸アンモニウム、炭酸アンモニウム、硫酸アンモニウム、塩化アンモニウム、塩化ナトリウム等の無機塩、セルロース、ポリビニルアルコール、ピリジン、ポリアクリルアミド、エチレングリコール、ポリエチレングリコール、グリセリン等の有機化合物等が挙げられる。 Examples of the binder component include inorganic salts such as ammonium nitrate, ammonium carbonate, ammonium sulfate, ammonium chloride, and sodium chloride, and organic compounds such as cellulose, polyvinyl alcohol, pyridine, polyacrylamide, ethylene glycol, polyethylene glycol, and glycerin.
バインダー成分の含有量としては、原料粉末と補強用繊維との混合物(以下、「触媒粉末」と言う。)100重量部に対して1〜20重量部、好ましくは1〜10重量部であるのがよい。 The content of the binder component is 1 to 20 parts by weight, preferably 1 to 10 parts by weight with respect to 100 parts by weight of the mixture of raw material powder and reinforcing fiber (hereinafter referred to as “catalyst powder”). Is good.
前記溶媒としては、例えば水、メタノール、エタノール、プロピルアルコール等の炭素数1〜4のアルコール、ヘキサン、ヘプタン等の炭化水素、流動パラフィン、大豆油、白絞油、軽油、灯油等のパラフィン類等が挙げられる。溶媒の含有量としては、触媒粉末100重量部に対して1〜20重量部、好ましくは1〜15重量部であるのがよい。 Examples of the solvent include water, alcohols having 1 to 4 carbon atoms such as methanol, ethanol, and propyl alcohol, hydrocarbons such as hexane and heptane, liquid paraffin, soybean oil, white drawn oil, light oil, and kerosene. Is mentioned. The content of the solvent is 1 to 20 parts by weight, preferably 1 to 15 parts by weight with respect to 100 parts by weight of the catalyst powder.
このような成形材料から押出成形体を製造するのに使用する押出成形装置としては、図1に示すものが挙げられる。図1は、本発明の押出成形体を製造する押出成形装置の一実施形態を示す部分拡大断面図である。同図に示すように、この押出成形装置20は、前記した成形材料を、ダイ10の略中央部に形成された押出孔11から連続的に押出すことができるよう構成されている。
As an extrusion molding apparatus used for producing an extrusion-molded body from such a molding material, the one shown in FIG. 1 can be mentioned. FIG. 1 is a partially enlarged cross-sectional view showing an embodiment of an extrusion molding apparatus for producing an extruded product of the present invention. As shown in the figure, the
具体的に説明すると、ダイ10は押出装置1の前面に取付けられている。該押出装置1としては、例えばプランジャー式押出装置、スクリュー式押出装置等が挙げられる。該押出装置1は、単軸(1軸)または2軸のいずれであってもよい。押出孔11後方の押出装置1内部には、流路2が形成されている。成形材料は、押出装置1により流路2を通って圧送され、一定流量で押出孔11から押出される。
More specifically, the die 10 is attached to the front surface of the
押出孔11は、流路2側から順に、縮径部12と直管部15とを有している。縮径部12は、流路2と同じ内径の一端12aと、直管部15と同じ内径の他端12bとを有し、流路2から直管部15に向かって縮径されている。直管部15は、押出孔11の先端に設けられており、該直管部15から成形材料が円柱状に押出される。
The
ここで、本実施形態では、この直管部15の内径Dと長さLとの比(D/L)が、2〜6である。このように、内径Dが長さLより大きく、かつそれらの比(D/L)が特定範囲になるよう構成された直管部15から成形材料を押出すことによって、成形体内の補強用繊維の向きが押出方向に配向されるのを抑制することができる。
Here, in this embodiment, the ratio (D / L) between the inner diameter D and the length L of the
長さLとしては3mm以下、好ましくは0.5〜3mmであるのがよく、この長さLとの比(D/L)が2〜6になるよう内径Dを決定するのが好ましい。なお、内径Dおよび長さLは、その比(D/L)が前記した特定範囲を有する限り、成形体の形状に応じて任意の値を選定することができ、前記で例示した値に限定されるものではない。 The length L is 3 mm or less, preferably 0.5 to 3 mm. The inner diameter D is preferably determined so that the ratio (D / L) to the length L is 2 to 6. In addition, as long as the ratio (D / L) has the specific range described above, the inner diameter D and the length L can be selected according to the shape of the molded body, and are limited to the values exemplified above. Is not to be done.
一方、前記比(D/L)が2より小さいと、成形体内の補強用繊維の向きが押出方向に配向されやすくなり、6より大きいと、直管部としての機能が得られにくくなり、成形体に曲がりや反りが発生しやすくなる。 On the other hand, when the ratio (D / L) is smaller than 2, the direction of the reinforcing fiber in the molded body is easily oriented in the extrusion direction, and when larger than 6, the function as the straight pipe portion is difficult to be obtained. The body is likely to bend and warp.
このような押出成形装置20を用いて押出成形体を得るには、まず、前記した成形材料を押出装置1に供給して混練しつつ、流路2内を圧送させて、一定流量で押出孔11から円柱状に押出す。
In order to obtain an extrusion-molded body using such an
このとき、成形材料は、内径Dと長さLとの比(D/L)が特定範囲になるよう構成された直管部15から押出されるので、成形体内の補強用繊維の向きが押出方向に配向され難い。したがって、押出方向の強度が弱くなるのを抑制することができ、機械的強度が向上した割れ難い成形体を得ることができる。
At this time, since the molding material is extruded from the
押出速度としては、特に限定されないが、10〜50mm/秒程度が適当である。また、成形材料を押出すときの温度(押出温度)としては、20〜25℃が適当である。 Although it does not specifically limit as an extrusion speed, About 10-50 mm / sec is suitable. Moreover, 20-25 degreeC is suitable as temperature (extrusion temperature) when extruding a molding material.
押出孔11から押出された成形体は、ダイ10の前面に設けた図示しない切断装置にて所定長さに切断され、これにより本発明の成形体が得られる。なお、成形体の長さとしては、2〜20mm程度が適当である。
The molded body extruded from the
本発明における成形体の具体例としては、例えば触媒、触媒担体、吸着材、乾燥材、調湿材等が挙げられる。また、成形体の材料は無機材料に限定されるものではなく、種々のプラスチック材料等に対しても本発明は適用可能である。 Specific examples of the molded body in the present invention include a catalyst, a catalyst carrier, an adsorbent, a desiccant, a humidity control material, and the like. Further, the material of the molded body is not limited to the inorganic material, and the present invention can be applied to various plastic materials.
なお、前記した実施形態では、押出孔の構成として、直管部と縮径部とを有する構成について説明したが、本発明はこれに限定されるものではない。すなわち、本発明にかかる押出孔は、直管部のみで構成されていてもよい。 In the above-described embodiment, the configuration having the straight pipe portion and the reduced diameter portion has been described as the configuration of the extrusion hole, but the present invention is not limited to this. That is, the extrusion hole concerning this invention may be comprised only by the straight pipe part.
また、前記した実施形態では、円柱状の成形体を得る場合について説明したが、例えば押出孔内にピンを挿入すれば、円筒形の成形体を得ることができる。すなわち、押出孔の直管部内に、該直管部の内径より小さい外径を有するピンを挿入する。このピンの先端を、ダイの前面と同じ位置か、または外方に位置するよう調整する。これにより、成形材料を押出孔から円筒状に押出して、円筒形の成形体を得ることができる。 In the above-described embodiment, the case of obtaining a columnar shaped body has been described. However, for example, if a pin is inserted into the extrusion hole, a cylindrical shaped body can be obtained. That is, a pin having an outer diameter smaller than the inner diameter of the straight pipe portion is inserted into the straight pipe portion of the extrusion hole. Adjust the tip of this pin to be in the same position as the front of the die or outward. Thereby, a molding material can be extruded cylindrically from an extrusion hole, and a cylindrical molded object can be obtained.
以下、実施例を挙げて本発明を詳細に説明するが、本発明は以下の実施例のみに限定されるものではない。 EXAMPLES Hereinafter, although an Example is given and this invention is demonstrated in detail, this invention is not limited only to a following example.
[実施例1〜3および比較例1,2]
<押出成形体の製造>
まず、成形材料を以下のようにして調製した。すなわち、原料粉末は、リン、モリブテン、バナジウム、アンチモン、銅およびセシウムから選ばれる元素をそれぞれ1.5、12、0.5、0.5、0.3および1.4の原子比で含むヘテロポリ酸を用いた。補強用繊維は、平均繊維長0.1mm、平均繊維径2μmのアルミナ繊維を用いた。
[Examples 1 to 3 and Comparative Examples 1 and 2]
<Manufacture of extrusion molding>
First, a molding material was prepared as follows. That is, the raw material powder is a heteropolyethylene containing an element selected from phosphorus, molybdenum, vanadium, antimony, copper and cesium in an atomic ratio of 1.5, 12, 0.5, 0.5, 0.3 and 1.4, respectively. Acid was used. As the reinforcing fibers, alumina fibers having an average fiber length of 0.1 mm and an average fiber diameter of 2 μm were used.
前記アルミナ繊維を、該アルミナ繊維の割合が原料粉末(乾燥重量)100重量部に対して表1に示す割合となるよう前記原料粉末に添加し、触媒粉末を得た。そして、純水に硝酸アンモニウム(バインダー成分)を溶解させた水溶液を、純水および硝酸アンモニウムの各割合が触媒粉末100重量部に対して表1に示す割合となるよう前記原料粉末に添加し、混合して成形材料を得た。 The alumina fiber was added to the raw material powder so that the ratio of the alumina fiber was as shown in Table 1 with respect to 100 parts by weight of the raw material powder (dry weight) to obtain a catalyst powder. Then, an aqueous solution in which ammonium nitrate (binder component) is dissolved in pure water is added to and mixed with the raw material powder so that each ratio of pure water and ammonium nitrate is the ratio shown in Table 1 with respect to 100 parts by weight of the catalyst powder. A molding material was obtained.
次に、得られた成形材料を、ダイの押出孔から連続的に押出して押出成形体を製造した。用いた押出成形装置の構成は、以下の通りである。
押出装置:単軸(1軸)スクリュー式押出装置を用いた。
ダイ:押出装置の流路側から順に、縮径部および直管部を有する押出孔が形成されたものを用いた。直管部における内径D、長さL、および比(D/L)は、表1に示す通りである。
Next, the obtained molding material was continuously extruded from the extrusion hole of the die to produce an extrusion molded body. The configuration of the extrusion molding apparatus used is as follows.
Extruder: A single screw (single screw) screw type extruder was used.
Die: A die in which an extrusion hole having a reduced diameter portion and a straight pipe portion was formed in order from the flow path side of the extrusion apparatus was used. Table 1 shows the inner diameter D, the length L, and the ratio (D / L) in the straight pipe portion.
成形材料を押出装置に供給して混練しつつ圧送し、押出孔から直径5.4mmの円柱状に押出し、長さ6.2mmで切断して、表1中の実施例1〜3および比較例1,2にかかる押出成形体を得た。なお、各押出成形体において、押出速度は、いずれも31mm/秒、押出温度は、いずれも25℃に設定した。また、押出成形体の切断は、押出孔の前面を一定速度でピアノ線を横切らせることによって行った。
The molding material was supplied to an extrusion apparatus and pumped while kneaded, extruded into a cylindrical shape having a diameter of 5.4 mm from the extrusion hole, cut to a length of 6.2 mm, and Examples 1 to 3 in Table 1 and Comparative
得られた各押出成形体を、恒温恒湿槽(90℃、30%Rh)にて3時間予備乾燥した後、空気気流中226℃で10時間、空気気流中250℃で1時間の順に熱処理した。続いて、窒素気流中で435℃に昇温して、同温度にて4時間保持した。その後、空気気流中で70℃まで冷却してから取り出した。冷却後の各押出成形体を目視観察した。その結果、いずれの押出成形体においても、曲がりや反りの発生は見られなかった。 Each obtained extrusion-molded body was pre-dried in a constant temperature and humidity chamber (90 ° C., 30% Rh) for 3 hours, then heat treated in the order of 10 hours at 226 ° C. in an air stream and 1 hour at 250 ° C. in an air stream. did. Then, it heated up to 435 degreeC in nitrogen stream, and hold | maintained at the same temperature for 4 hours. Then, after cooling to 70 degreeC in an airflow, it took out. Each extrudate after cooling was visually observed. As a result, no bending or warping was observed in any of the extruded products.
<評価>
得られた各押出成形体について、耐圧強度試験および落下強度試験を行った。各試験方法を以下に示すと共に、その結果を表1に示す。
<Evaluation>
About each obtained extrusion-molded body, the compressive strength test and the drop strength test were done. Each test method is shown below, and the results are shown in Table 1.
(耐圧強度試験)
押出成形体に対し、押出方向に直交する方向(径方向)に圧力を加えていき、成形体が割れた圧力を測定し、これを径方向の耐圧強度とした。同様に、押出成形体に対し、押出方向(軸方向)に圧力を加えていき、成形体が割れた圧力を測定し、これを軸方向の耐圧強度とした。
(Pressure strength test)
A pressure was applied to the extruded product in a direction perpendicular to the extrusion direction (radial direction), and the pressure at which the molded product was cracked was measured, and this was defined as the pressure resistance in the radial direction. Similarly, pressure was applied to the extruded product in the extrusion direction (axial direction), the pressure at which the molded product was cracked was measured, and this was defined as the axial pressure strength.
(落下強度試験)
押出成形体を、垂直に立てられ下端に高さ30mmのシリコーンゴム製の栓をした内径25.4mm、長さ5mの鉄パイプ中を上端から落下させた。このときの成形体の粉化率を測定した。すなわち、落下した成形体を篩にかけ、粉砕品、半割れ品および良品に篩別し、良品の割合にて評価した。
(Drop strength test)
The extruded product was dropped from an upper end in an iron pipe having an inner diameter of 25.4 mm and a length of 5 m, which was vertically placed and was plugged with a silicone rubber plug having a height of 30 mm at the lower end. The powdering rate of the molded body at this time was measured. That is, the dropped molded body was sieved and classified into a pulverized product, a half-cracked product, and a non-defective product, and evaluated based on the proportion of non-defective products.
粉砕品、半割れ品および良品の割合は、以下の基準にて評価した。
粉砕品:8メッシュ下(−8#)[8メッシュの篩(目開き2.36mm)を通過したものの割合(質量%)]
半割品:8メッシュ上4メッシュ下(+8#〜+4#)[4メッシュの篩(目開き4.75mm)を通過し、8メッシュ篩(目開き2.36mm)を通過しないものの割合(質量%)]
良品:4メッシュ上(+4#)[4メッシュの篩(目開き4.75mm)を通過しないものの割合(質量%)]
The ratio of the pulverized product, the half-broken product, and the non-defective product was evaluated according to the following criteria.
Pulverized product: Under 8 mesh (−8 #) [Percentage (mass%) of having passed through 8-mesh sieve (aperture 2.36 mm)]
Half-cut product: 8 mesh upper 4 mesh lower (+ 8 # to + 4 #) [ratio of mass that passes through a 4-mesh sieve (mesh 4.75 mm) and does not pass an 8-mesh sieve (mesh 2.36 mm) (mass %)]
Non-defective product: on 4 mesh (+ 4 #) [ratio of mass not passing through 4-mesh sieve (aperture 4.75 mm) (mass%)]
表1から明らかなように、耐圧強度試験において、実施例1〜3の成形体は、比較例1,2の成形体よりも軸方向(押出方向)の強度が高いのがわかる。また、落下強度試験において、実施例1〜3の成形体は、比較例1,2の成形体よりも優れた結果を示しているのがわかる。これらの結果から、本発明によれば、成形体内の補強用繊維の向きがランダムに分散されて、押出方向の強度が弱くなるのを抑制することができ、機械的強度が向上した割れ難い成形体を得ることができると言える。 As is apparent from Table 1, in the pressure resistance test, it can be seen that the molded bodies of Examples 1 to 3 have higher strength in the axial direction (extrusion direction) than the molded bodies of Comparative Examples 1 and 2. Moreover, in the drop strength test, it turns out that the molded object of Examples 1-3 has shown the result superior to the molded object of Comparative Examples 1 and 2. FIG. From these results, according to the present invention, the direction of the reinforcing fibers in the molded body is randomly dispersed, and the strength in the extrusion direction can be suppressed from being weakened, and the mechanical strength is improved. It can be said that the body can be obtained.
1 押出装置
2 流路
10 ダイ
11 押出孔
12 縮径部
15 直管部
20 押出成形装置
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US20210078929A1 (en) * | 2018-01-02 | 2021-03-18 | Shanghai Huayi New Material Co., Ltd. | (Meth)acrolein Oxidation Catalyst and Preparation Method Thereof |
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JPH07276332A (en) * | 1994-04-11 | 1995-10-24 | Sekisui Chem Co Ltd | Manufacture of hydraulic inorganic cured product |
JP2000313008A (en) * | 1999-04-30 | 2000-11-14 | Sumitomo Chem Co Ltd | Die for extrusion molding, extrusion molding apparatus using the die, and production of molded body |
JP2003010690A (en) * | 2001-06-28 | 2003-01-14 | Sumitomo Chem Co Ltd | Catalyst for manufacturing methacrylic acid, method for manufacturing the same, and method for manufacturing methacrylic acid |
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JPH0216005A (en) * | 1988-07-04 | 1990-01-19 | Sekisui Chem Co Ltd | Manufacture of fiber reinforced inorganic plate |
JPH07276332A (en) * | 1994-04-11 | 1995-10-24 | Sekisui Chem Co Ltd | Manufacture of hydraulic inorganic cured product |
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