WO2008123566A1 - 炭酸基含有水酸化マグネシウム粒子およびその製造方法 - Google Patents
炭酸基含有水酸化マグネシウム粒子およびその製造方法 Download PDFInfo
- Publication number
- WO2008123566A1 WO2008123566A1 PCT/JP2008/056630 JP2008056630W WO2008123566A1 WO 2008123566 A1 WO2008123566 A1 WO 2008123566A1 JP 2008056630 W JP2008056630 W JP 2008056630W WO 2008123566 A1 WO2008123566 A1 WO 2008123566A1
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- WIPO (PCT)
- Prior art keywords
- magnesium hydroxide
- magnesium
- ions
- surface area
- specific surface
- Prior art date
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Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F5/00—Compounds of magnesium
- C01F5/14—Magnesium hydroxide
- C01F5/22—Magnesium hydroxide from magnesium compounds with alkali hydroxides or alkaline- earth oxides or hydroxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F5/00—Compounds of magnesium
- C01F5/14—Magnesium hydroxide
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F5/00—Compounds of magnesium
- C01F5/02—Magnesia
- C01F5/06—Magnesia by thermal decomposition of magnesium compounds
- C01F5/08—Magnesia by thermal decomposition of magnesium compounds by calcining magnesium hydroxide
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F5/00—Compounds of magnesium
- C01F5/24—Magnesium carbonates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/88—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by thermal analysis data, e.g. TGA, DTA, DSC
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
Definitions
- the present invention C_ ⁇ 3 magnesium hydroxide synthesized BET specific surface area is greater in the presence of ion particles, and a method for producing the same.
- Magnesium hydroxide particles have been known for a long time, pharmaceutical, industrial and agricultural documents
- antacids and laxatives are used for pharmaceuticals, and are used as flame retardants, flue gas desulfurization agents, wastewater neutralizers, ceramic raw materials, and sintering aids for industrial use. In agriculture, it is used as a bitter soil fertilizer to neutralize acidic soil and supplement minerals.
- a typical method for producing magnesium hydroxide particles is a seawater method in which seawater reacts with slaked lime.
- the seawater because it contains C 0 3 ions of approximately 0. Lg / L in C 0 2 conversion, the C a C_ ⁇ 3 Adding without pretreatment slaked lime mixed as produced impurities. Therefore, seawater is usually used for the reaction after decarboxylation.
- Other methods include reacting with Mg source as bitter and caustic soda as alkali source, hydrating MgO, and reacting magnesium salt with ammonia to crystallize magnesium hydroxide crystals. .
- the C a C 0 3 or M g C_ ⁇ 3 CO 3 ions to generate impurities such as disliked, tended to be excluded only from the reaction system possible.
- Magnesium carbonate is a soda ash method in which a magnesium salt solution and sodium carbonate are reacted, a carbon dioxide method in which a magnesium salt solution and ammonium carbonate solution are reacted, and a carbon dioxide method in which carbon dioxide gas is allowed to act on magnesium hydroxide. It is manufactured by.
- Patent Document 1 magnesium hydroxide particles and amorphous caustic acid are heated in an aqueous medium to form magnesium kainate on the surface of the magnesium hydroxide particles to produce magnesium hydroxide particles having a large specific surface area.
- a method is disclosed.
- the specific surface area of the magnesium hydroxide particles obtained by this production method is large because of the non-reactive amorphous kaic acid that appears to remain partially unreacted with the magnesium silicate formed only on the surface. Presumably due to the influence of both, it is difficult to say that the specific surface area of magnesium hydroxide particles has increased.
- Patent Document 1 Japanese Patent Laid-Open No. 2003-40616 Disclosure of Invention
- magnesium hydroxide particles having a large BET method specific surface area can obtain magnesium hydroxide particles having a large BET method specific surface area by adding divalent anions that inhibit crystal growth of magnesium hydroxide particles. I had the idea that it might be. Based on this idea, when magnesium salt solution and an alkaline substance were reacted in the presence of C0 3 ions, it was found that magnesium hydroxide particles having a BET specific surface area larger than before were obtained. Completed the invention.
- x and m satisfy the following conditions.
- grains represented by these is provided.
- a fired product obtained by firing the magnesium hydroxide particles at 400 ° C. or higher.
- FIG. 1 is an X-ray diffraction image of the magnesium hydroxide particles obtained in Example 6.
- FIG. 2 is an X-ray diffraction image of the magnesium hydroxide particles obtained in Comparative Example 1.
- FIG. 3 is an X-ray diffraction image of the basic magnesium carbonate particles obtained in Comparative Example 4.
- FIG. 4 is a differential thermal analysis curve (DTA) of the magnesium hydroxide particles obtained in Example 6.
- FIG. 5 is a differential thermal analysis curve (DTA) of the magnesium hydroxide particles obtained in Comparative Example 3.
- FIG. 6 is a differential thermal analysis curve (DTA) of the basic magnesium carbonate particles obtained in Comparative Example 4.
- DTA differential thermal analysis curve
- the magnesium hydroxide particles of the present invention have the following formula (1)
- composition represented by these.
- 0.02 ⁇ x ⁇ 0.7 is satisfied.
- X preferably satisfies 0.04 ⁇ 0.6, more preferably 0.006 ⁇ x ⁇ 0.3.
- m satisfies 0 ⁇ m ⁇ l. m preferably satisfies 0 ⁇ m ⁇ 0.5.
- the BET specific surface area of the magnesium hydroxide particles of the present invention is 80 to 40 OmV g.
- the lower limit of the BET specific surface area of the magnesium hydroxide particles of the present invention is 8 Om 2 Zg, preferably 10 Om 2 Zg, more preferably 12 Om 2 Zg.
- the upper limit of the BET specific surface area is 400 m 2 / g, preferably 350 m 2 / g, and more preferably 300 m 2 / g.
- the BET specific surface area of the magnesium hydroxide particles of the present invention is preferably 80 to 350 m 2 Zg.
- the magnesium hydroxide particle of the present invention contains about 0.75 to 23 wt% of C0 3 ion in terms of CO 2 in the particle, but is characteristic of magnesium hydroxide in X-ray diffraction images and differential thermal analysis (DTA). And the BET specific surface area is 80 to 40 Om 2 Zg. C ⁇ The higher the content of 3 ions, the more hindered the crystal growth of magnesium hydroxide particles and the higher the BET specific surface area of the resulting magnesium hydroxide particles.
- the present invention includes a fired product obtained by firing the magnesium hydroxide particles at 400 ° C. or higher.
- Magnesium hydroxide particles of the present invention have a decomposition temperature slightly lower than that of conventional magnesium hydroxide particles, so that magnesium oxide can be obtained at 370 or higher.
- the firing temperature is 400 ° C or higher. I like it.
- Magnesium hydroxide particles of the present invention in the presence of C0 3 ions, and Mg ions It can be produced by contacting OH ions with water.
- Mg ions are preferably used in the form of an aqueous solution of magnesium salt.
- Magnesium salts include magnesium chloride (including bitter juice from which Ca has been removed), magnesium sulfate, magnesium nitrate, magnesium acetate, and the like.
- the magnesium salt aqueous solution preferably contains no Ca ions as much as possible.
- C a ions present in the reaction system since yield a C a C_ ⁇ 3 reacts with C 0 3 ions added for the purpose of crystal growth inhibition hydroxide ⁇ magnesium particle.
- O ions are preferably used in the form of an aqueous solution of alkali metal hydroxide, ammonium hydroxide or the like.
- alkali metal hydroxide caustic soda is preferable.
- C_ ⁇ 3 ions in the production method of the present invention carbonates aqueous solutions, such as alkali metal carbonates and ammonium Niumu, or can be supplied from the form of co 2 gas, controlling the existence ratio of OH ions and CO 3 ions In order to do so, it is preferable to use a carbonate solution.
- the abundance ratio upon reaction with ⁇ _H ions C_ ⁇ 3 ion is the main point. Because since the chemical composition of the water the magnesium oxide particles of the present invention is determined by the existence ratio of ⁇ _H ions C_ ⁇ 3 ions. When there are a lot of CO 3 ions, magnesium carbonate is naturally generated, and its presence is confirmed by X-ray diffraction images and differential thermal analysis (DTA), and the specific surface area of the generated magnesium hydroxide particles is reduced.
- DTA differential thermal analysis
- C ⁇ 3 ions are incorporated together with OH ions when the magnesium hydroxide particles are formed, thereby inhibiting the crystal growth of the magnesium hydroxide particles. Therefore, CO 3 ions are added after the magnesium hydroxide particles are formed.
- magnesium hydroxide particles having a high BET specific surface area as in the present invention cannot be obtained. Therefore, it is important to provide a stable supply of H ions and CO 3 ions at a certain ratio. ⁇ It is preferable to prepare a mixed solution of 3 ions and use it for the reaction.
- the mixed solution of OH ions C_ ⁇ 3 ions such as mixed aqueous solution of mixed aqueous solution and ammonia and carbon Anmoniumu between caustic soda and carbonated soda and the like, sodium hydroxide and carbonic acid in terms of yield of the magnesium hydroxide particles A mixed aqueous solution with soda is preferred.
- the magnesium hydroxide particles of the present invention can be obtained by continuously and continuously adding OH ions and CO 2 gas to a magnesium salt aqueous solution with stirring.
- reaction temperature is preferably 0 to 100 ° C, more preferably 10 to 80. (Reaction time) F
- reaction time is preferably within 120 minutes, more preferably within 60 minutes.
- Magnesium hydroxide particles of the present invention are, for example, an aqueous solution of a magnesium salt (Mg I on), and a mixed aqueous solution of caustic soda (OH ion) and sodium carbonate (C_ ⁇ 3 ions), continuously feeding to a reaction vessel,
- the product can be continuously extracted from the reaction tank by a continuous stirring tank anti-J heart (c on ti nu nu sstirred tank reaction).
- the residence time in this reaction is preferably within 120 minutes, more preferably within 60 minutes.
- the aqueous solution of the magnesium salt in the reaction vessel can be prepared by a batch reaction adding a mixed aqueous solution of caustic soda ( ⁇ H ion) and sodium carbonate (C0 3 ions).
- magnesium hydroxide particles obtained by the reaction contain C 1 ions and S0 4 ions as impurities. May be.
- the content of C 1 ions is preferably 0.5 wt% or less and 0.3 wt% or less.
- the content of S O 4 ions is preferably 2 wt% or less and 1.5 wt% or less. If it is better to reduce these impurities depending on the use of magnesium hydroxide particles, these impurities can be halved by further washing the magnesium hydroxide particles obtained by the reaction with an emulsified or alkaline solution. The following can be eliminated and reduced.
- a caustic soda diluted aqueous solution or a sodium carbonate diluted aqueous solution is preferable.
- Power that can reduce impurities even by heat treatment Heating and aging reduces the specific surface area power that characterizes the present invention.
- the magnesium hydroxide particles of the present invention have extremely excellent filterability despite a large BET specific surface area. It is estimated that for the synthesized cohesive secondary particle size compared to the conventional magnesium hydroxide particles without adding a C_ ⁇ 3 ions are larger summer, performed quickly and easily dehydrated and cleaning of reaction slurry be able to. (Filtration, dehydration, drying, powdered rice cake)
- the slurry product obtained by the reaction is preferably filtered, washed with water or an aqueous alkali diluted solution, and dried. Drying can be performed by shelf hot air drying, spray drying, or the like. In this case, drying is preferably performed at 80 to 250 ° C. in order to remove water. It is also possible to vacuum dry without replacing the moisture with an organic solvent. Since shelf-type hot-air dried products and vacuum-dried products are lumps, it is preferable to grind them into powders according to the purpose of use.
- Example 1 Example 1
- Reaction slurry of Example 1 1. Filter 30 L, wash with 1 L of water, and then continue to pass 0.02 mo 1ZL of sodium carbonate dilute aqueous solution 2 L, then add 1 L of water. After washing with water, it was dewatered and dried at 105 with a shelf dryer for 16 hours. The dried product was pulverized in a mortar and passed through a wire mesh with an opening of 150 m to obtain 97 g of a white powder having a BET specific surface area of 90 m 2 Zg.
- Reaction slurry of Example 5 1. Filter 80 L, wash with 1 L of water, and then continue to pass 0.04 mo 1 ZL of dilute aqueous solution of 1 L of caustic soda into 1 L of water. After washing with water, it was dewatered and dried at 105 ° C for 16 hours in a shelf dryer. The dried product was pulverized in a mortar and passed through a wire mesh with a mesh opening of 150 to obtain 96 g of a white powder having a BET specific surface area of 177 m 2 / g.
- Example 7 (alkali cleaning) Reaction slurry of Example 5 1.
- Filter 80 L wash with 1 L of water, and then continue to pass 0.02 mo 1 / L of sodium carbonate diluted aqueous solution 2 L, and further into 1 L of water. After washing with water, it was dewatered and dried at 105 ° C for 16 hours in a shelf dryer.
- the dried product was pulverized in a mortar, and passed through a wire mesh having an opening of 150 m to obtain 98 g of white powder having a specific surface area of 197 m 2 Zg.
- Example 8 The reaction slurry of Example 8 was filtered, and 0 L was filtered and washed with 0.5 L of water, followed by 0.04 mo 1 ZL of aqueous sodium hydroxide solution diluted with 1 L, and further, 0. The water was washed with 5 L of water, dehydrated, and dried at 105 ° C for 16 hours with a shelf dryer. The dried product was pulverized in a mortar and passed through a wire mesh with an opening of 150 m to obtain 46 g of a white powder having a BET specific surface area of 2 16 m 2 / g.
- Example 11 (alkali cleaning) 4. React slurry of Example 10 4. Filter 65 L, wash with 1 L of water, and then pass 0.02 mo 1 ZL of dilute aqueous sodium carbonate solution with 2 L. The water was washed with 1 L of water, dehydrated, and dried at 105 ° C for 16 hours with a shelf dryer. The dried product was ground in a mortar, passed through a wire mesh of mesh opening 0.99 m, to obtain a BET specific surface area of 249 ⁇ 2 / ⁇ white powder 100 g of.
- Magnesium hydroxide having a BET specific surface area of 249 m 2 Zg in Example 11 was calcined at 400 ° C. for 2 hours.
- Magnesium hydroxide having a BET specific surface area of 177 m 2 / g in Example 6 was calcined at 750 ° C. for 2 hours.
- Magnesium hydroxide having a BET specific surface area of 37 m 2 / g in Comparative Example 2 was calcined at 400 ° C. for 2 hours.
- the magnesium hydroxide of Comparative Example 3 having a BET specific surface area of 58 m 2 Z g was calcined at 400 ° C. for 2 hours.
- Magnesium hydroxide having a BET specific surface area of 58 m 2 Zg in Comparative Example 3 was calcined at 750 ° C. for 2 hours.
- Example;! -14 and Comparative Examples 1 to 8 were analyzed by the following method.
- Table 1 shows the composition analysis and BET specific surface area measurement results
- Fig. 1 to 3 show the structural analysis using an X-ray diffractometer
- the magnesium hydroxide particles of the present invention have a large BET method specific surface area. According to the production method of the present invention, magnesium hydroxide particles having a large BET method specific surface area can be produced.
- the acid magnesium (baked product) obtained by firing the magnesium hydroxide particles of the present invention has a high BET method specific surface area.
- the magnesium hydroxide particles of the present invention have a very high BET specific surface area compared to conventional magnesium hydroxide basic magnesium carbonate. for that reason In addition to adsorbents and neutralizers, it can be used in a wide variety of applications, including various fillers, ceramic materials, food additives, and antacids. Also wash with a dilute aqueous solution.
- Magnesium oxide obtained by firing the magnesium hydroxide particles of the present invention with reduced C 1 has a higher BET specific surface area than magnesium oxide obtained by firing conventional magnesium hydroxide. A wide range of uses can be expected.
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- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
Description
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Priority Applications (5)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
KR1020097015942A KR101354837B1 (ko) | 2007-04-02 | 2008-03-27 | 탄산기 함유 수산화마그네슘 입자 및 그 제조 방법 |
EP08739740.2A EP2135845A4 (en) | 2007-04-02 | 2008-03-27 | PARTICLES FROM CARBON GROUP-BASED MAGNESIUM HYDROXIDE AND MANUFACTURING METHOD THEREFOR |
US12/450,610 US9346683B2 (en) | 2007-04-02 | 2008-03-27 | Carbonate radical-containing magnesium hydroxide particle and manufacturing method thereof |
JP2009509287A JP5202514B2 (ja) | 2007-04-02 | 2008-03-27 | 炭酸基含有水酸化マグネシウム粒子およびその製造方法 |
CN200880010937XA CN101652323B (zh) | 2007-04-02 | 2008-03-27 | 含碳酸基的氢氧化镁颗粒及其制备方法 |
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JP2007096013 | 2007-04-02 | ||
JP2007-096013 | 2007-04-02 |
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WO2008123566A1 true WO2008123566A1 (ja) | 2008-10-16 |
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PCT/JP2008/056630 WO2008123566A1 (ja) | 2007-04-02 | 2008-03-27 | 炭酸基含有水酸化マグネシウム粒子およびその製造方法 |
Country Status (7)
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US (1) | US9346683B2 (ja) |
EP (1) | EP2135845A4 (ja) |
JP (1) | JP5202514B2 (ja) |
KR (1) | KR101354837B1 (ja) |
CN (1) | CN101652323B (ja) |
TW (1) | TWI402216B (ja) |
WO (1) | WO2008123566A1 (ja) |
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2011158675A1 (ja) * | 2010-06-15 | 2011-12-22 | 協和化学工業株式会社 | 複合水酸化マグネシウム、その製造方法および吸着剤 |
JP2012020885A (ja) * | 2010-07-12 | 2012-02-02 | Kyowa Chem Ind Co Ltd | 増粘剤 |
WO2012050144A1 (ja) | 2010-10-13 | 2012-04-19 | 協和化学工業株式会社 | 食用油用脱酸剤およびそれを用いた使用済み食用油の再生方法 |
WO2012124827A1 (ja) | 2011-03-17 | 2012-09-20 | 協和化学工業株式会社 | 錠剤成形用結合剤 |
JP2015124318A (ja) * | 2013-12-26 | 2015-07-06 | 東ソー株式会社 | クロロスルホン化ポリオレフィン組成物 |
Families Citing this family (3)
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CN106573197B (zh) * | 2014-04-10 | 2019-08-23 | 剑桥碳捕集有限公司 | 活化硅酸盐矿物质的方法和体系 |
KR101885843B1 (ko) | 2016-09-12 | 2018-08-06 | 주식회사 단석산업 | 합성 하이드로마그네사이트 입자 및 그의 제조방법 |
CN115491477B (zh) * | 2021-06-18 | 2024-01-12 | 协和化学工业株式会社 | 退火隔离剂的制备方法以及退火隔离剂和方向性电磁钢板 |
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2008
- 2008-03-27 CN CN200880010937XA patent/CN101652323B/zh not_active Expired - Fee Related
- 2008-03-27 US US12/450,610 patent/US9346683B2/en not_active Expired - Fee Related
- 2008-03-27 EP EP08739740.2A patent/EP2135845A4/en not_active Withdrawn
- 2008-03-27 JP JP2009509287A patent/JP5202514B2/ja active Active
- 2008-03-27 WO PCT/JP2008/056630 patent/WO2008123566A1/ja active Application Filing
- 2008-03-27 KR KR1020097015942A patent/KR101354837B1/ko not_active IP Right Cessation
- 2008-04-01 TW TW097111841A patent/TWI402216B/zh not_active IP Right Cessation
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Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2011158675A1 (ja) * | 2010-06-15 | 2011-12-22 | 協和化学工業株式会社 | 複合水酸化マグネシウム、その製造方法および吸着剤 |
CN102892710A (zh) * | 2010-06-15 | 2013-01-23 | 协和化学工业株式会社 | 复合氢氧化镁、其制造方法及吸附剂 |
JP5656298B2 (ja) * | 2010-06-15 | 2015-01-21 | 協和化学工業株式会社 | 複合水酸化マグネシウム、その製造方法および吸着剤 |
JP2012020885A (ja) * | 2010-07-12 | 2012-02-02 | Kyowa Chem Ind Co Ltd | 増粘剤 |
WO2012050144A1 (ja) | 2010-10-13 | 2012-04-19 | 協和化学工業株式会社 | 食用油用脱酸剤およびそれを用いた使用済み食用油の再生方法 |
WO2012124827A1 (ja) | 2011-03-17 | 2012-09-20 | 協和化学工業株式会社 | 錠剤成形用結合剤 |
JP5835849B2 (ja) * | 2011-03-17 | 2015-12-24 | 協和化学工業株式会社 | 圧縮成形物およびその製造方法 |
JP2015124318A (ja) * | 2013-12-26 | 2015-07-06 | 東ソー株式会社 | クロロスルホン化ポリオレフィン組成物 |
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JP5202514B2 (ja) | 2013-06-05 |
US9346683B2 (en) | 2016-05-24 |
EP2135845A1 (en) | 2009-12-23 |
TWI402216B (zh) | 2013-07-21 |
JPWO2008123566A1 (ja) | 2010-07-15 |
KR101354837B1 (ko) | 2014-01-22 |
US20100098781A1 (en) | 2010-04-22 |
CN101652323A (zh) | 2010-02-17 |
CN101652323B (zh) | 2011-09-07 |
TW200904757A (en) | 2009-02-01 |
KR20100014349A (ko) | 2010-02-10 |
EP2135845A4 (en) | 2014-05-14 |
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