JPS58166926A - Method for granulating inorganic powder - Google Patents

Method for granulating inorganic powder

Info

Publication number
JPS58166926A
JPS58166926A JP57050459A JP5045982A JPS58166926A JP S58166926 A JPS58166926 A JP S58166926A JP 57050459 A JP57050459 A JP 57050459A JP 5045982 A JP5045982 A JP 5045982A JP S58166926 A JPS58166926 A JP S58166926A
Authority
JP
Japan
Prior art keywords
water
solvent
slurry
compatible
materials
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
JP57050459A
Other languages
Japanese (ja)
Other versions
JPS6329579B2 (en
Inventor
Migiwa Ando
安藤 汀
Yukiaki Ito
伊藤 幸昭
Kiyoshige Ochiai
落合 清成
Takashi Kato
隆史 加藤
Yukito Nakayama
仲山 幸人
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Nippon Tokushu Togyo KK
Niterra Co Ltd
Original Assignee
NGK Spark Plug Co Ltd
Nippon Tokushu Togyo KK
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by NGK Spark Plug Co Ltd, Nippon Tokushu Togyo KK filed Critical NGK Spark Plug Co Ltd
Priority to JP57050459A priority Critical patent/JPS58166926A/en
Publication of JPS58166926A publication Critical patent/JPS58166926A/en
Publication of JPS6329579B2 publication Critical patent/JPS6329579B2/ja
Granted legal-status Critical Current

Links

Abstract

PURPOSE:To improve the yield of granules and packing density by adding a solvent which differs from water and hardly dissolves water soluble polymer materials to water and making powder of inorg. raw materials and polymer binder materials into a slurry. CONSTITUTION:Polymer materials which are soluble in water or disperse uniformly in water are compounded together with a granular binder into water added with a solvent which is compatible with water and hardly dissolves said polymer materials and the mixture thereof is made into a slurry, whereafter the slurry of the powder of the inorg. raw materials is sprayed, dried and granulated. 3-Methyl 3-methoxy butanol, ethylene glycol, n-butanol, etc. are suitably usable for the above-described solvent which is compatible with water and hardly dissolves said polymer materials. The mixing ratio of said solvent and water is made preferably 30-90% water and 70-10% solvent based on weight.

Description

【発明の詳細な説明】 竜うミックス、サーメットあるいは超硬合金等の焼結体
はそれらのU特性に大きな影曽を与える内部のピンホー
ルを可及的に少なく、かつ倣細なものとする必要がある
ため、素体のプレス成形に使用する無機質の原料粉0体
(以下単に原料粉体という)からなる顆粒の真円度を高
めこれによって充填密度を上ける必要がある。
[Detailed description of the invention] A sintered body of cermet, cemented carbide, etc. should have as few internal pinholes as possible, which greatly affect its U characteristics, and be made as thin as possible. Therefore, it is necessary to increase the roundness of granules made of inorganic raw material powder (hereinafter simply referred to as raw material powder) used for press molding of the element body, thereby increasing the packing density.

上記の^い真円度を有する顆粒を製造するために噴膳乾
燥による造粒が一般に実用されているが、噴霧乾燥を行
なうため原料粉体を泥漿化するに際し、水と共に該原料
粉体を結合して顆粒化する水溶性または水と均一に分散
する一分子材料(以下単に高分子結合剤という)を添加
する必費がお9、この高分子結合剤が噴鱒乾燥の過程に
おいて、高温O乾燥室内に噴出された泥秦滴の周囲を覆
って内部の水蒸気の通過を妨げ、内圧を高めるので該泥
漿滴の異常膨張をもたらし、あるいは顆粒化する前に破
壊させるなどによって歩留シの面において不満があった
Granulation by spray drying is generally used to produce granules with the above-mentioned high roundness, but when turning the raw material powder into a slurry for spray drying, the raw material powder is mixed with water. It is necessary to add a water-soluble or monomolecular material (hereinafter simply referred to as a polymeric binder) that binds and forms granules (hereinafter simply referred to as a polymeric binder). It covers the periphery of the slurry droplets ejected into the drying chamber and prevents the passage of water vapor inside, increasing the internal pressure, causing abnormal expansion of the slurry droplets, or causing them to break before they become granules, thereby reducing the yield rate. There was some dissatisfaction with this aspect.

上記顆粒O異状j1彊、破壊は泥漿−の乾燥速成を小さ
くすることによって若干の改善は見られるが、本質的の
解決は期待できなかった。
Although some improvement in the above-mentioned granule abnormality and destruction was seen by reducing the rapid drying of the slurry, no substantial solution could be expected.

本発明は、原料粉体に水と共に、水溶性または水と均一
に分散するエマルジ日ンタイグの高分子結合剤を加えて
泥漿化するに際し、水と相溶し、かつ上記高分子結合剤
と溶解し難い溶媒を添加することによって上記の不満を
解消し、均一な粒径で真円度の高い顆粒の歩留9を改譬
すると共に、焼結体を緻密化して抗折力によって代表さ
れる機械、的特性を初め、他のM特性を大巾に高めるこ
とに成功し友ものである。
In the present invention, when a water-soluble or uniformly dispersible Emulsion Suntaig polymer binder is added to raw material powder together with water to form a slurry, the present invention is compatible with water and dissolves in the polymer binder. The above-mentioned dissatisfaction is resolved by adding a solvent that is difficult to dissolve, and the yield rate of granules with uniform particle size and high roundness is improved, and the sintered body is densified, as represented by transverse rupture strength. It has succeeded in greatly improving mechanical and mechanical properties as well as other M properties.

本発明において、上記の原料粉体を泥漿化するに際して
水と相浴し、か′)ii116分子結合剤と溶解し難い
溶媒を添加した1由紘、噴霧乾燥工程においてノズルが
ち噴射される原料粉体、高分子結合剤、水、溶媒からな
る泥漿嫡がs吐の熱風によって乾燥する過榔において、
先ず水と上記溶媒の液相よシも水分め多い蒸気を蒸発さ
せ温度上昇に従って上記液相の滴謀議度を高めて泥漿滴
中の高分子結合剤の淡解度を急速に低くして内方へ析出
させ、泥漿滴の乾燥峙において肩書な内圧の上昇を抑え
ようとするもので、図面の気液平衡−−によって説明す
る。
In the present invention, when the above-mentioned raw material powder is turned into a slurry, the raw material powder is mixed with water, and (ii) a 116 molecule binder and a solvent that is difficult to dissolve are added. In the process of drying the slurry consisting of the body, polymeric binder, water, and solvent by hot air,
First, the liquid phase of water and the solvent is evaporated, and as the temperature rises, the degree of droplet concentration of the liquid phase is increased to rapidly lower the solubility of the polymeric binder in the slurry droplets. This is intended to suppress the increase in internal pressure during drying of slurry droplets, and will be explained by referring to the vapor-liquid equilibrium in the drawing.

図面はJメチルJメトキシブタノールを溶媒として水に
溶解し友場合を示し、例えば水を70TLjk’A、溶
媒を70重量−としたP点の沸点は約10/ Cであっ
て、そのときの蒸気中の水分はP′点の約Pコ一となっ
て泥漿滴から蒸発するが同時に蒸発する溶媒成分は約を
−の倣蓋にすぎない。続いて泥漿滴の温度が液相線を越
えて上昇するに従ってm*する溶媒成分を高めるが12
0℃に昇温してもP’点として示されるよう6(c蒸気
中の水分は約77−1溶媒成分は約コJ%に止まり、泥
漿滴から害鳥に蒸発して内部の溶媒の#I直を高め、共
に存在する高分子結合剤を内方へ析出して原料粉体を包
み込んで乾燥を完了する。
The drawing shows the case where J methyl J methoxybutanol is dissolved in water as a solvent. For example, when water is 70 TLjk'A and solvent is 70 wt -, the boiling point at point P is about 10/C, and the vapor at that time is The water inside evaporates from the slurry droplet at about P' point, but the solvent component that evaporates at the same time is just a copy of the point P'. Subsequently, as the temperature of the slurry droplet rises above the liquidus line, the m* solvent component increases, but 12
Even if the temperature is raised to 0°C, the water content in the steam remains at about 77-1 and the solvent component remains at about 77-1%, as indicated by the P' point. The drying process is completed by increasing the directivity and precipitating the coexisting polymer binder inward to envelop the raw material powder.

夾抛例 ア ル ミ す(昭和軽金属人−/J)   P4θV
無 水 珪 #(林純薬/M)       /If訳
緻カルシウム(片山化学1級)     34f酸化マ
グネシウム(来由薬品1級)    コoyを原料粉体
とし、これに可履剤ポリエチレ/オ゛キサイド(M鉄化
学PE0−/ )jf 、沈障防止剤メチルセルp−ズ
(ダウケミカルA−IM)J9.と共に高分子結合剤ポ
リビニルアルコール(デンカB−oj)toy、水6J
OCAQよび溶媒として撰んだJメチルJメトキシブタ
ノール(クラレ、ツルフィツト) 70ctを加え・、
内容積Jtのボールミルによって/を時間の混合、粉砕
を行なって泥漿となし、この泥漿をガス鉦[tto℃、
ディスク径lコ0閤−141−100R,P、h41毎
秒10acの条件で噴霧乾燥を行なって得た本発明によ
る顆粒と、上記S媒の3メチルJメトキシブタノールを
除いて水を700escとし、同一条件で成粒した従来
の方法にょる比軟品の顆粒とを比較した結果を第7表に
示す。
Aluminium (Showa light metal worker-/J) P4θV
Anhydrous silicon # (Hayashi Junyaku/M) /If translated calcium (Katayama Chemical 1st grade) 34F Magnesium oxide (Katayama Chemical 1st grade) Coy is the raw material powder, and the lubricant polyethylene/oxide is added to it. (M Iron Chemical PE0-/)jf, anti-scattering agent Methylcell p-z (Dow Chemical A-IM) J9. Along with polymer binder polyvinyl alcohol (Denka B-oj) toy, water 6J
Add OCAQ and 70ct of J Methyl J Methoxybutanol (Kuraray, Trufit) selected as a solvent.
A ball mill with an internal volume of Jt was used to mix and crush the mixture for a period of time to form a slurry, and the slurry was heated with a gas cylinder [tto℃,
The granules according to the present invention obtained by spray drying under the conditions of 10 ac per second with a disk diameter of l 0 - 141-100 R, P, h41, and the same granules obtained by spray drying at 700 esc of water except for the 3 methyl J methoxybutanol in the S medium. Table 7 shows the results of comparison with soft granules produced by conventional methods.

#i     l     表 但し、歩*bは全乾燥粉末中、目標の≦0〜Jλ!メツ
シュの範囲内にあるものを重量優で示し、充横書度は、
内径10■、深さ11111Mのステンレスの客器に自
然充填させ、充填重量を測定して求め友。
#i l Table However, step*b is the target ≦0~Jλ in all dry powder! Items within the range of metshu are shown in terms of weight and weight, and the full and horizontal writing quality is
A stainless steel vessel with an inner diameter of 10 cm and a depth of 11111 m was filled naturally, and the filled weight was measured.

上衣によって、本発明によって得られた顆粒は従来品に
比して歩留9、充填密度共に高い値を示すことが明らか
にされた。
It was revealed that the granules obtained by the present invention exhibited higher values of both yield 9 and packing density than conventional products.

次に、上記2種の顆粒を用いて/Jx≦0■で厚さtu
の角板の素体をプレスによって製作し。
Next, using the above two types of granules, /Jx≦0■, thickness tu
The square plate element is produced by pressing.

これ・を電気炉の駿化性雰囲気中/!ti′c/時間に
よって焼成して得た焼結体について比較した結果’t#
!−2表に示す。
This is in the hot atmosphere of an electric furnace! The results of comparing sintered bodies obtained by firing at ti'c/time 't#
! - Shown in Table 2.

第      2      表 第−表から、本発明品は成形圧力joo 、 1ooo
 。
From Table 2, the products of the present invention have molding pressures of joo and 1ooo.
.

1zoox、7aaのいずれの場合も素体、焼結晶共に
比較品よりも明らかに尚い密&を示し、抗病力において
は比較品に比して格段と^い麺に7J<L本発明の優れ
た幼果を確かめることができた一本発明における上1の
効果は、1闇で欧明し友通り泥漿粒の乾燥に際して#発
する蒸気の水分を溶媒成分よりも着しく11iliめる
ことe(よって得られるものでめるから、液相よすも気
相の肯で水の#I&度が尚くなるような気敵平倫曲−k
mする溶媒の水浴液がよく、また溶媒も高沸点のものが
好ましく、これらの理由から実施例として示した3メチ
ルJメトキシブタノールの他、エチレングリコールが同
様の効果を奏し、n−ツタノール、酢酸等も満足できる
が、毒性あるいケよ悲臭の点から前者Jメチル3メトキ
シブタノールおよびエチレングリコ−λが好ましい。
In both cases of 1zoox and 7aa, both the base body and the baked crystals clearly showed even higher density than the comparative product, and in terms of anti-disease power, the noodles of the present invention were significantly higher than the comparative product. The first effect of the present invention is that the water content of the steam released during the drying of slurry grains is reduced by 11 ili more than the solvent component. (Thus, since it is determined by what can be obtained, the liquid phase is good, and the gas phase is positive, so the #I & degree of water becomes even higher - k
A water-bath solution of a solvent is preferred, and a solvent with a high boiling point is preferred.For these reasons, in addition to 3-methyl J methoxybutanol shown in the example, ethylene glycol has a similar effect, n-tutanol, acetic acid However, the former J-methyl-3-methoxybutanol and ethylene glyco-λ are preferred from the viewpoint of toxicity and unpleasant odor.

しかして、これら溶媒と水とOa合割合はム電比で水3
0〜り0重量%、溶媒70−103に皿−の範囲内で、
溶媒が下限のto11量−に満たないときは有機質結合
剤が泥漿滴の外周に滲出しまた上限の70優を超えた場
合は、泥漿中の水分が自然的に少なくなって高分子結合
剤の#解kが小さくなシ、所容量の高分子結合剤を完全
蒸解できず、これを補償するため水を増菫すれば泥漿の
til1度が薄くなって噴霧乾燥に困離を生ずるから上
記の範囲内に限定する必要がある。
Therefore, the combined ratio of these solvents, water, and Oa is expressed as water 3
Within the range of 0 to 0% by weight, solvent 70-103,
When the amount of solvent is less than the lower limit of to11, the organic binder oozes out to the outer periphery of the slurry droplets, and when it exceeds the upper limit of 70, the water in the slurry naturally decreases and the polymer binder is absorbed. # If the solution k is small, the required amount of polymeric binder cannot be completely digested, and if water is increased to compensate for this, the til1 degree of the slurry will become thinner, making spray drying difficult. It is necessary to limit it within the range.

【図面の簡単な説明】[Brief explanation of the drawing]

図面は本発明を説明する溶媒の水溶液の気故〒4xI曲
−図である6
The drawing is a diagram showing the structure of an aqueous solution of a solvent to illustrate the present invention.

Claims (1)

【特許請求の範囲】[Claims] (1)  水棲性ま九は水と均一に分散する高分子材料
を粒子結合剤として泥漿化した無機質(DIIIL料験
体を、噴霧乾燥によって造粒するに際して、水と相溶し
、かつ上記高分子材料を溶解し難いill謀を水に加え
て無機質0IIA料看体および為分子の結合材料を泥漿
化することを特徴とし九無機質のIX料粉体の造粒法。 9) 特許請求の範囲第1IK記載の水と相溶し、かつ
上記高分子材料を溶解し難い溶媒が、JメチルJメトキ
シブタノール、エチレングリコール、n−ブタノールま
九は酢酸であ如、かつ該溶媒と水の混合比が重量比で水
J0〜り0−1濤厳70〜10−であることを特徴とし
九無機質粉体の造粒法。
(1) Aquatic Maku is an inorganic material (DIIIL material) made of a slurry using a polymeric material that is uniformly dispersed in water as a particle binder (DIIIL material), which is compatible with water and has the above-mentioned high 9. A method for granulating inorganic IX material powder, characterized by adding an illumination agent that is difficult to dissolve the molecular material to water to turn the inorganic 0IIA material and the binding material of the molecules into a slurry. 9) Claims The solvent that is compatible with water and difficult to dissolve the polymeric material described in IK is J methyl J methoxybutanol, ethylene glycol, n-butanol, or acetic acid, and the mixing ratio of the solvent and water is 9. A method for granulating inorganic powder, characterized in that the weight ratio of water is J0 to 0-1 to 70 to 10.
JP57050459A 1982-03-29 1982-03-29 Method for granulating inorganic powder Granted JPS58166926A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP57050459A JPS58166926A (en) 1982-03-29 1982-03-29 Method for granulating inorganic powder

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP57050459A JPS58166926A (en) 1982-03-29 1982-03-29 Method for granulating inorganic powder

Publications (2)

Publication Number Publication Date
JPS58166926A true JPS58166926A (en) 1983-10-03
JPS6329579B2 JPS6329579B2 (en) 1988-06-14

Family

ID=12859453

Family Applications (1)

Application Number Title Priority Date Filing Date
JP57050459A Granted JPS58166926A (en) 1982-03-29 1982-03-29 Method for granulating inorganic powder

Country Status (1)

Country Link
JP (1) JPS58166926A (en)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0474898A1 (en) * 1990-09-11 1992-03-18 Alcoa Chemie GmbH Process for the production of alumina grinding media without kiln furniture
US5958458A (en) * 1994-06-15 1999-09-28 Dumex-Alpharma A/S Pharmaceutical multiple unit particulate formulation in the form of coated cores
US7476644B2 (en) * 2001-09-26 2009-01-13 Cooke Jr Claude E Method and materials for hydaulic fracturing of wells

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5023408A (en) * 1973-07-04 1975-03-13
JPS5039688A (en) * 1973-08-15 1975-04-11

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5023408A (en) * 1973-07-04 1975-03-13
JPS5039688A (en) * 1973-08-15 1975-04-11

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0474898A1 (en) * 1990-09-11 1992-03-18 Alcoa Chemie GmbH Process for the production of alumina grinding media without kiln furniture
US5958458A (en) * 1994-06-15 1999-09-28 Dumex-Alpharma A/S Pharmaceutical multiple unit particulate formulation in the form of coated cores
US7476644B2 (en) * 2001-09-26 2009-01-13 Cooke Jr Claude E Method and materials for hydaulic fracturing of wells

Also Published As

Publication number Publication date
JPS6329579B2 (en) 1988-06-14

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