JPS6136535B2 - - Google Patents
Info
- Publication number
- JPS6136535B2 JPS6136535B2 JP53040024A JP4002478A JPS6136535B2 JP S6136535 B2 JPS6136535 B2 JP S6136535B2 JP 53040024 A JP53040024 A JP 53040024A JP 4002478 A JP4002478 A JP 4002478A JP S6136535 B2 JPS6136535 B2 JP S6136535B2
- Authority
- JP
- Japan
- Prior art keywords
- acid
- resin
- carbonate
- parts
- mixture
- 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.)
- Expired
Links
- 229920005989 resin Polymers 0.000 claims description 24
- 239000011347 resin Substances 0.000 claims description 24
- 239000000203 mixture Substances 0.000 claims description 11
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 10
- LNOPIUAQISRISI-UHFFFAOYSA-N n'-hydroxy-2-propan-2-ylsulfonylethanimidamide Chemical compound CC(C)S(=O)(=O)CC(N)=NO LNOPIUAQISRISI-UHFFFAOYSA-N 0.000 claims description 5
- 239000005038 ethylene vinyl acetate Substances 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 claims description 4
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 3
- 238000000748 compression moulding Methods 0.000 claims description 3
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 claims description 3
- 239000001095 magnesium carbonate Substances 0.000 claims description 3
- 229910000021 magnesium carbonate Inorganic materials 0.000 claims description 3
- 229910000008 nickel(II) carbonate Inorganic materials 0.000 claims description 3
- ZULUUIKRFGGGTL-UHFFFAOYSA-L nickel(ii) carbonate Chemical compound [Ni+2].[O-]C([O-])=O ZULUUIKRFGGGTL-UHFFFAOYSA-L 0.000 claims description 3
- 238000000465 moulding Methods 0.000 claims description 2
- 150000007524 organic acids Chemical class 0.000 claims description 2
- 238000004073 vulcanization Methods 0.000 claims 1
- 239000002253 acid Substances 0.000 description 13
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 8
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 6
- 150000007513 acids Chemical class 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 6
- 229910000029 sodium carbonate Inorganic materials 0.000 description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 4
- 229910017604 nitric acid Inorganic materials 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 3
- 229910000019 calcium carbonate Inorganic materials 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000003960 organic solvent Substances 0.000 description 3
- 229910000027 potassium carbonate Inorganic materials 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 2
- LQNUZADURLCDLV-UHFFFAOYSA-N nitrobenzene Chemical compound [O-][N+](=O)C1=CC=CC=C1 LQNUZADURLCDLV-UHFFFAOYSA-N 0.000 description 2
- 239000000779 smoke Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- QTWJRLJHJPIABL-UHFFFAOYSA-N 2-methylphenol;3-methylphenol;4-methylphenol Chemical compound CC1=CC=C(O)C=C1.CC1=CC=CC(O)=C1.CC1=CC=CC=C1O QTWJRLJHJPIABL-UHFFFAOYSA-N 0.000 description 1
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- HDYRYUINDGQKMC-UHFFFAOYSA-M acetyloxyaluminum;dihydrate Chemical compound O.O.CC(=O)O[Al] HDYRYUINDGQKMC-UHFFFAOYSA-M 0.000 description 1
- 238000010306 acid treatment Methods 0.000 description 1
- 229940009827 aluminum acetate Drugs 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 229930003836 cresol Natural products 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000013505 freshwater Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 235000005985 organic acids Nutrition 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- IIACRCGMVDHOTQ-UHFFFAOYSA-N sulfamic acid group Chemical class S(N)(O)(=O)=O IIACRCGMVDHOTQ-UHFFFAOYSA-N 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 238000004506 ultrasonic cleaning Methods 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
Landscapes
- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
Description
【発明の詳細な説明】
本発明は多孔質樹脂の製造方法に関するもので
ある。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for producing porous resin.
多孔質材の製法として樹脂内部に微細分末を均
一に分散せしめ、この樹脂を圧縮成形し成形後、
塩酸と硝酸との混合溶液で樹脂内の炭酸カルシウ
ムを抽出し多孔質樹脂を製造する方法がある。し
かしながらこの方法は炭酸カルシウムを使用して
いるため、硫酸を使用すると硫酸カルシウムが生
成されるため、使用する酸は塩酸又は硝酸或は両
者の混合液に限定される。さらにこれらの酸は揮
発性であり、空気中で発煙し刺激臭を与え有害で
あり、又著しく腐蝕性であり特に混合液の場合に
は極めて著しい欠点を有する。 As a manufacturing method for porous materials, fine particles are uniformly dispersed inside the resin, and after compression molding,
There is a method of producing porous resin by extracting calcium carbonate from the resin with a mixed solution of hydrochloric acid and nitric acid. However, since this method uses calcium carbonate, the acid used is limited to hydrochloric acid, nitric acid, or a mixture of both, since calcium sulfate is produced when sulfuric acid is used. Moreover, these acids are volatile, emit smoke in the air, give off a pungent odor and are harmful, and are also extremely corrosive, which is a very serious drawback, especially when mixed.
本願発明は前述の欠点を除き有害物の発生のな
い安全な印判用樹脂を製造する方法を提供するも
ので、ゴムに似た弾性を有し、柔軟性に富み強靭
で低温性に優れ、加硫を要せず射出成形可能なエ
チレン酢酸ビニル共重合体に微細粉末とした炭酸
ナトリウム、炭酸カリウム、炭酸マグネシウム、
炭酸ニツケルのいずれか、又はそれら二種以上の
任意の混合体とを混合し、次にシクロヘキサン、
ベンゼン、アセトン、酢酸アルミ等のエチレン酢
酸ビニル共重合体の溶剤を加えて均一に混合撹拌
したのち、加えた前記炭酸塩の分散性を良好なら
しめるため、エチレングリコール、又はジエチレ
ングリコール或はプロピレングリコール等の如き
親水性溶剤を加えて良く撹拌混合し、この混合物
を80〜110℃に加熱し硬度を変化せしめ成形性を
良くしロールにかけて前記炭酸塩の分散を均一な
らしめ、シート状に成形したのち酸処理をする。
使用する酸としては、炭酸カルシウム使用の場合
には使用出来なかつた硫酸が使用出来ると共に、
同類のスルフアミン酸を始めその他多くの有機酸
も又使用出来、使用する酸に限定はない。 The present invention provides a method for producing a safe resin for stamps that does not generate harmful substances except for the above-mentioned drawbacks. Sodium carbonate, potassium carbonate, magnesium carbonate, finely powdered ethylene vinyl acetate copolymer that can be injection molded without the need for sulfur.
Mix nickel carbonate or any mixture of two or more thereof, then cyclohexane,
After adding a solvent for ethylene-vinyl acetate copolymer such as benzene, acetone, and aluminum acetate and stirring uniformly, ethylene glycol, diethylene glycol, propylene glycol, etc. are added to improve the dispersibility of the added carbonate. Add a hydrophilic solvent such as and mix well with stirring, heat this mixture to 80 to 110°C to change the hardness and improve moldability, roll it to uniformly disperse the carbonate, and then shape it into a sheet. Treat with acid.
As the acid used, sulfuric acid, which cannot be used when calcium carbonate is used, can be used, and
Many other organic acids, including the related sulfamic acids, can also be used, and there is no limit to the acids used.
特に塩酸、硝酸の様な揮発性の酸に対して硫酸
又はスルフアミン酸の様に不揮発性の酸を使用出
来る事は大なる利点であり、又低濃度の酸でこと
たりる等の利点を有する。特に脱炭酸塩促進のた
め40〜60℃で行なうと塩酸及び硝酸又はその混合
液で処理の場合は前記揮発に依る発煙性著しく、
又刺激臭強く腐蝕性が激しくなるのでこれら酸を
使用する場合には低温で行なわれなければならず
脱炭酸塩に長時間を要した。しかるに硫酸又はス
ルフアミン酸は揮発性ではなく、高温脱炭酸塩処
理が可能であるばかりでなく、脱炭酸塩処理の促
進のために超音波装置等を用いる場合に於いては
装置を腐蝕させる事がないから極めて有利であ
り、この目的にはスルフアミン酸の使用が最適で
ある。 In particular, it is a great advantage to be able to use non-volatile acids such as sulfuric acid or sulfamic acid over volatile acids such as hydrochloric acid and nitric acid, and it also has the advantage of being able to be used with low concentration acids. . In particular, when treatment is carried out at 40 to 60°C to promote decarbonation, smoke generation due to the above-mentioned volatilization is significant when treatment is performed with hydrochloric acid, nitric acid, or a mixture thereof.
Furthermore, since these acids have a strong pungent odor and are highly corrosive, they must be carried out at low temperatures and decarbonation requires a long time. However, sulfuric acid or sulfamic acid is not volatile, and not only can high-temperature decarbonation treatment be performed, but when an ultrasonic device or the like is used to promote decarbonation treatment, it may corrode the device. The use of sulfamic acid is most advantageous for this purpose.
又前記炭酸塩中、炭酸ナトリウム、炭酸カリウ
ムのいずれか或はその混合体を使用の場合には酸
に依る脱炭酸塩の除去が極めて容易であるばかり
でなく、多少時間がかゝるが水でも抽出可能であ
る等の利点を有するのである。以上の脱炭酸塩の
抽出後水洗し、樹脂の収縮を一定にすると共に軟
化性を与えるため有機溶媒に浸漬させ乾燥させる
事に依り強い弾性を有し、吸水吸油に依る膨脹変
形が少ない、多孔質樹脂が得られる。又多孔質化
を行なつてからも圧縮成形が可能であり、更に酸
処理を加減する事に依つても任意の弾性を有する
多孔質樹脂を得る事が出来る。この様にして得ら
れた樹脂は、印材に最適である他防音材、炉材等
に使用可能である。以下実施例に依り本願発明を
説明する。 In addition, when using either sodium carbonate or potassium carbonate or a mixture thereof among the carbonates, not only is it extremely easy to remove the decarbonate with an acid, but it is also possible to remove the decarbonate with an acid, although it takes some time. It has the advantage that it can be extracted even if After extraction of the above decarbonate, the resin is washed with water, immersed in an organic solvent to maintain constant shrinkage and soften, and then dried, resulting in strong elasticity, less expansion deformation due to water and oil absorption, and a porous resin. A high quality resin is obtained. Further, compression molding is possible even after making the resin porous, and a porous resin having arbitrary elasticity can be obtained by controlling the acid treatment. The resin thus obtained is ideal for stamp materials, and can also be used for soundproofing materials, furnace materials, etc. The present invention will be explained below with reference to Examples.
実施例 1
エチレン酢酸ビニル共重合体20部(重量比以下
同様)に500〜650℃で焼成微粉末とした炭酸ナト
リウム60部をよく混合し、次にこれにシクロヘキ
サン25部を加えて均一に撹拌したのち約20分間放
置する。Example 1 20 parts of ethylene-vinyl acetate copolymer (same ratio below) was thoroughly mixed with 60 parts of sodium carbonate, which was calcined as a fine powder at 500 to 650°C, and then 25 parts of cyclohexane was added thereto and stirred uniformly. After that, leave it for about 20 minutes.
次いでエチレングリコール20部を加えてよく撹
拌し暫らく放置したのちこの混合物を80〜110℃
に加熱した開放型混合ロールにかけ約15分間この
操作を反覆したのちロールの巾を調節して任意の
厚さのシートに成形する。 Next, 20 parts of ethylene glycol was added, stirred well and left to stand for a while, and the mixture was heated to 80-110°C.
After repeating this operation for about 15 minutes on an open-type mixing roll heated to , the width of the roll is adjusted to form a sheet of desired thickness.
次に必要なればこれを任意の形状に加熱成形し
たのち20%一硫酸に24時間浸漬後流水中で1時間
洗浄する。 Next, if necessary, this is heated and molded into any shape, immersed in 20% monosulfuric acid for 24 hours, and then washed in running water for 1 hour.
次いでブチルアルコール30部、キシレン30部、
ニトロベンゼン10部、クレゾール5部の有機溶媒
に20分間浸漬し樹脂の収縮を一定にすれば多孔質
樹脂が出来上る。尚上記有機溶媒処理は本願発明
の多孔質化に於いては副次的なものである。 Next, 30 parts of butyl alcohol, 30 parts of xylene,
A porous resin can be created by immersing it in an organic solvent of 10 parts of nitrobenzene and 5 parts of cresol for 20 minutes to keep the resin shrinkage constant. Note that the organic solvent treatment described above is secondary to the process of forming a porous structure according to the present invention.
実施例 2
実施例1同様にして処理し加熱成形して得られ
た樹脂を13%一スルフアミン酸溶液を用い超音波
洗浄装置を使用し、脱炭酸塩処理を4時間行なつ
た。次いで水洗処理も超音波洗浄装置を使用しそ
の都度新しい水を用い5分間ずつ5回処理を行な
つた。出来上つた多孔質樹脂は実施例1の樹脂と
同じであつた。又スルフアミン酸のかわりにクエ
ン酸の20%溶液を用いた場合に於いても同様結果
が得られた。Example 2 A resin obtained by treatment and heat molding in the same manner as in Example 1 was subjected to decarbonation treatment for 4 hours using a 13% monosulfamic acid solution and an ultrasonic cleaning device. Next, water washing was carried out five times for 5 minutes each time using an ultrasonic washing device and using fresh water each time. The resulting porous resin was the same as the resin of Example 1. Similar results were also obtained when a 20% solution of citric acid was used instead of sulfamic acid.
実施例 3
炭酸カリウム60部を使用した以外実施例1と同
様に処理して得られた樹脂を実施例2に依る装置
と方法に依り処理した樹脂は実施例1の樹脂と同
様であつた。Example 3 A resin obtained by processing in the same manner as in Example 1 except that 60 parts of potassium carbonate was used was treated using the apparatus and method according to Example 2. The resin was the same as the resin in Example 1.
実施例 4
炭酸ナトリウム30部と炭酸マグネシウム30部と
の混合使用を用した以外実施例1の場合同様に処
理して得られた樹脂を実施例2に依る装置と方法
に依り処理した。得られた樹脂は実施例1の場合
と同じであつた。Example 4 A resin obtained by the same treatment as in Example 1 except that a mixture of 30 parts of sodium carbonate and 30 parts of magnesium carbonate was used was treated using the apparatus and method according to Example 2. The resin obtained was the same as in Example 1.
実施例 5
炭酸ナトリウム30部と炭酸ニツケル30部との混
合体を用いた以外実施例1の場合同様に処理して
得られた樹脂を実施例2に依る装置と方法に依り
処理した。得られた樹脂は実施例1の場合と同等
であつた。Example 5 A resin obtained by the same treatment as in Example 1 except that a mixture of 30 parts of sodium carbonate and 30 parts of nickel carbonate was used was treated using the apparatus and method according to Example 2. The resin obtained was the same as in Example 1.
Claims (1)
に炭酸マグネシウム、炭酸ニツケルのいずれか、
又はそれらの二種以上の混合体を分散混入せし
め、次いで圧縮成形し成形後硫酸又はスルフアミ
ン酸或は有機酸で処理し、前記分散炭酸塩を抽出
する事を特徴とする多孔質樹脂の製造方法。1. Ethylene-vinyl acetate copolymer that does not require vulcanization and either magnesium carbonate or nickel carbonate,
or a method for producing a porous resin, which comprises dispersing and mixing a mixture of two or more thereof, followed by compression molding, and after molding, treating with sulfuric acid, sulfamic acid, or an organic acid to extract the dispersed carbonate. .
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP4002478A JPS54131665A (en) | 1978-04-04 | 1978-04-04 | Production of porous resin |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP4002478A JPS54131665A (en) | 1978-04-04 | 1978-04-04 | Production of porous resin |
Publications (2)
Publication Number | Publication Date |
---|---|
JPS54131665A JPS54131665A (en) | 1979-10-12 |
JPS6136535B2 true JPS6136535B2 (en) | 1986-08-19 |
Family
ID=12569326
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP4002478A Granted JPS54131665A (en) | 1978-04-04 | 1978-04-04 | Production of porous resin |
Country Status (1)
Country | Link |
---|---|
JP (1) | JPS54131665A (en) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS6339637U (en) * | 1986-08-29 | 1988-03-15 | ||
JPH051788Y2 (en) * | 1986-05-15 | 1993-01-18 |
Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS503348A (en) * | 1973-05-10 | 1975-01-14 | ||
JPS5074667A (en) * | 1973-11-02 | 1975-06-19 | ||
JPS5346226A (en) * | 1976-10-08 | 1978-04-25 | Toshiba Corp | Color television receiving circuit for pal |
JPS5742651A (en) * | 1980-07-17 | 1982-03-10 | Kurosa Yozefu | Non-hygroscopic salt of 4-hydroxybutyric acid, manufacture and drug containing same |
JPS5745782A (en) * | 1980-09-02 | 1982-03-15 | Sony Corp | Flicker preventing circuit |
-
1978
- 1978-04-04 JP JP4002478A patent/JPS54131665A/en active Granted
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS503348A (en) * | 1973-05-10 | 1975-01-14 | ||
JPS5074667A (en) * | 1973-11-02 | 1975-06-19 | ||
JPS5346226A (en) * | 1976-10-08 | 1978-04-25 | Toshiba Corp | Color television receiving circuit for pal |
JPS5742651A (en) * | 1980-07-17 | 1982-03-10 | Kurosa Yozefu | Non-hygroscopic salt of 4-hydroxybutyric acid, manufacture and drug containing same |
JPS5745782A (en) * | 1980-09-02 | 1982-03-15 | Sony Corp | Flicker preventing circuit |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH051788Y2 (en) * | 1986-05-15 | 1993-01-18 | ||
JPS6339637U (en) * | 1986-08-29 | 1988-03-15 |
Also Published As
Publication number | Publication date |
---|---|
JPS54131665A (en) | 1979-10-12 |
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