JPH0388824A - Purification of polyethers - Google Patents
Purification of polyethersInfo
- Publication number
- JPH0388824A JPH0388824A JP22464489A JP22464489A JPH0388824A JP H0388824 A JPH0388824 A JP H0388824A JP 22464489 A JP22464489 A JP 22464489A JP 22464489 A JP22464489 A JP 22464489A JP H0388824 A JPH0388824 A JP H0388824A
- Authority
- JP
- Japan
- Prior art keywords
- catalyst
- polyether
- polyethers
- treatment
- deactivated
- 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
Links
- 229920000570 polyether Polymers 0.000 title claims abstract description 47
- 238000000746 purification Methods 0.000 title description 2
- 239000003054 catalyst Substances 0.000 claims abstract description 39
- 239000004721 Polyphenylene oxide Substances 0.000 claims abstract description 32
- 238000011282 treatment Methods 0.000 claims abstract description 17
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000003463 adsorbent Substances 0.000 claims abstract description 6
- 238000007142 ring opening reaction Methods 0.000 claims abstract description 5
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- 239000003999 initiator Substances 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 10
- 125000004432 carbon atom Chemical group C* 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 abstract description 7
- 239000002184 metal Substances 0.000 abstract description 7
- 239000011541 reaction mixture Substances 0.000 abstract 2
- 238000002425 crystallisation Methods 0.000 abstract 1
- 230000008025 crystallization Effects 0.000 abstract 1
- 238000006243 chemical reaction Methods 0.000 description 7
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 6
- 239000002253 acid Substances 0.000 description 5
- 239000002131 composite material Substances 0.000 description 4
- 229910052500 inorganic mineral Inorganic materials 0.000 description 4
- 239000011707 mineral Substances 0.000 description 4
- 235000010755 mineral Nutrition 0.000 description 4
- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 229920005862 polyol Polymers 0.000 description 3
- 150000003077 polyols Chemical class 0.000 description 3
- 230000009257 reactivity Effects 0.000 description 3
- 208000005156 Dehydration Diseases 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- XSTXAVWGXDQKEL-UHFFFAOYSA-N Trichloroethylene Chemical compound ClC=C(Cl)Cl XSTXAVWGXDQKEL-UHFFFAOYSA-N 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 239000004927 clay Substances 0.000 description 2
- 230000018044 dehydration Effects 0.000 description 2
- 238000006297 dehydration reaction Methods 0.000 description 2
- XCOBTUNSZUJCDH-UHFFFAOYSA-B lithium magnesium sodium silicate Chemical compound [Li+].[Li+].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Na+].[Na+].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].O1[Si](O2)([O-])O[Si]3([O-])O[Si]1([O-])O[Si]2([O-])O3.O1[Si](O2)([O-])O[Si]3([O-])O[Si]1([O-])O[Si]2([O-])O3.O1[Si](O2)([O-])O[Si]3([O-])O[Si]1([O-])O[Si]2([O-])O3.O1[Si](O2)([O-])O[Si]3([O-])O[Si]1([O-])O[Si]2([O-])O3.O1[Si](O2)([O-])O[Si]3([O-])O[Si]1([O-])O[Si]2([O-])O3.O1[Si](O2)([O-])O[Si]3([O-])O[Si]1([O-])O[Si]2([O-])O3 XCOBTUNSZUJCDH-UHFFFAOYSA-B 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 150000002825 nitriles Chemical class 0.000 description 2
- 235000021317 phosphate Nutrition 0.000 description 2
- 229920001228 polyisocyanate Polymers 0.000 description 2
- 239000005056 polyisocyanate Substances 0.000 description 2
- 239000004814 polyurethane Substances 0.000 description 2
- 229920002635 polyurethane Polymers 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 241000894007 species Species 0.000 description 2
- -1 urethane compound Chemical class 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 241001655798 Taku Species 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000009849 deactivation Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000001784 detoxification Methods 0.000 description 1
- XLIDPNGFCHXNGX-UHFFFAOYSA-N dialuminum;oxygen(2-);silicon(4+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Al+3].[Al+3].[Si+4] XLIDPNGFCHXNGX-UHFFFAOYSA-N 0.000 description 1
- 238000010494 dissociation reaction Methods 0.000 description 1
- 230000005593 dissociations Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 239000012948 isocyanate Substances 0.000 description 1
- 150000002513 isocyanates Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- ZADYMNAVLSWLEQ-UHFFFAOYSA-N magnesium;oxygen(2-);silicon(4+) Chemical compound [O-2].[O-2].[O-2].[Mg+2].[Si+4] ZADYMNAVLSWLEQ-UHFFFAOYSA-N 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920001451 polypropylene glycol Polymers 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- AVWRKZWQTYIKIY-UHFFFAOYSA-N urea-1-carboxylic acid Chemical group NC(=O)NC(O)=O AVWRKZWQTYIKIY-UHFFFAOYSA-N 0.000 description 1
- 239000011592 zinc chloride Substances 0.000 description 1
- 235000005074 zinc chloride Nutrition 0.000 description 1
Landscapes
- Polyethers (AREA)
Abstract
Description
【発明の詳細な説明】 [産業上の利用分野] 本発明はポリエーテルの精製方法に関するものである。[Detailed description of the invention] [Industrial application field] The present invention relates to a method for purifying polyether.
[従来の技術]
従来、複合金属シアン化物錯隊を触媒に用いてポリエー
テル類を合成したのち、これをナトリウム、カリウム金
属又は水酸化ナトリウム。[Prior Art] Conventionally, polyethers are synthesized using a composite metal cyanide complex as a catalyst, and then this is synthesized with sodium, potassium metal or sodium hydroxide.
水酸化カリウム等で処理して触媒を失活せしめ、ついで
リン酸塩等の鉱酸で上記ポリエーテル類を処理して、失
活した触媒成分と処理剤を沈殿させ、ポリエーテル類か
ら濾別する方法が提案されている(特開昭57−760
28 )。The catalyst is deactivated by treatment with potassium hydroxide, etc., and then the polyethers are treated with a mineral acid such as phosphate to precipitate the deactivated catalyst components and the processing agent, which are filtered out from the polyethers. A method has been proposed to
28).
【発明の解決しようとする問題点]
不飽和モノオールの生成が少なく、また極めて高分子量
なポリオール類を合成する触媒として複合金属シアン化
物錯体は好適であるが、重合後これらポリエーテル類中
に上記触媒が存在するとポリウレタン製造時のポリエー
テルとポリイソシアネートの反応の際に有意義な量のア
ロファネートの基の形成等の触媒作用を示し、ポリウレ
タン生成物の物性を低下させるため、上記触媒成分をポ
リエーテル類から除去するか又は完全失活せしめ無害化
する必要がある。[Problems to be Solved by the Invention] Multimetal cyanide complexes are suitable as catalysts for synthesizing polyols with a small amount of unsaturated monools and have extremely high molecular weights, but after polymerization, there are The presence of the above catalysts catalyzes the reaction of polyether and polyisocyanate during polyurethane production, including the formation of significant amounts of allophanate groups, reducing the physical properties of the polyurethane product. It is necessary to remove it from ethers or completely deactivate it to render it harmless.
前述した触媒をアルカリ等の処理剤で失活せしめる方法
は、有効な手段の一つではあるが、前記処理剤がウレタ
ン製造の際に好ましくない反応の触媒作用を提するため
、これを各種鉱酸で中和、再精製する等の複雑な処理が
必要となる欠点を有していた。The method of deactivating the catalyst with a treating agent such as alkali is one effective method, but since the treating agent catalyzes undesirable reactions during the production of urethane, it is used in various minerals. It had the disadvantage of requiring complicated treatments such as neutralization with acid and repurification.
c問題点を解決するための手段J
本発明は前述の問題を解決すべく種々研究の結果見い出
された下記の発明を提案するものであり、複合金属シア
ン化物錯隊触媒の存在下、イニシェークーに炭素数3以
上のモノエポキサイドを開環反応せしめて得られた、上
記触媒を含むポリエーテル類を水の存在下又は非存在下
で熱処理して触媒を失活せしめ、ついで必要に応じて晶
析剤もしくは無機質吸着剤から成る処理剤で処理後、濾
過することにより、失活した触媒をポリエーテル類から
除去することを特徴とするポリエーテル類の精製法を提
供するものである。cMeans for Solving the ProblemsJ The present invention proposes the following invention, which was discovered as a result of various studies, in order to solve the above-mentioned problems. A polyether containing the above-mentioned catalyst obtained by subjecting a monoepoxide having 3 or more carbon atoms to a ring-opening reaction is heat-treated in the presence or absence of water to deactivate the catalyst, and then crystallized as necessary. The present invention provides a method for purifying polyethers, which is characterized in that deactivated catalysts are removed from polyethers by filtration after treatment with a treatment agent consisting of a catalyst or an inorganic adsorbent.
複合金属シアン化物錯体を含むポリエーテル類の精製法
として、前記触媒を含むポリエーテル類を触媒を失活せ
しめるのに十分な量の水と温度条件のもと熱処理して複
合金属シアン化物錯体をイオン種に分解、無害化する。As a method for purifying polyethers containing a composite metal cyanide complex, the polyether containing the catalyst is heat-treated in an amount of water and under temperature conditions sufficient to deactivate the catalyst to obtain a composite metal cyanide complex. Decomposes into ionic species and becomes harmless.
添加する水の量は使用する複合金属シアン化物触媒の量
、ポリエーテル類の種類によっても異なるが、通常0.
2〜10 wt%の範囲から適宜選べば良く、例えば分
子量10.000のトリオールで触媒添加量が500
ppm /ポリエーテルの場合、処理に用いる水の量は
0.5〜3wt%/ポリエーテル、好ましくは1〜2
wt%が適当である。水の量が少ないと触媒成分を無害
化するに長時間を要し、又水の量が多くなるとポリエー
テルを含む液系の粘度が上昇し、水による触媒の無害化
反応が阻害されるので好ましくない。The amount of water added varies depending on the amount of composite metal cyanide catalyst used and the type of polyether, but is usually 0.
It may be selected as appropriate from the range of 2 to 10 wt%, for example, a triol with a molecular weight of 10.000 and a catalyst addition amount of 500.
ppm/polyether, the amount of water used for treatment is 0.5-3 wt%/polyether, preferably 1-2
wt% is appropriate. If the amount of water is small, it will take a long time to detoxify the catalyst components, and if the amount of water is large, the viscosity of the liquid system containing polyether will increase and the detoxification reaction of the catalyst by water will be inhibited. Undesirable.
処理温度の範囲は処理する触媒を含むポリエーテルの種
類、水添加の有無等によって若干異なるが、通常100
〜180℃の範囲から適宜選べば良く、例えば分子量1
0.000のポリエーテルで水添加系の場合120〜1
70℃、好ましくは130〜150℃が適当であり、水
熱添加系では温度を150〜180℃に保つと良い。温
度が上記範囲以下では、複合金属シアン化物錯体触媒の
失活が十分に進行せず、又180℃以上の温度領域では
ポリエーテルの分解が一部進行するので好ましくない。The treatment temperature range varies slightly depending on the type of polyether containing the catalyst to be treated, presence or absence of water addition, etc., but is usually 100
It may be selected appropriately from the range of ~180°C, for example, molecular weight 1
0.000 polyether and water addition system: 120-1
A suitable temperature is 70°C, preferably 130-150°C, and in a hydrothermal addition system, the temperature is preferably maintained at 150-180°C. If the temperature is below the above range, the deactivation of the multimetal cyanide complex catalyst will not proceed sufficiently, and if the temperature is above 180° C., part of the decomposition of the polyether will proceed, which is not preferable.
処理時間は使用する複合金属シアン化物錯隊の添加量、
ポリオールの種類等によって異なるが、1〜6時間、好
ましくは2〜4時間の範囲から適宜選べば良い。The processing time depends on the amount of compound metal cyanide complex used,
Although it varies depending on the type of polyol, etc., the time may be appropriately selected from the range of 1 to 6 hours, preferably 2 to 4 hours.
前記処理により触媒は失活し、脱水処理後、これらポリ
エーテル類と、ポリイソシアネートによるウレタン化合
物の合成に直接供することも可能であるが、ポリエーテ
ル中に懸濁している失活した触媒残留物を前記ポリエー
テル類から除去するため、晶析剤又は無機質吸着剤から
なる処理剤で処理して、ポリエーテル類から濾別すると
良い。The catalyst is deactivated by the above treatment, and after dehydration treatment, it is possible to directly use these polyethers and polyisocyanate to synthesize a urethane compound, but the deactivated catalyst residue suspended in the polyether In order to remove it from the polyethers, it is preferable to treat it with a treatment agent consisting of a crystallizing agent or an inorganic adsorbent and filter it from the polyethers.
処理剤として晶析剤を用いる場合は、25℃の水溶液中
における解離常数が10””以上の鉱酸を用いるのが適
しており、Na 、Ba 、K 、Ca 、A1等の1
種又は1種以上からなる硫酸塩、リン酸塩等の中から適
宜選べば良い。処理剤として無機質吸着剤を使用する場
合、例えばLizCO□Na黛COi 、MgCO5、
CaCO5等のI族および■族、■族の酸化物もしくは
水酸化物、2.5Mg0・A1□03・xH,O(キジ
ワード300.共和化学品)等で示される合成ケイ酸ア
ルミニウム、合成ケイ酸マグネシウムもしくは活性白土
、酸性白土又はそれらの混合物の1種又は1種以上を適
宜使用すれば良く、失活した複合金属シアン化物錯体を
含むポリエーテルも脱水処理する前に前記処理剤をポリ
エーテル類中に添加し、温度90〜150℃、好ましく
は100〜120℃の条件下で1〜2時間撹拌後、上記
温度条件下で減圧脱気して、失活した触媒を晶析剤と共
沈させるかもしくは吸着剤で処理して除去せしめる。When using a crystallizer as a treatment agent, it is suitable to use a mineral acid with a dissociation constant of 10'' or more in an aqueous solution at 25°C, and mineral acids such as Na, Ba, K, Ca, A1, etc.
It may be selected as appropriate from sulfates, phosphates, etc. consisting of one or more species. When using an inorganic adsorbent as a treatment agent, for example, LizCO□NamayuzushiCOi, MgCO5,
Oxides or hydroxides of Group I, Group ■, Group ■ such as CaCO5, synthetic aluminum silicate, synthetic silicic acid represented by 2.5Mg0・A1□03・xH,O (Kijiward 300. Kyowa Chemicals), etc. One or more of magnesium, activated clay, acid clay, or a mixture thereof may be used as appropriate, and polyethers containing deactivated multimetal cyanide complexes may also be treated with the above-mentioned treating agent before dehydration treatment. After stirring for 1 to 2 hours at a temperature of 90 to 150°C, preferably 100 to 120°C, the degassed under reduced pressure at the above temperature conditions to coprecipitate the deactivated catalyst with the crystallizer. Remove it by letting it dry or by treating it with an adsorbent.
上記一連の処理により、ウレタン反応に好適な精製され
たポリエーテル類の提供が可能となる。Through the above series of treatments, it is possible to provide purified polyethers suitable for urethane reactions.
[実施例]
以下に本発明を実施例および比較例により具体的に説明
するが、本発明はこれら実施例のみに限定されるもので
はない。[Examples] The present invention will be specifically explained below using Examples and Comparative Examples, but the present invention is not limited only to these Examples.
(実施例1)
塩化亜鉛とアルカリ金属シアノコパルテートから合成し
た複合金属シアン化物錯体(Zn60 、Co 30
ppm )を用いて合成した分子量5、000のポリオ
キシプロピレントリオールに重量で2 wt%の水を添
加し、150℃の温度条件下で3時間混合した。次いで
温度120℃、圧力10 Torrの条件下、減圧脱気
し共存する水分を除去することにより失活した触媒成分
が微量懸濁したポリエーテルを得た。このポリエーテル
とP−MDIとの反応性を調べた結果を第1図に示すが
、触媒を含まないポリエーテルと同等の反応挙動が得ら
れることを確認した。(Example 1) Multimetal cyanide complex synthesized from zinc chloride and alkali metal cyanocopaltate (Zn60, Co30
2 wt% of water was added to a polyoxypropylene triol with a molecular weight of 5,000 synthesized using (ppm) and mixed at a temperature of 150°C for 3 hours. Next, the mixture was degassed under reduced pressure at a temperature of 120° C. and a pressure of 10 Torr to remove coexisting moisture, thereby obtaining a polyether in which a small amount of the deactivated catalyst component was suspended. The results of examining the reactivity of this polyether with P-MDI are shown in FIG. 1, and it was confirmed that reaction behavior equivalent to that of polyether containing no catalyst was obtained.
(実施例2)
実施例1の処理をほどこした失活した触媒を含むポリエ
ーテルに重量で0.8 wt%のNa5HP107と
l wt%の合成ケイ酸マグネシウム(KW−600S
、共和化学)を添加し、120 ”C(7)温度条件
下0.5Hrs混合後、上記温度条件で10Torrの
圧力下で減圧脱気した。(Example 2) 0.8 wt% Na5HP107 was added to the polyether containing the deactivated catalyst treated in Example 1.
l wt% synthetic magnesium silicate (KW-600S
, Kyowa Kagaku) and mixed for 0.5 hours under a temperature condition of 120''C(7), and then degassed under reduced pressure under a pressure of 10 Torr under the above temperature condition.
ついでN15Cの濾紙を用いて、ポリエーテルから前記
失活した触媒と処理剤を分離した結果、ポリエーテル中
からZn 、Goの約92%相当量を除去できた。この
ポリエーテルは透明でありイソシアネートと正常な反応
を示すことが確認された。Next, the deactivated catalyst and processing agent were separated from the polyether using N15C filter paper, and as a result, approximately 92% of Zn and Go could be removed from the polyether. It was confirmed that this polyether was transparent and showed normal reaction with isocyanate.
(実施例3)
実施例1と同様のポリエーテルを温度170’Cの条件
下3時間熱処理後、合成ケイ酸マグネシウム(KW−6
0O3、共和化学)をポリエーテルに対して1.5wt
%添加し、温度120’Cの条件下約1時間減圧処理し
た。ついで&5Cの濾紙を用いて上記ポリエーテルから
失活触媒と処理剤を分離した結果、ポリエーテル中から
Zn 、G。(Example 3) After heat treating the same polyether as in Example 1 at a temperature of 170'C for 3 hours, synthetic magnesium silicate (KW-6
0O3, Kyowa Kagaku) to polyether at 1.5wt.
% was added and treated under reduced pressure at a temperature of 120'C for about 1 hour. Then, the deactivated catalyst and processing agent were separated from the polyether using a &5C filter paper, and as a result, Zn and G were extracted from the polyether.
の約80%相当量が除去できており、P−MDIとの反
応性も正常であった。About 80% of the amount was removed, and the reactivity with P-MDI was also normal.
[発明の効果]
本発明は、複合金属シアン化物錯体を触媒に用いて、イ
ニシエーターに炭素数3以上のモノエポキサイドを開環
反応せしめて得られたポリエーテル類を規定された温度
条件下で熱処理することにより、上記ポリエーテル中の
触媒を失活させる簡便な精製法を提案するものである。[Effects of the Invention] The present invention provides polyethers obtained by ring-opening a monoepoxide having 3 or more carbon atoms as an initiator using a multimetal cyanide complex as a catalyst under specified temperature conditions. We propose a simple purification method in which the catalyst in the polyether is deactivated by heat treatment.
従来採用されてきた分解剤としてKOH等のアルカリを
用いる方法では、上記分解剤が次のウレタン工程で有害
な反応の触媒として作用するため、再度このアルカリ成
分を除去するための精製処理が必要となりコストアップ
の要因となっていた。In the conventional method of using an alkali such as KOH as a decomposing agent, the decomposing agent acts as a catalyst for harmful reactions in the next urethane process, so refining treatment is required to remove this alkaline component again. This was a factor in increasing costs.
本性では、上記触媒を熱処理のみで失活、無害化するも
ので、より安価な精製ポリエーテルの提供が可能となる
。In essence, the above-mentioned catalyst is deactivated and rendered harmless only by heat treatment, making it possible to provide purified polyether at a lower cost.
第1図は本発明により得られたポリエーテルポリオール
の反応性を表わすグラフである。
拓
!
図
一政団Tf1開(HIS)FIG. 1 is a graph showing the reactivity of the polyether polyol obtained according to the present invention. Taku! Figure 1 Seidan Tf1 Kai (HIS)
Claims (2)
ーターに炭素数3以上のモノエポキサイドを開環反応せ
しめて得られた、上記触媒を含むポリエーテル類を水の
存在下又は非存在下で熱処理して触媒を失活せしめ、つ
いで必要に応じて晶析剤もしくは無機質吸着剤 から成る処理剤で処理後、濾過することにより、失活し
た触媒をポリエーテル類から除去することを特徴とする
ポリエーテル類の精製法。(1) Polyethers containing the above catalyst obtained by ring-opening a monoepoxide having 3 or more carbon atoms as an initiator in the presence of a multimetal cyanide complex catalyst in the presence or absence of water. The deactivated catalyst is removed from the polyether by heat treatment to deactivate the catalyst, and then optionally treated with a treatment agent consisting of a crystallizer or an inorganic adsorbent, followed by filtration. A method for purifying polyethers.
する請求項第1項に記載の方法。(2) The method according to claim 1, characterized in that the treatment temperature is 100 to 180°C.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP22464489A JP2954604B2 (en) | 1989-09-01 | 1989-09-01 | Purification method of polyethers |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP22464489A JP2954604B2 (en) | 1989-09-01 | 1989-09-01 | Purification method of polyethers |
Publications (2)
Publication Number | Publication Date |
---|---|
JPH0388824A true JPH0388824A (en) | 1991-04-15 |
JP2954604B2 JP2954604B2 (en) | 1999-09-27 |
Family
ID=16816949
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP22464489A Expired - Fee Related JP2954604B2 (en) | 1989-09-01 | 1989-09-01 | Purification method of polyethers |
Country Status (1)
Country | Link |
---|---|
JP (1) | JP2954604B2 (en) |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0693513A2 (en) | 1994-07-18 | 1996-01-24 | Asahi Glass Company Ltd. | Process for purifying a polyether |
WO2008026657A1 (en) | 2006-08-31 | 2008-03-06 | Asahi Glass Company, Limited | Method of purifying polyether compound |
WO2011040418A1 (en) | 2009-09-30 | 2011-04-07 | 旭硝子株式会社 | Method for manufacturing an isocyanate-terminated prepolymer, prepolymer obtained thereby, and polyurethane resin |
JP4717467B2 (en) * | 2005-02-22 | 2011-07-06 | ライオン株式会社 | container |
-
1989
- 1989-09-01 JP JP22464489A patent/JP2954604B2/en not_active Expired - Fee Related
Cited By (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0693513A2 (en) | 1994-07-18 | 1996-01-24 | Asahi Glass Company Ltd. | Process for purifying a polyether |
US5811566A (en) * | 1994-07-18 | 1998-09-22 | Asahi Glass Company Ltd. | Process for purifying a polyether |
US5973096A (en) * | 1994-07-18 | 1999-10-26 | Asahi Glass Company Ltd. | Process for purifying a polyether |
JP4717467B2 (en) * | 2005-02-22 | 2011-07-06 | ライオン株式会社 | container |
WO2008026657A1 (en) | 2006-08-31 | 2008-03-06 | Asahi Glass Company, Limited | Method of purifying polyether compound |
US8354559B2 (en) | 2006-08-31 | 2013-01-15 | Asahi Glass Company, Limited | Process for purifying polyether |
WO2011040418A1 (en) | 2009-09-30 | 2011-04-07 | 旭硝子株式会社 | Method for manufacturing an isocyanate-terminated prepolymer, prepolymer obtained thereby, and polyurethane resin |
US8431672B2 (en) | 2009-09-30 | 2013-04-30 | Asahi Glass Company, Limited | Method for manufacturing an isocyanate-terminated prepolymer, prepolymer obtained thereby, and polyurethane resin |
JP5716668B2 (en) * | 2009-09-30 | 2015-05-13 | 旭硝子株式会社 | Method for producing isocyanate group-terminated prepolymer and method for producing polyurethane resin |
Also Published As
Publication number | Publication date |
---|---|
JP2954604B2 (en) | 1999-09-27 |
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