JPH01316335A - Crystallization of adduct of bisphenol a with phenol - Google Patents
Crystallization of adduct of bisphenol a with phenolInfo
- Publication number
- JPH01316335A JPH01316335A JP1038190A JP3819089A JPH01316335A JP H01316335 A JPH01316335 A JP H01316335A JP 1038190 A JP1038190 A JP 1038190A JP 3819089 A JP3819089 A JP 3819089A JP H01316335 A JPH01316335 A JP H01316335A
- Authority
- JP
- Japan
- Prior art keywords
- phenol
- bisphenol
- crystallizer
- adduct
- temperature
- 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
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 title claims abstract description 50
- 238000002425 crystallisation Methods 0.000 title claims abstract description 8
- 230000008025 crystallization Effects 0.000 title claims abstract description 8
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims abstract description 76
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 39
- 238000000034 method Methods 0.000 claims description 21
- 229920006351 engineering plastic Polymers 0.000 abstract description 2
- 239000003822 epoxy resin Substances 0.000 abstract description 2
- 229920005668 polycarbonate resin Polymers 0.000 abstract description 2
- 239000004431 polycarbonate resin Substances 0.000 abstract description 2
- 229920000647 polyepoxide Polymers 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 239000013078 crystal Substances 0.000 description 16
- 239000007788 liquid Substances 0.000 description 9
- 239000000203 mixture Substances 0.000 description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 238000001704 evaporation Methods 0.000 description 6
- 230000008020 evaporation Effects 0.000 description 6
- 239000006227 byproduct Substances 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 150000002989 phenols Chemical class 0.000 description 4
- 239000011541 reaction mixture Substances 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 239000003377 acid catalyst Substances 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000012452 mother liquor Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 229930185605 Bisphenol Natural products 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 description 1
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明はビスフェノールＡとフェノールとの付加物の晶
出方法に関する。DETAILED DESCRIPTION OF THE INVENTION [Industrial Field of Application] The present invention relates to a method for crystallizing an adduct of bisphenol A and phenol.
更に詳しくは、ビスフェノールＡとフェノールとの付加
物を水の存在下に晶出させる際に、晶析器の内壁面の温
度を内容物の温度よりも高く保つことによって、純度の
高いビスフェノールＡとフェノールとの付加物を得る方
法に関するものである。More specifically, when an adduct of bisphenol A and phenol is crystallized in the presence of water, by keeping the temperature of the inner wall of the crystallizer higher than the temperature of the contents, highly pure bisphenol A and This invention relates to a method for obtaining an adduct with phenol.
ビスフェノールＡはポリカーボネート樹脂やエポキシ樹
脂の他、近年ではエンジニアリングプラスチック等の原
料としての需要が増大している。In addition to polycarbonate resins and epoxy resins, demand for bisphenol A has been increasing in recent years as a raw material for engineering plastics and the like.
これらの用途には無色で高純度のビスフェノールＡが要
求される。Colorless and highly pure bisphenol A is required for these uses.
ビスフェノールＡの製造方法の一つは、酸触媒の存在下
にフェノールとアセトンとを反応させ、該反応混合物か
ら触媒、水および少量のフェノールを除いた後に残った
液状混合物を冷却することによってビスフェノールＡを
フェノールとの付加物として晶出させ、この結晶を母液
から分離し、該付加物からフェノールを除去してビスフ
ェノールＡを回収することからなる。One method for producing bisphenol A is to react phenol with acetone in the presence of an acid catalyst, remove the catalyst, water and a small amount of phenol from the reaction mixture, and then cool the remaining liquid mixture. The process consists of crystallizing the compound as an adduct with phenol, separating the crystals from the mother liquor, and removing phenol from the adduct to recover bisphenol A.
ビスフェノールＡとフェノールとの付加物の晶出方法と
しては、特開昭５８−１３５８３２号公報に開示されて
いるように、水を添加し、その蒸発熱によって結晶化熱
等の除熱を行う方法がある。As a method for crystallizing an adduct of bisphenol A and phenol, as disclosed in JP-A-58-135832, water is added and the heat of crystallization is removed by the heat of evaporation. There is.
この方法は結晶化に伴う熱を内部から取り除く点で、晶
析器内面にスケールが付着しにくいと考えられるが、晶
析器の保温については何もふれていない。This method removes the heat associated with crystallization from the inside, which is thought to make it difficult for scale to adhere to the inner surface of the crystallizer, but there is no mention of keeping the crystallizer warm.
連続晶析における問題点の一つは、晶析器内壁面でのス
ケールの発生である。One of the problems in continuous crystallization is the formation of scale on the inner wall surface of the crystallizer.
スケールが発生すると晶析器の運転を中断しなければな
らず、安定して一定の品質の結晶を生産することができ
ない。When scale occurs, the operation of the crystallizer must be interrupted, making it impossible to stably produce crystals of a certain quality.
晶析における一逓的なスケール発生防止方法としては、
化学工学協会編、化学工学便覧第４版、ｐ、４５３にあ
るように、保温または二重管の外管に熱水を循環させて
、壁面の過飽和度が大になるのを防ぐ方法、壁面に生成
したスケール除去のためにかき取り機で除去する方法ま
たは溶媒添加で溶解する方法がある。As a method to prevent scale generation in crystallization,
As described in Chemical Engineering Handbook, 4th edition, p. 453, edited by the Japan Society of Chemical Engineers, there is a method to prevent the degree of supersaturation on the wall surface from increasing by keeping it warm or circulating hot water through the outer tube of a double tube. There are two methods to remove the scale that is generated: use a scraper to remove it, or dissolve it by adding a solvent.
水を添加して、ビスフェノールＡとフェノールとの付加
物を晶出する際に、前者の方法では、あまりにも温度差
が大きいと蒸発量が多くなり、装置の大型化およびエネ
ルギーのロスにつながる。When adding water to crystallize an adduct of bisphenol A and phenol, in the former method, if the temperature difference is too large, the amount of evaporation increases, leading to an increase in the size of the equipment and energy loss.
また、水の蒸発が激しくなるため、突沸等が起こり、結
晶成長に好ましくない攪乱効果をもたらし、付加物の純
度および粒径の低下をきたす。In addition, water evaporates more intensely, causing bumping and the like, resulting in an unfavorable disturbance effect on crystal growth and a decrease in the purity and particle size of the adduct.
後者の方法の場合には、かき取り機による結晶の破砕の
ため、後の固液分離での分離が困難になり、母液付着に
よる品質の低下、収率の悪化がある。In the case of the latter method, since the crystals are crushed by a scraper, separation in the subsequent solid-liquid separation becomes difficult, and there is a drop in quality and yield due to adhesion of the mother liquor.
溶媒を添加した場合には、回収設備等が必要になり、経
済的ではない。When a solvent is added, recovery equipment etc. are required, which is not economical.
またその溶媒によって、品質低下を招きかねない。Moreover, the solvent may lead to quality deterioration.
本発明の目的は、ビスフェノールＡとフェノールとの付
加物を水の存在下に晶出させる際に、上記問題点のない
、純度の高いビスフェノールＡとフェノールとの付加物
を得ることのできる方法を提供することにある。The object of the present invention is to provide a method that does not have the above-mentioned problems and can obtain a highly pure adduct of bisphenol A and phenol when the adduct of bisphenol A and phenol is crystallized in the presence of water. It is about providing.
本発明者らは、上記目的を達成するために鋭意検討し、
ビスフェノールＡとフェノールとの付加物を水の存在下
に晶出させる際に、晶析器の内壁面の温度を内容物の温
度よりも高く保つことによって本発明の目的が達成され
ることを見出し、ついに本発明を完成させるに到った。The present inventors have made extensive studies to achieve the above objectives,
It has been found that the object of the present invention can be achieved by keeping the temperature of the inner wall of the crystallizer higher than the temperature of the contents when crystallizing an adduct of bisphenol A and phenol in the presence of water. Finally, we have completed the present invention.
即ち、本発明は、ビスフェノールＡとフェノールとの付
加物を、ビスフェノールＡのフェノール溶液から水の存
在下に晶出させる方法において、晶析器内壁面の温度を
内容物の温度よりも高く保ち、かつその温度差が、５℃
以下であることを特徴とするビスフェノールＡとフェノ
ールとの付加物の晶出方法である。That is, the present invention provides a method for crystallizing an adduct of bisphenol A and phenol from a phenol solution of bisphenol A in the presence of water, by maintaining the temperature of the inner wall surface of the crystallizer higher than the temperature of the contents, And the temperature difference is 5℃
This is a method for crystallizing an adduct of bisphenol A and phenol, characterized by the following.
本発明において、晶析器に供給される粗ビスフェノール
Ａのフェノール溶液は、酸触媒の存在下にフェノールと
アセトンとを反応させ、該反応混合物から触媒、水およ
び少量のフェノールを除いた後、残った液状混合物であ
っても良いし、粗ビスフェノールＡをフェノールに溶解
したものであっても良い。In the present invention, the phenol solution of crude bisphenol A supplied to the crystallizer is prepared by reacting phenol with acetone in the presence of an acid catalyst, removing the catalyst, water and a small amount of phenol from the reaction mixture, and then removing the remaining phenol from the reaction mixture. It may be a liquid mixture containing crude bisphenol A, or it may be a mixture of crude bisphenol A dissolved in phenol.
粗ビスフェノールＡのフェノール溶液は晶析器内でゆる
やかに攪拌され、３５〜７０℃の範囲まで冷却され、ビ
スフェノールＡとフェノールとの付加物が晶出する。A phenol solution of crude bisphenol A is gently stirred in a crystallizer and cooled to a temperature in the range of 35 to 70°C to crystallize an adduct of bisphenol A and phenol.
該冷却は、晶析器に添加される水と少量のフェノールの
蒸発による除熱により行われる。The cooling is carried out by heat removal by evaporation of water and a small amount of phenol added to the crystallizer.
蒸留による留出物は水と少量のフェノールとからなり、
循環再使用することができる。The distillate from distillation consists of water and a small amount of phenol.
Can be recycled and reused.
添加される水の量は、粗ビスフェノールＡのフェノール
溶液の冷却に要する熱と、付加物結晶生成の際発生する
結晶化熱を蒸発によって除去するために必要な量で十分
である。The amount of water added is sufficient to remove the heat required for cooling the phenol solution of crude bisphenol A and the heat of crystallization generated during the formation of adduct crystals by evaporation.
これは該フェノール溶液の２〜２０重量％に相当する。This corresponds to 2-20% by weight of the phenol solution.
晶析器は一定の圧力のもとで操作され、内容物の温度は
晶析器に添加される水の量によって制御される。The crystallizer operates under constant pressure and the temperature of the contents is controlled by the amount of water added to the crystallizer.
操作圧力は２０〜１００ｍｄｇが好ましい。The operating pressure is preferably 20 to 100 mdg.
晶析器内壁面の温度を内容物の°温度よりも高く保つ方
法としては、例えば、ジャケット付の晶析器を用い、ジ
ャケット内を温度が制御された温水を通す方法が考えら
れる。As a method of keeping the temperature of the inner wall surface of the crystallizer higher than the temperature of the contents, for example, a method of using a crystallizer with a jacket and passing temperature-controlled hot water through the jacket can be considered.
さらに、本願にしたがって晶析器壁面を保温した場合で
も、晶析器がドラフトチューブタイプの場合にはチュー
ブ表面、特に蒸発面近くに少しずつ結晶の付着がおこり
、長時間の運転が困難になる。このため、チューブ自身
を内部に温水を通せるジャラケット式とし、温度が制御
された温水を通す方法をとることが好ましい。Furthermore, even if the crystallizer wall is kept warm according to the present application, if the crystallizer is a draft tube type, crystals will gradually accumulate on the tube surface, especially near the evaporation surface, making long-term operation difficult. . For this reason, it is preferable to use a method in which the tube itself is of a jacket type that allows hot water to pass through it, and hot water is passed through the tube at a controlled temperature.
この温水の温度が晶析器の内容物の温度よりも低い場合
には、内壁面の過飽和度が大になるため、内壁面で付加
物結晶が成長し、一定期間でスケール除去を行わなけれ
ばならず、安定して操作することができない。If the temperature of this hot water is lower than the temperature of the contents of the crystallizer, the degree of supersaturation on the inner wall surface will increase, and adduct crystals will grow on the inner wall surface, and the scale must be removed at a certain period of time. It cannot be operated stably.
温水の温度と内容物の温度との差は５℃以下である。こ
の差が５℃を越える場合には、気液界面での水の蒸発が
激しくなるため、突沸等が起こり、結晶成長に好ましく
ない撹乱効果をもたらし、付加物の純度および粒径の低
下をきたす。The difference between the temperature of the hot water and the temperature of the contents is 5°C or less. If this difference exceeds 5°C, the evaporation of water at the gas-liquid interface increases, causing bumping, etc., which causes an unfavorable disturbance effect on crystal growth, resulting in a decrease in the purity and particle size of the adduct. .
以下、実施例により本発明の方法を具体的に説明する。 Hereinafter, the method of the present invention will be specifically explained with reference to Examples.
なお１％は特にことわりのない限り、重量％とする。Note that 1% is % by weight unless otherwise specified.
実施例１
フェノールとアセトンとを混合し、これに塩化水素を吹
き込みなから５５℃で８時間環合反応を行った。Example 1 Phenol and acetone were mixed, hydrogen chloride was blown into the mixture, and a ring reaction was carried out at 55° C. for 8 hours.
反応混合物を減圧下に加熱して塩酸および反応で生成し
た水を除去した。The reaction mixture was heated under reduced pressure to remove hydrochloric acid and water produced by the reaction.
この脱塩酸液の組成はビスフェノールＡ３５％、フェノ
ール６３％、副生物２％であった。The composition of this dehydrochloric acid solution was 35% bisphenol A, 63% phenol, and 2% by-product.
二のフェノール溶液を９０℃、４００ｋｇ／ＩＩ？の流
量で、ｓｏｍｍｔ＋ｇで操作されている晶析器に供給し
た。2. Phenol solution at 90℃, 400kg/II? was fed to a crystallizer operating at sommt+g.
晶析器はジャケット付きのものを用い、ジャケットには
５２℃の温水を流した。The crystallizer used was one with a jacket, and 52°C hot water was flowed through the jacket.
晶析器には別の経路を用いて４０ｋｇ／ＩＩＨの割合で
水を添加した。Water was added to the crystallizer using a different route at a rate of 40 kg/IIH.
晶析器の内容物の温度は５０″Ｃで一定となった。The temperature of the contents of the crystallizer remained constant at 50''C.
晶析器の液面を一定に保つように、スラリーを連続的に
抜き取り、連続的に濾過した。The slurry was continuously drawn out and filtered continuously so as to keep the liquid level in the crystallizer constant.
得られたビスフェノールＡとフェノールとの付加物の平
均粒径は０．４ｍｍであり、副生物を０．０５χ含んで
いた。The average particle size of the resulting adduct of bisphenol A and phenol was 0.4 mm, and it contained 0.05x of by-products.
５０χエタノールン容液のハーゼンカラーは５ＡｐＨＡ
であった。The Hazen color of 50χ ethanol solution is 5ApHA.
Met.
また、晶析器内壁面での結晶の成長はみられず、安定し
た運転を行うことができた。Furthermore, no crystal growth was observed on the inner wall surface of the crystallizer, and stable operation was possible.
実施例２
実施例１と同様の方法でビスフェノールへのフェノール
溶液を調製した。Example 2 A phenol solution in bisphenol was prepared in the same manner as in Example 1.
フェノール溶液の組成は実施例１に記載されたものと同
一であった。The composition of the phenol solution was the same as described in Example 1.
このフェノール溶液を９０℃，４００ｋｇ／ＨＲの流量
で、５０ｍｍ１１ｇで操作されているドラフトチューブ
タイプの晶析器（月島機械■製、ＤＰ型晶析器）に供給
した。This phenol solution was supplied at 90° C. and a flow rate of 400 kg/HR to a draft tube type crystallizer (manufactured by Tsukishima Kikai ■, DP type crystallizer) operated at 50 mm and 11 g.
晶析器はジャケット付きのものを用い、ジャケットには
５２℃の温水を流した。また、チューブ部分にも同温度
の温水を流した。The crystallizer used was one with a jacket, and 52°C hot water was flowed through the jacket. Warm water at the same temperature was also poured into the tube.
晶析器には別の経路を用いて４０ｋｇ／ＨＲの割合で水
を添加した。Water was added to the crystallizer using a different route at a rate of 40 kg/HR.
晶析器の内容物の温度は５０℃で一定となった。The temperature of the contents of the crystallizer remained constant at 50°C.
晶析器の液面を一定に保つように、スラリーを連続的に
抜き取り、連続的に濾過した。The slurry was continuously drawn out and filtered continuously so as to keep the liquid level in the crystallizer constant.
得られたビスフェノールＡとフェノールとの付加物の平
均粒径は０．５ｍｍであり、副生物を０．０４χ含んで
いた。The resulting adduct of bisphenol A and phenol had an average particle size of 0.5 mm and contained 0.04x of by-products.
５０Ｘエタノール溶液のハーゼンカラーは５ＡＰＨＡで
あった。The Hazen color of the 50X ethanol solution was 5APHA.
また、晶析器内壁面での結晶の成長はみられず、安定し
た運転を行うことができた。Furthermore, no crystal growth was observed on the inner wall surface of the crystallizer, and stable operation was possible.
比較例１
実施例１と同様の方法でビスフェノールＡのフェノール
溶液を調製した。Comparative Example 1 A phenol solution of bisphenol A was prepared in the same manner as in Example 1.
フェノール溶液の組成は実施例１に記載されたものと同
一であった。The composition of the phenol solution was the same as described in Example 1.
このフェノール溶液を９０℃、４００ｋｇ／ＩＩＨの流
量で、５０ｆｆｌＩＩＩＨｇで操作されている晶析器に
供給した。This phenol solution was fed to a crystallizer operating at 90° C. and 50 fflIIIHg at a flow rate of 400 kg/IIH.
晶析器はジャケット付きのものを用い、ジャケットには
４８℃の温水を流した。The crystallizer used was one with a jacket, and 48°C hot water was flowed through the jacket.
晶析器には別の経路を用いて３５ｋｇ／ＨＲの割合で水
を添加したところ、晶析器の内容物の温度は５０℃で一
定となった。Water was added to the crystallizer at a rate of 35 kg/HR using a different route, and the temperature of the crystallizer contents remained constant at 50°C.
一週間で晶析器内壁面で結晶に成長し、巨大な塊となり
、連続運転が不可能になった。Within a week, crystals had grown on the inner wall of the crystallizer, forming a huge lump, making continuous operation impossible.
比較例２
実施例１と同様の方法でビスフェノールＡのフェノール
溶液を調製した。Comparative Example 2 A phenol solution of bisphenol A was prepared in the same manner as in Example 1.
フェノール溶液の組成は実施例１に記載されたものと同
一であった。The composition of the phenol solution was the same as described in Example 1.
このフェノール溶液を９０℃、 ４００ｋｇ／ＨＲのｆ
Ｌ量で、５０ｍｍＨｇで操作されている実施例２と同一
の晶析器に供給した。This phenol solution was heated at 90°C and at a rate of 400 kg/HR.
L quantities were fed into the same crystallizer as in Example 2, operating at 50 mmHg.
晶析器はジャケット付きのものを用い、ジャケントには
４８℃の温水を流した。チューブ部分への温水の導入は
おこなわなかった。A jacketed crystallizer was used, and 48°C hot water was flowed through the jacket. Hot water was not introduced into the tube section.
晶析器には別の経路を用いて３５ｋｇ／ＩＩＲの割合で
水を添加したところ、晶析器の内容物の温度は５０℃で
一定となった。Water was added to the crystallizer at a rate of 35 kg/IIR using a different route, and the temperature of the crystallizer contents remained constant at 50°C.
一週間で晶析器内壁面での結晶成長はみられなかったが
、チューブ上部に結晶が成長し、巨大な塊となり、内部
の液の循環ができなり連続運転が不可能になった。Although no crystal growth was observed on the inner wall of the crystallizer within a week, crystals grew in the upper part of the tube and formed a huge lump, which prevented the circulation of the liquid inside and made continuous operation impossible.
比較例３
実施例１と同様の方法でビスフェノールＡのフェノール
溶液を調製した。Comparative Example 3 A phenol solution of bisphenol A was prepared in the same manner as in Example 1.
フェノール溶液の組成は実施例１に記載されたものと同
一である。The composition of the phenol solution is the same as described in Example 1.
このフェノール溶液を９０℃、４００ｋｇ／）ＩＲの流
量で、５０ｍｍ）Ｉｇで操作されている晶析器に供給し
た。This phenol solution was fed at 90° C. and a flow rate of 400 kg/) IR to a crystallizer operating on 50 mm) Ig.
晶析器はジャケット付きのものを用い、ジャケットには
５７℃の温水を流した。The crystallizer used was one with a jacket, and 57°C hot water was flowed through the jacket.
晶析器には別の経路を用いて５０ｋｇ／ＨＲの割合で水
を添加したところ、晶析器の内容物の温度は５０℃で一
定となった。Water was added to the crystallizer at a rate of 50 kg/HR using a different route, and the temperature of the contents of the crystallizer remained constant at 50°C.
スケール発生はなかったが、液中で激しく水が突沸し、
攪拌が乱された。Although there was no scale formation, the water violently bumped in the liquid,
The stirring was disturbed.
晶析器の液面を一定に保つように、スラリーを連続的に
抜き取ったところ、微細結晶を多く含み、結晶の平均粒
径は０．２ｍｍであった。When the slurry was continuously drawn out while keeping the liquid level in the crystallizer constant, it was found that it contained many fine crystals and the average grain size of the crystals was 0.2 mm.
連続的に濾過したところ、得られた結晶には副生物が０
．２％含まれていた。After continuous filtration, the resulting crystals contained zero by-products.
．． It contained 2%.
５０％エタノールン容液のハーゼンカラーは３０ＡＰＩ
ＩＡであった。Hazen color of 50% ethanol solution is 30 API
It was IA.
本発明は上記した構成をとるので、ビスフェノールＡと
フェノールとの付加物を水の存在下に晶出する際に、安
定して操作することができ、しかも純度の高い付加物を
得ることができる。Since the present invention has the above-described configuration, when an adduct of bisphenol A and phenol is crystallized in the presence of water, the operation can be performed stably and an adduct with high purity can be obtained. .
特許出願人 三井東圧化学株式会社Patent applicant: Mitsui Toatsu Chemical Co., Ltd.
Claims (1)
フェノールＡのフェノール溶液から水の存在下に晶出さ
せる方法において、晶析器内壁面の温度を内容物の温度
よりも高く保ち、かつその温度差が、５℃以下であるこ
とを特徴とするビスフェノールＡとフェノールとの付加
物の晶出方法。 ２、ビスフェノールＡとフェノールとの付加物を、ビス
フェノールＡのフェノール溶液から水の存在下に晶出さ
せる方法において、ドラフトチューブタイプの晶析器を
用いて晶析を行い、その際に晶析器内壁面およびドラフ
トチューブ壁面の温度を内容物の温度よりも高く保ち、
かつその温度差が、５℃以下であることを特徴とするビ
スフェノールＡとフェノールとの付加物の晶出方法。[Claims] 1. In a method for crystallizing an adduct of bisphenol A and phenol from a phenol solution of bisphenol A in the presence of water, the temperature of the inner wall surface of the crystallizer is higher than the temperature of the contents. A method for crystallizing an adduct of bisphenol A and phenol, characterized in that the temperature difference is 5°C or less. 2. In a method of crystallizing an adduct of bisphenol A and phenol from a phenol solution of bisphenol A in the presence of water, crystallization is performed using a draft tube type crystallizer, and at that time, the crystallizer Maintains the temperature of the inner wall surface and draft tube wall surface higher than the temperature of the contents,
A method for crystallizing an adduct of bisphenol A and phenol, characterized in that the temperature difference is 5°C or less.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3819089A JPH07107006B2 (en) | 1988-02-22 | 1989-02-20 | Method for crystallizing adduct of bisphenol A and phenol |
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63-37520 | 1988-02-22 | ||
| JP3752088 | 1988-02-22 | ||
| JP3819089A JPH07107006B2 (en) | 1988-02-22 | 1989-02-20 | Method for crystallizing adduct of bisphenol A and phenol |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH01316335A true JPH01316335A (en) | 1989-12-21 |
| JPH07107006B2 JPH07107006B2 (en) | 1995-11-15 |
Family
ID=26376642
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP3819089A Expired - Lifetime JPH07107006B2 (en) | 1988-02-22 | 1989-02-20 | Method for crystallizing adduct of bisphenol A and phenol |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH07107006B2 (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1992003400A1 (en) * | 1990-08-21 | 1992-03-05 | Mitsui Toatsu Chemicals, Inc. | Method of crystallizing bisphenol a having phenol added thereto |
| JP2003511429A (en) * | 1999-10-12 | 2003-03-25 | ゼネラル・エレクトリック・カンパニイ | Bisphenol prereactor cleaning method |
| WO2011115136A1 (en) * | 2010-03-16 | 2011-09-22 | 三菱化学株式会社 | Method for producing succinic acid |
-
1989
- 1989-02-20 JP JP3819089A patent/JPH07107006B2/en not_active Expired - Lifetime
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1992003400A1 (en) * | 1990-08-21 | 1992-03-05 | Mitsui Toatsu Chemicals, Inc. | Method of crystallizing bisphenol a having phenol added thereto |
| US5245088A (en) * | 1990-08-21 | 1993-09-14 | Mitsui Toatsu Chemicals, Inc. | Process for crystallizing adduct of bisphenol a with phenol |
| JP2003511429A (en) * | 1999-10-12 | 2003-03-25 | ゼネラル・エレクトリック・カンパニイ | Bisphenol prereactor cleaning method |
| JP4902920B2 (en) * | 1999-10-12 | 2012-03-21 | サビック・イノベーティブ・プラスチックス・アイピー・ベスローテン・フェンノートシャップ | Cleaning method of bisphenol pre-reactor |
| WO2011115136A1 (en) * | 2010-03-16 | 2011-09-22 | 三菱化学株式会社 | Method for producing succinic acid |
| JPWO2011115136A1 (en) * | 2010-03-16 | 2013-06-27 | 三菱化学株式会社 | Method for producing succinic acid |
| US9035095B2 (en) | 2010-03-16 | 2015-05-19 | Mitsubishi Chemical Corporation | Processes for producing succinic acid |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH07107006B2 (en) | 1995-11-15 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US4354046A (en) | Process for obtaining high purity bisphenol A | |
| JP5030472B2 (en) | Manufacturing method and manufacturing equipment of high purity bisphenol A | |
| KR910003868B1 (en) | Process for crystallizing adduct of bisphenola with phenol | |
| JP2604333B2 (en) | Novel λ-modified crystal of pentaerythritol tetrakis- [3- (3,5-di-tert-butyl-4-hydroxyphenyl) propionate] and a method for producing the same | |
| JP2016020370A (en) | Recovery and refining of dianhydrosugar | |
| US4927973A (en) | Process for continuous purification of bisphenols | |
| JPH01316335A (en) | Crystallization of adduct of bisphenol a with phenol | |
| JPS6326735B2 (en) | ||
| JPH075543B2 (en) | Method for producing high-purity caprolactam | |
| JP2000327614A (en) | Production of bisphenol a | |
| US3649686A (en) | Continuous process for the preparation of acylsulfanilyl chloride | |
| EP0081063A1 (en) | Method for producing sodium persulfate | |
| EP2374786A1 (en) | Purification of monochloroacetic acid rich streams | |
| JP3674010B2 (en) | Process for producing paraphenylene diisocyanate | |
| US4568776A (en) | Process for purifying 2,6-xylenol | |
| JPH0361605B2 (en) | ||
| JP2623344B2 (en) | Method for separation and purification of β-monoisopropylnaphthalene | |
| US6011184A (en) | Descaling of bisphenol-A reactor using water | |
| JPH03284641A (en) | Production of bisphenol a | |
| JPWO2004085357A1 (en) | Method for producing bisphenol A | |
| JPS62138443A (en) | Production of biscresol | |
| US4382896A (en) | Process for producing 4,4'-diphenyldisulfonic acid and its monopotassium salt | |
| JP4552418B2 (en) | Method for producing bisphenol A | |
| JPH07291879A (en) | Method for crystallizing adduct of bisphenol a and phenol | |
| JPH0544933B2 (en) |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20071115 Year of fee payment: 12 |
|
| R154 | Certificate of patent or utility model (reissue) |
Free format text: JAPANESE INTERMEDIATE CODE: R154 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20081115 Year of fee payment: 13 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20091115 Year of fee payment: 14 |
|
| EXPY | Cancellation because of completion of term | ||
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20091115 Year of fee payment: 14 |