JPH0425938B2 - - Google Patents
Info
- Publication number
- JPH0425938B2 JPH0425938B2 JP59164300A JP16430084A JPH0425938B2 JP H0425938 B2 JPH0425938 B2 JP H0425938B2 JP 59164300 A JP59164300 A JP 59164300A JP 16430084 A JP16430084 A JP 16430084A JP H0425938 B2 JPH0425938 B2 JP H0425938B2
- Authority
- JP
- Japan
- Prior art keywords
- tpa
- terephthalic acid
- acid
- waste liquid
- activated carbon
- 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 - Lifetime
Links
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims description 69
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 24
- 239000007788 liquid Substances 0.000 claims description 22
- 239000002699 waste material Substances 0.000 claims description 21
- 239000002253 acid Substances 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 239000000706 filtrate Substances 0.000 claims description 5
- 229920000728 polyester Polymers 0.000 claims description 5
- 239000012209 synthetic fiber Substances 0.000 claims description 5
- 229920002994 synthetic fiber Polymers 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 230000003472 neutralizing effect Effects 0.000 claims 2
- 238000005406 washing Methods 0.000 claims 2
- 230000002378 acidificating effect Effects 0.000 description 7
- 239000005725 8-Hydroxyquinoline Substances 0.000 description 3
- 238000000975 co-precipitation Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 229960003540 oxyquinoline Drugs 0.000 description 3
- MCJGNVYPOGVAJF-UHFFFAOYSA-N quinolin-8-ol Chemical compound C1=CN=C2C(O)=CC=CC2=C1 MCJGNVYPOGVAJF-UHFFFAOYSA-N 0.000 description 3
- 239000013078 crystal Substances 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- FJNCXZZQNBKEJT-UHFFFAOYSA-N 8beta-hydroxymarrubiin Natural products O1C(=O)C2(C)CCCC3(C)C2C1CC(C)(O)C3(O)CCC=1C=COC=1 FJNCXZZQNBKEJT-UHFFFAOYSA-N 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
- Y02P70/62—Manufacturing or production processes characterised by the final manufactured product related technologies for production or treatment of textile or flexible materials or products thereof, including footwear
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Description
〔産業上の利用分野〕
ポリエステル系合成繊維の製造工程中に生じる
テレフタル酸含有アルカリ性廃液より高純度のテ
レフタル酸を回収する方法に関するものである。
〔従来の技術〕
テレフタル酸含有アルカリ性廃液を酸性にして
テレフタル酸を析出させ、結晶をろ別後乾燥して
回収している。
〔発明が解決しようとする問題点〕
ポリエステル系合成繊維の製造工程中に生じる
廃液には主原料であるテレフタル酸がかなりの量
含まれており、その回収は製造コスト及び廃液処
理上の重要な課題である。
しかしながら上記廃液中にはテレフタル酸以外
に触媒や顔料として使用した金属イオン、金属酸
化物や有機高分子化合物等の不純物が含まれる為
実用に供しうる高純度テレフタル酸の回収は容易
ではない。
〔問題点を解決するための手段〕
本発明者等はポリエステル系合成繊維の製造工
程で生じるテレフタル酸含有アルカリ性廃液を酸
でPH４〜６の弱酸性とし、テレフタル酸のごく一
部を析出させ、ろ過後、ろ液からテレフタル酸を
回収（酸性にして結晶をろ別）することにより高
純度品を得ることを見い出した。弱酸性で析出す
るごく一部のテレフタル酸は損失することになる
が、上記の不純物はテレフタル酸と共沈して除去
される。更にこの不純物と共沈したテレフタル酸
のろ別時に活性炭、好ましくは８−ヒドロキシキ
ノリン添着活性炭を使用すると一層高純度品が得
られた。
〔作用〕
従来の技術ａ、ｂ、ｃと本発明ｄ、ｅを比較す
ると次の通りであつた。
以下テレフタル酸をTPAと略記する。
ａ TPA廃液 酸性晶析
――――→ 回収TPA（灰分0.23％）
ｂ TPA廃液 活性炭ろ過
―――――→
酸性晶析
――――→
回収TPA（灰分0.20％）
ｃ TPA廃液 ８−ヒドロキシキノリン添着活性炭ろ過
――――――――――――――――――――――→
酸性晶析
――――→
回収TPA（灰分0.18％）
ｄ TPA廃液 弱酸共沈ろ過
―――――――→
酸性晶析
――――→
回収TPA（灰分0.03％）
ｅ TPA廃液 弱酸共沈８−ヒドロキシキノリン添着活
性炭ろ過
ｅ TPA廃液 弱酸共沈８−ヒドロキシキノリン添着活
性炭ろ過
―――――――――――――――――――――――――
―→
酸性晶析
――――→
回収TPA（灰分0.01％）
〔実施例〕
尚、実施例１〜４は比較のために示すものであ
り、本発明の実施例ではない。
実施例 １
TPA廃液5.0KgをHClにてPH2.0としTPAを析
出させる。このものをNo.5Cろ紙にてろ過し、ろ
過後イオン交換水500mlにて洗浄後乾燥する。
実施例 ２
TPA廃液5.0Kgに活性炭10ｇを投入し撹拌後、
No.5Cろ紙にてろ過する。このろ液をHClにてPH
2.0としTPAを析出させる。以降実施例１と同様
に操作する。
実施例 ３
TPA廃液5.0Kgに８−ヒドロキシキノリン添着
活性炭10ｇを投入し撹拌後、No.5Cろ紙にてろ過
する。このろ液をHClにてPH2.0としTPAを析出
させる。以降実施例１と同様に操作する。
実施例 ４
TPA廃液5.0KgをHClにてPH5.4となしTPAの
一部を析出させ、No.5Cろ紙にてろ過する。この
ろ液を更にHClにてPH2.0としTPAを析出させる。
以降実施例１と同様に操作する。
実施例 ５
TPA廃液5.0KgをHClにてPH5.1となしTPAの
一部を析出させNo.5Cろ紙にてろ過する。以降実
施例４と同様に操作する。
実施例 ６
TPA廃液5.0KgをHClにてPH5.4となしTPAの
一部を析出させた後、活性炭10ｇを投入し撹拌後
No.5Cろ紙にてろ過する。以降実施例４と同様に
操作する。
実施例 ７
TPA廃液5.0KgをHClにてPH5.4となしTPAの
一部を析出させた後、８−ヒドロキシキノリン添
着活性炭10ｇを投入し撹拌後、No.5Cろ紙にてろ
過する。以降実施例４と同様に操作する。
〔発明の効果〕
実施例１〜７の分析結果を以下に表記する。
[Industrial Application Field] The present invention relates to a method for recovering highly purified terephthalic acid from terephthalic acid-containing alkaline waste liquid produced during the manufacturing process of polyester synthetic fibers. [Prior Art] A terephthalic acid-containing alkaline waste liquid is acidified to precipitate terephthalic acid, and the crystals are filtered and then dried and recovered. [Problem to be solved by the invention] The waste liquid generated during the manufacturing process of polyester synthetic fibers contains a considerable amount of terephthalic acid, which is the main raw material, and its recovery is an important issue in terms of manufacturing costs and waste liquid treatment. This is a challenge. However, since the waste liquid contains impurities such as metal ions, metal oxides, and organic polymer compounds used as catalysts and pigments in addition to terephthalic acid, it is not easy to recover high-purity terephthalic acid that can be used for practical purposes. [Means for solving the problem] The present inventors made the terephthalic acid-containing alkaline waste liquid generated in the manufacturing process of polyester synthetic fibers weakly acidic with pH 4 to 6 with acid, and precipitated a small portion of the terephthalic acid. It was discovered that a highly pure product could be obtained by recovering terephthalic acid from the filtrate after filtration (by making it acidic and filtering out the crystals). Although a small portion of the terephthalic acid that precipitates under weak acidity is lost, the above impurities are coprecipitated with the terephthalic acid and removed. Further, when activated carbon, preferably activated carbon impregnated with 8-hydroxyquinoline, was used to filter out the terephthalic acid co-precipitated with these impurities, a product with even higher purity was obtained. [Operation] A comparison between conventional techniques a, b, and c and the present inventions d and e was as follows. Terephthalic acid will be abbreviated as TPA below. a TPA waste liquid Acidic crystallization――――→ Recovered TPA (ash content 0.23%) b TPA waste liquid Activated carbon filtration――――――→ Acidic crystallization――――→ Recovered TPA (ash content 0.20%) c TPA waste liquid 8-Hydroxy Quinoline-impregnated activated carbon filtration――――――――――――――――――――→ Acidic crystallization――――→ Recovered TPA (ash content 0.18%) d TPA waste liquid Weak acid coprecipitation filtration― ――――――→ Acidic crystallization――――→ Recovered TPA (ash content 0.03%) e TPA waste liquid Weak acid coprecipitation 8-hydroxyquinoline impregnated activated carbon filtration e TPA waste liquid Weak acid coprecipitation 8-hydroxyquinoline impregnated activated carbon filtration―― ――――――――――――――――――――――
-→ Acidic crystallization ----→ Recovered TPA (ash content 0.01%) [Example] Examples 1 to 4 are shown for comparison, and are not examples of the present invention. Example 1 5.0 kg of TPA waste liquid was adjusted to pH 2.0 with HCl to precipitate TPA. This material is filtered using No. 5C filter paper, and after filtration, it is washed with 500 ml of ion-exchanged water and dried. Example 2 10g of activated carbon was added to 5.0Kg of TPA waste liquid and after stirring,
Filter with No.5C filter paper. PH this filtrate with HCl.
2.0 and precipitate TPA. Thereafter, operations are performed in the same manner as in Example 1. Example 3 10 g of 8-hydroxyquinoline-impregnated activated carbon was added to 5.0 kg of TPA waste liquid, stirred, and then filtered using No. 5C filter paper. This filtrate was adjusted to pH 2.0 with HCl to precipitate TPA. Thereafter, operations are performed in the same manner as in Example 1. Example 4 5.0 kg of TPA waste liquid was adjusted to pH 5.4 with HCl to precipitate a portion of TPA, and filtered through No. 5C filter paper. This filtrate was further adjusted to pH 2.0 with HCl to precipitate TPA.
Thereafter, operations are performed in the same manner as in Example 1. Example 5 5.0 kg of TPA waste liquid was adjusted to pH 5.1 with HCl to precipitate a portion of TPA, and filtered through No. 5C filter paper. Thereafter, operations are performed in the same manner as in Example 4. Example 6 5.0 kg of TPA waste liquid was adjusted to pH 5.4 with HCl to precipitate a part of TPA, then 10 g of activated carbon was added and stirred.
Filter with No.5C filter paper. Thereafter, operations are performed in the same manner as in Example 4. Example 7 After adjusting the pH of 5.0 kg of TPA waste liquid to 5.4 with HCl to precipitate a portion of TPA, 10 g of 8-hydroxyquinoline-impregnated activated carbon was added, stirred, and filtered using No. 5C filter paper. Thereafter, operations are performed in the same manner as in Example 4. [Effects of the Invention] The analysis results of Examples 1 to 7 are described below.
【表】
この表から分るように本発明の実施例４〜７で
高純度テレフタル酸が回収された。[Table] As seen from this table, high purity terephthalic acid was recovered in Examples 4 to 7 of the present invention.
Claims (1)
テレフタル酸含有アルカリ性廃液を酸で中和後、
更に弱酸性としてテレフタル酸を一部分析出さ
せ、ろ過後ろ液を酸にて更に酸性とし、析出した
テレフタル酸をろ過後水洗して回収する方法。 ２ ポリエステル系合成繊維の製造工程で生じる
テレフタル酸含有アルカリ性廃液を酸で中和後、
更に弱酸性としてテレフタル酸を一部分析出さ
せ、活性炭または８−ヒドロキシキノリン添着活
性炭でろ過後、ろ液を酸にて更に酸性とし、析出
したテレフタル酸をろ過後水洗して回収する方
法。[Claims] 1. After neutralizing terephthalic acid-containing alkaline waste liquid generated in the manufacturing process of polyester synthetic fibers with acid,
A method in which a portion of terephthalic acid is further analyzed as a weak acid, the filtrated liquid is further acidified with acid, and the precipitated terephthalic acid is recovered by washing with water after filtration. 2 After neutralizing the terephthalic acid-containing alkaline waste liquid generated in the manufacturing process of polyester synthetic fibers with acid,
A method in which a portion of terephthalic acid is further analyzed as a weak acid, and after filtration with activated carbon or 8-hydroxyquinoline-impregnated activated carbon, the filtrate is further acidified with an acid, and the precipitated terephthalic acid is recovered by washing with water after filtration.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP59164300A JPS6143140A (en) | 1984-08-07 | 1984-08-07 | Method of recovering high-purity terepthalic acid from terephthalic acid-containing waste liquir |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP59164300A JPS6143140A (en) | 1984-08-07 | 1984-08-07 | Method of recovering high-purity terepthalic acid from terephthalic acid-containing waste liquir |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6143140A JPS6143140A (en) | 1986-03-01 |
| JPH0425938B2 true JPH0425938B2 (en) | 1992-05-06 |
Family
ID=15790496
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP59164300A Granted JPS6143140A (en) | 1984-08-07 | 1984-08-07 | Method of recovering high-purity terepthalic acid from terephthalic acid-containing waste liquir |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6143140A (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH078822B2 (en) * | 1986-05-26 | 1995-02-01 | 三菱レイヨン株式会社 | Phthalic acid recovery method |
| CN102583813B (en) * | 2012-01-12 | 2013-11-13 | 江苏爱特恩高分子材料有限公司 | Recovery method for terephthalic acid in alkali deweighting wastewater as well as production method and application of terephthalic acid metal salt whisker |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6143139A (en) * | 1984-08-03 | 1986-03-01 | Mitsubishi Chem Ind Ltd | Method of recovering terephthalic acid |
-
1984
- 1984-08-07 JP JP59164300A patent/JPS6143140A/en active Granted
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6143139A (en) * | 1984-08-03 | 1986-03-01 | Mitsubishi Chem Ind Ltd | Method of recovering terephthalic acid |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS6143140A (en) | 1986-03-01 |
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