CN1257064A - Process for recovering terephthalic acid from alkali reduced sewage - Google Patents
Process for recovering terephthalic acid from alkali reduced sewage Download PDFInfo
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- CN1257064A CN1257064A CN 99124266 CN99124266A CN1257064A CN 1257064 A CN1257064 A CN 1257064A CN 99124266 CN99124266 CN 99124266 CN 99124266 A CN99124266 A CN 99124266A CN 1257064 A CN1257064 A CN 1257064A
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Abstract
The present invention relates to a technological process for recovering terephthalic acid by using polyester fibre hydrolytic sewage in textile industry-alkali-decreased sewage as raw material, and includes the following steps: adding flocculating agent to make flocculation, microporous filtering, then acid-separating to make terephthalic acid precipitate in the form of solid phase, further solid-liquid separating and evaporating to dryness to obtain the terephthalic acid product whose purity is greather than 98%. As compared with existent technology, it not only can recover high-purity terephthalic acid to make up for acid precipitation cost, but also can reduce COD value of sewage so as to attain the goal of controlling sewage.
Description
The present invention relates to the textile sewage processing technology field.
Alkali reduced sewage is that textile industry is to polyester fabric (raw material: the industrial sewage of alkaline hydrolysis polyethylene terephthalate), the COD value is generally 8000～12000, it mainly contains para-phthalic sodium and ethylene glycol, because para-phthalic sodium is the benzene ring structure molecule, therefore difficultly handled by biochemical process cheaply, this for a long time sewage is never effectively administered.Chinese patent 97106539 discloses a kind of " alkali decrement process for waste water processing ", and it is to add trivalent iron salt in waste water, and uses acid for adjusting pH value, and terephthalic acid is separated out with solid-state, thereby reduces the COD value of waste water.The general COD value of this method can reduce by 70～80%, but terephthalic acid simply to separate out impurity a lot, the raw material back of can't regenerating utilizes, and can cause pollute the second time of solid waste on the contrary; Simultaneously, the acid out cost is very high, and general enterprise is difficult to bear.
Purpose of the present invention is exactly to provide a kind of processing method that reclaims terephthalic acid from alkali reduced sewage for the defective that overcomes above-mentioned prior art existence, and it can reclaim highly purified terephthalic acid, can reach the purpose of administering sewage again.
Purpose of the present invention can realize in the following manner: a kind of processing method that reclaims terephthalic acid from alkali reduced sewage, it adopts following processing step: at first alkali reduced sewage is collected to water collecting basin by the workshop and carries out homogenizing, enter mixing tank then, in mixing tank, add aluminium salt medicament, and the pH value of sewage transferred to 7～9, the alumine hydroxide colloid that the produce this moment mechanical impurity in the sewage that promptly can flocculate, again with this mixed solution through the settling vessel gravity settling, supernatant liquor is again through the millipore filter ultrafiltration, further remove remaining tiny mechanical impurity, this solution adds acid and carries out acid out in the acid out groove, and constantly stir, be that the adularescent terephthalic acid crystals is separated out, mixed solution behind acid out separates through solid-liquid separator again, with the solid formation after the dehydration is that terephthalic acid evaporation drying in 105 ℃～230 ℃ moisture eliminators is removed residual solvent, can obtain purity greater than 98% terephthalate product.
Described aluminium salt medicament is to be selected from wherein a kind of in Tai-Ace S 150, polymerize aluminum chloride, the alum.
The acid of described acid out process using is to be selected from wherein a kind of in sulfuric acid, nitric acid, hydrochloric acid, the acetic acid.
Described acid out technology adds the acid out groove with concentration less than 50% diluted acid.
Described acid out technology adds the acid out groove in concentrated acid atomize mode.
Described solid-liquid separator adopts gravity separator or middle fluid centrifuge separator.
Described moisture eliminator adopts fluid bed dryer.
The drying temperature of described moisture eliminator be 210 ℃～230 ℃ preferable.
Compared with prior art, the present invention is owing to adopted the processing method that adds flocculation agent and removal of impurities before adding acid, make that to add the terephthalic acid purity that acid out goes out very high, therefore the present invention not only has been recovered to highly purified terephthalic acid, making it become useful industrial chemicals is utilized again, thereby remedied the acid out cost, and reduced the COD value of sewage again, reached the purpose of administering sewage.
Accompanying drawing is a process flow sheet of the present invention.
Below in conjunction with drawings and the specific embodiments, the present invention is described in further detail.
Alkali reduced sewage is collected to water collecting basin by the workshop, with the homogenizing concentration of wastewater, sewage adds aluminium salt medicament in mixing tank, the pH value of sewage is transferred to 8 ± 0.5, the aluminium hydroxide gel that produce this moment is known from experience the mechanical impurity in the flocculation sewage, as: the organic oil pollutent, titanium dioxide, spinning, the agent mixture that weaving process adds etc., mixed solution is through the settling vessel gravity settling, supernatant liquor is again through the millipore filter ultrafiltration, and to remove remaining tiny mechanical impurity, the sewage of this moment has become the stoste that only contains water-soluble impurity, this stoste adds sulfuric acid and carries out acid out in the acid out groove, be that the adularescent terephthalic acid crystals is separated out, make the terephthalic acid transposition generate phthalic acid or m-phthalic acid for preventing the localized hyperthermia that the sulfuric acid dehydration produces, sulfuric acid needs to add with diluted acid or concentrated acid atomize mode.Mixed solution behind acid out carries out solid-liquid separation through gravity separator or middle fluid centrifuge separator again, to reduce of the absorption of aqueous solution impurity at terephthaldehyde's acid surfaces, through the evaporation drying in 210 ℃～230 ℃ fluid bed dryers of the terephthalic acid after the above-mentioned dehydration, remove residual solvent, the purity that can obtain main contains sodium sulfate ash is greater than 98% terephthalate product.
Embodiment 1
The polyester filament alkali decrement waste water 1m of PH12.1
3, add 10% concentration Tai-Ace S 150 medicament, make the waste water pH value reduce to 8.3, through 2 hours gravity settlings, with 1 μ m polytetrafluoroethylene microporous pipe pressure filtration, clear liquid was 20% sulfuric acid acid out through concentration, the terephthalic acid white crystal is separated out immediately, obtains terephthalate product through dehydrating.
Embodiment 2
The emulation blended fabric of silk and polyester lining alkali decrement waste water 0.5m of PH11.5
3, add the Tai-Ace S 150 medicament of 5% concentration, make the waste water pH value transfer to 7.8, through sedimentation in 1.5 hours, supernatant liquor with 2 μ m tubular ceramic membranes filter, clear liquid drips through 98% the vitriol oil and analyses, the terephthalic acid white crystal is separated out immediately, through dehydrating, promptly get terephthalic acid white crystal product.
Embodiment 3
The dacron short silk lining of PH12, alkali reduced sewage is with 4m
3/ h treatment capacity is moved at pilot plant; Sewage through the smart filter of planar ceramic membrane strainer, is 98% acetic acid acid out through 5% Tai-Ace S 150 medicament flocculation sediment through concentration again, and terephthalic acid crystals is separated out immediately, through dehydration, drying, promptly gets terephthalate product.
Claims (8)
1. processing method that from alkali reduced sewage, reclaims terephthalic acid, it is characterized in that, it adopts following processing step: at first alkali reduced sewage is collected to water collecting basin by the workshop and carries out homogenizing, enter mixing tank then, in mixing tank, add aluminium salt medicament, and the pH value of sewage transferred to 7～9, the alumine hydroxide colloid that the produce this moment mechanical impurity in the sewage that promptly can flocculate, again with this mixed solution through the settling vessel gravity settling, supernatant liquor is again through the millipore filter ultrafiltration, further remove remaining tiny mechanical impurity, this solution adds acid and carries out acid out in the acid out groove, and constantly stir, be that the adularescent terephthalic acid crystals is separated out, mixed solution behind acid out separates through solid-liquid separator again, is that terephthalic acid evaporation drying in 105 ℃～230 ℃ moisture eliminators is removed residual solvent with the solid formation after the dehydration, can obtain purity greater than 98% terephthalate product.
2. a kind of processing method that reclaims terephthalic acid from alkali reduced sewage according to claim 1 is characterized in that: described aluminium salt medicament is to be selected from wherein a kind of in Tai-Ace S 150, polymerize aluminum chloride, the alum.
3. a kind of processing method that reclaims terephthalic acid from alkali reduced sewage according to claim 1 is characterized in that: the acid of described acid out process using is to be selected from wherein a kind of in sulfuric acid, nitric acid, hydrochloric acid, the acetic acid.
4. a kind of processing method that reclaims terephthalic acid from alkali reduced sewage according to claim 1 is characterized in that: described acid out technology adds the acid out groove with concentration less than 50% diluted acid.
5. a kind of processing method that reclaims terephthalic acid from alkali reduced sewage according to claim 1, it is characterized in that: described acid out technology adds the acid out groove in concentrated acid atomize mode.
6. a kind of processing method that reclaims terephthalic acid from alkali reduced sewage according to claim 1, it is characterized in that: described solid-liquid separator adopts gravity separator or middle fluid centrifuge separator.
7. a kind of processing method that reclaims terephthalic acid from alkali reduced sewage according to claim 1, it is characterized in that: described moisture eliminator adopts fluid bed dryer.
8. a kind of processing method that reclaims terephthalic acid from alkali reduced sewage according to claim 1 is characterized in that: the drying temperature of described moisture eliminator be 210 ℃～230 ℃ preferable.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 99124266 CN1257064A (en) | 1999-12-16 | 1999-12-16 | Process for recovering terephthalic acid from alkali reduced sewage |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 99124266 CN1257064A (en) | 1999-12-16 | 1999-12-16 | Process for recovering terephthalic acid from alkali reduced sewage |
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| CN1257064A true CN1257064A (en) | 2000-06-21 |
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| CN 99124266 Pending CN1257064A (en) | 1999-12-16 | 1999-12-16 | Process for recovering terephthalic acid from alkali reduced sewage |
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Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2434794A (en) * | 2006-02-03 | 2007-08-08 | Prom Ltd | Continuous process for forming anthranilic acid and treatment of waste water containing organic material |
| CN100404440C (en) * | 2003-09-02 | 2008-07-23 | 杭州国泰环保科技有限公司 | Chemical fiber printing alkali reducing quantity waste water resources pretreatment method |
| CN100436348C (en) * | 2006-10-13 | 2008-11-26 | 浙江大学 | Color fiber alkali decremental waste water treating and recovering process |
| CN100460348C (en) * | 2007-03-16 | 2009-02-11 | 嘉兴市新大众印染有限公司 | Method for treating and reclaiming wastewater of polyester piece goods dyeing and finishing |
| CN101982452A (en) * | 2010-10-26 | 2011-03-02 | 扬州市革领高科技纳米环保设备有限公司 | Method for extracting terephthalic acid from alkali weight reduction waste liquor |
| CN101244857B (en) * | 2007-02-12 | 2012-12-19 | 绍兴县精盛树酯科技有限公司 | Alkali deweighting wastewater processing method and device |
| CN103951106A (en) * | 2014-04-28 | 2014-07-30 | 上海大学 | Method for recycling terephthalic acid in polyester fiber alkali peeling process wastewater |
| CN104829879A (en) * | 2015-05-09 | 2015-08-12 | 江苏爱特恩东台新材料科技有限公司 | Method for preparing multifunctional rubber assistant by recycling alkali-weight-reduction processing discharged liquor |
| CN104829030A (en) * | 2015-05-12 | 2015-08-12 | 苏州苏净环保工程有限公司 | Treatment and recovery method of wastewater containing sodium terephthalate and 1,4-butanediol |
| CN105753687A (en) * | 2016-02-15 | 2016-07-13 | 常州市五洲化工有限公司 | Method for acquiring large-particle terephthalic acid crystals from alkali peeling wastewater |
| CN106032299A (en) * | 2015-03-14 | 2016-10-19 | 骆阿明 | Process for recycling and purification of PTA from printing and dyeing alkali decrement wastewater |
| CN106032351A (en) * | 2015-03-14 | 2016-10-19 | 王建中 | Crude PTA purification method |
| CN106519299A (en) * | 2016-12-07 | 2017-03-22 | 合肥工业大学 | Method for directly preparing modified hydrotalcite stabilizer from alkali deweighting wastewater |
| CN107459192A (en) * | 2016-06-06 | 2017-12-12 | 陈鸣 | A kind of strong basicity dyeing waste water is directly except slurry purification method |
| CN109019977A (en) * | 2018-08-31 | 2018-12-18 | 绍兴众聚环保科技有限公司 | A kind of dyeing alkali decrement waste water pretreating process |
| CN114195331A (en) * | 2021-12-31 | 2022-03-18 | 淄博志升信息科技有限公司 | Treatment process of terylene alkali weight reduction wastewater |
| CN114315043A (en) * | 2021-12-31 | 2022-04-12 | 淄博志升信息科技有限公司 | Treatment method of terylene alkali weight reduction wastewater |
-
1999
- 1999-12-16 CN CN 99124266 patent/CN1257064A/en active Pending
Cited By (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100404440C (en) * | 2003-09-02 | 2008-07-23 | 杭州国泰环保科技有限公司 | Chemical fiber printing alkali reducing quantity waste water resources pretreatment method |
| GB2434794A (en) * | 2006-02-03 | 2007-08-08 | Prom Ltd | Continuous process for forming anthranilic acid and treatment of waste water containing organic material |
| CN100436348C (en) * | 2006-10-13 | 2008-11-26 | 浙江大学 | Color fiber alkali decremental waste water treating and recovering process |
| CN101244857B (en) * | 2007-02-12 | 2012-12-19 | 绍兴县精盛树酯科技有限公司 | Alkali deweighting wastewater processing method and device |
| CN100460348C (en) * | 2007-03-16 | 2009-02-11 | 嘉兴市新大众印染有限公司 | Method for treating and reclaiming wastewater of polyester piece goods dyeing and finishing |
| CN101982452A (en) * | 2010-10-26 | 2011-03-02 | 扬州市革领高科技纳米环保设备有限公司 | Method for extracting terephthalic acid from alkali weight reduction waste liquor |
| CN103951106A (en) * | 2014-04-28 | 2014-07-30 | 上海大学 | Method for recycling terephthalic acid in polyester fiber alkali peeling process wastewater |
| CN106032351A (en) * | 2015-03-14 | 2016-10-19 | 王建中 | Crude PTA purification method |
| CN106032351B (en) * | 2015-03-14 | 2020-06-30 | 绍兴众聚环保科技有限公司 | Crude PTA purification treatment method |
| CN106032299A (en) * | 2015-03-14 | 2016-10-19 | 骆阿明 | Process for recycling and purification of PTA from printing and dyeing alkali decrement wastewater |
| CN104829879A (en) * | 2015-05-09 | 2015-08-12 | 江苏爱特恩东台新材料科技有限公司 | Method for preparing multifunctional rubber assistant by recycling alkali-weight-reduction processing discharged liquor |
| CN104829030A (en) * | 2015-05-12 | 2015-08-12 | 苏州苏净环保工程有限公司 | Treatment and recovery method of wastewater containing sodium terephthalate and 1,4-butanediol |
| CN105753687B (en) * | 2016-02-15 | 2018-08-07 | 常州市五洲化工有限公司 | A method of obtaining bulky grain terephthalic acid crystals from alkali decrement waste water |
| CN105753687A (en) * | 2016-02-15 | 2016-07-13 | 常州市五洲化工有限公司 | Method for acquiring large-particle terephthalic acid crystals from alkali peeling wastewater |
| CN107459192A (en) * | 2016-06-06 | 2017-12-12 | 陈鸣 | A kind of strong basicity dyeing waste water is directly except slurry purification method |
| CN106519299A (en) * | 2016-12-07 | 2017-03-22 | 合肥工业大学 | Method for directly preparing modified hydrotalcite stabilizer from alkali deweighting wastewater |
| CN109019977A (en) * | 2018-08-31 | 2018-12-18 | 绍兴众聚环保科技有限公司 | A kind of dyeing alkali decrement waste water pretreating process |
| CN114195331A (en) * | 2021-12-31 | 2022-03-18 | 淄博志升信息科技有限公司 | Treatment process of terylene alkali weight reduction wastewater |
| CN114315043A (en) * | 2021-12-31 | 2022-04-12 | 淄博志升信息科技有限公司 | Treatment method of terylene alkali weight reduction wastewater |
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