CN105085230A - Method for recycling terephthalic acid in terylene alkali peeling waste residue using mixed solvent - Google Patents

Method for recycling terephthalic acid in terylene alkali peeling waste residue using mixed solvent Download PDF

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Publication number
CN105085230A
CN105085230A CN201510557599.3A CN201510557599A CN105085230A CN 105085230 A CN105085230 A CN 105085230A CN 201510557599 A CN201510557599 A CN 201510557599A CN 105085230 A CN105085230 A CN 105085230A
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mixed solvent
waste residue
terephthalic acid
alkali
dmf
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CN201510557599.3A
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Chinese (zh)
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刘健
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Individual
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/42Separation; Purification; Stabilisation; Use of additives
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/42Separation; Purification; Stabilisation; Use of additives
    • C07C51/47Separation; Purification; Stabilisation; Use of additives by solid-liquid treatment; by chemisorption

Abstract

The invention discloses a method for recycling terephthalic acid in terylene alkali peeling waste residue using a mixed solvent. The method includes the following steps: dissolving the alkali peeling waste residue into a DMF/MEK mixed solvent, stirring, filtering, adjusting the pH value, bleaching, precipitating and recycling to obtain the product. The experiment shows that with the increasing of the mass percentage of DMF in the mixed solvent, the recycled terephthalic acid amount increases gradually; when DMF in the mixed solvent is excess, the recycled terephthalic acid amount tends to be stable; with the increase in the mass ratio of the mixed solvent to the alkali peeling waste residue, the recycled terephthalic acid amount increases gradually; when the mass ratio of the mixed solvent to the alkali peeling waste residue reaches an equilibrium value, the recycled terephthalic acid amount reaches the maximum; when the mass ratio of the mixed solvent to the alkali peeling waste residue is continuously increased, the recycled terephthalic acid amount shows a downtrend. The method provided by the invention has the advantages of being high in recycled terephthalic acid amount, small in solvent toxicity and safe in process, and can be mainly applied to the field of recycling terephthalic acid in terylene alkali peeling waste residue.

Description

A kind of mixed solvent reclaims the method for terephthalic acid in Alkali Weight Reduction Treatment of Polyester waste residue
Technical field
The present invention relates to the method field of reclaiming terephthalic acid in Alkali Weight Reduction Treatment of Polyester waste residue, particularly relate to a kind of method that mixed solvent reclaims terephthalic acid in Alkali Weight Reduction Treatment of Polyester waste residue.
Background technology
At present, the research of reclaiming about terephthalic acid in alkali decrement waste water (TPA) mainly adopts neutralisation, ion exchange method and ultrafiltration neutralisation etc., and the TPA purity that these methods reclaim all has much room for improvement.
" He Yonglin; Textile journal [J]; Organic solvent is on the impact of reclaiming terephthalic acid in Alkali Weight Reduction Treatment of Polyester waste residue; 12nd phase in 2013; 12-15 " in a literary composition with DMF be solvent, gac as discoloring agent, the TPA adopting solventing-out process to reclaim, has higher purity.But DMF is as toxic substance, and use as solvent separately, the security of technique is poor; In addition, with gac as discoloring agent, carry out heavy metal ion adsorbed in, can absorbed portion TPA effective constituent, cause the reduction of reclaiming TPA efficiency.
Summary of the invention
For the defect of current techniques, the present invention is intended to openly a kind of mixed solvent and reclaims the method for terephthalic acid in Alkali Weight Reduction Treatment of Polyester waste residue.
The present invention solves the problems of the technologies described above by the following technical solutions: a kind of mixed solvent reclaims the method for terephthalic acid in Alkali Weight Reduction Treatment of Polyester waste residue, Alkali reduction waste residue is dissolved in mixed solvent, through stirring, filtering, decolour, separate out and recycling, obtain product; Described mixed solvent comprises DMF, MEK, and described bleaching process uses rare earth material as discoloring agent.
Preferably: in described mixed solvent, the massfraction of DMF is 70% ~ 90%, that remaining is MEK.
Preferably: the mass ratio of described mixed solvent and Alkali reduction waste residue is 1:5 ~ 15.
Preferably: described rare earth material is yttrium oxide or cerium oxide or lanthanum trioxide.
Preferably: described rare earth material is yttrium oxide.
Preferably: described yttrium oxide is 0.1 ~ 2:1 with described slag quality ratio.
Preferably: carry out as follows, described DMF is mixed with described MEK, prepare described mixing solutions, described Alkali reduction waste residue is added in described mixing solutions, at 20 ~ 30 DEG C, after abundant stirring 30 ~ 90min, filter, add appropriate yttrium oxide in filtrate after filtration, after reacting completely, through secondary filtration, precipitation and recycling, obtain product.
Preferably: described churning time is 60min, whipping temp is 25 DEG C.
The present invention is by utilizing similar to mix and rare earth material heavy metal ion has the principles such as good adsorptivity, TPA in waste residue is dissolved in DMF/MEK mixed solvent, adopt distilled water as precipitation agent, rare earth material is decolorizing adsorbent, through process such as stirring, filtration, decolouring, precipitation and recovery, obtain the object of product.
The invention has the advantages that: the TPA rate of recovery is high, recovery TPA purity is large, reduce toxicity, improve security.
Accompanying drawing explanation
Fig. 1 is the graph of relation of DMF massfraction and the TPA rate of recovery in the present invention.
Fig. 2 is the graph of relation of Alkali reduction waste residue add-on and the TPA rate of recovery in the present invention.
Embodiment
Below in conjunction with accompanying drawing, the present invention is described in detail.
Embodiment 1
Prepare the DMF/MEK mixed solvent 50g that DMF and MEK mass ratio is 1:1,3:2,7:3,4:1,9:1 respectively, the Alkali reduction waste residue taking 3g is added in described mixed solvent, at 25 DEG C, after abundant stirring 60min, filter, in filtrate after filtration, add the Yttrium trinitrate of 2g, after reacting completely, through secondary filtration, separate out and recycling, obtain product.
As shown in Figure 1, along with the increase gradually of DMF massfraction, the TPA rate of recovery increases gradually, when DMF massfraction is 80%.The rate of recovery of TPA reaches 89.21%, and increase DMF massfraction further, the rate of recovery of TPA tends towards stability.This is because DMF is strong solvent, and along with the raising of DMF massfraction in mixed solvent, TPA dissolution degree is larger, after the massfraction of DMF reaches certain value, TPA fully dissolves, and continues the massfraction improving DMF, and TPA dissolution degree is not in generation considerable change.
Embodiment 2
Preparation DMF and MEK mass ratio is the DMF/MEK mixed solvent 50g of 4:1, the Alkali reduction waste residue taking 1g, 2g, 3g, 5g, 10g is respectively added in described mixed solvent, at 25 DEG C, after abundant stirring 60min, filter, in filtrate after filtration, add the Yttrium trinitrate of 2g, after reacting completely, through secondary filtration, separate out and recycling, obtain product.
As shown in Figure 2, along with the increase of Alkali reduction waste residue add-on, the change of the TPA rate of recovery is not obvious, and the rate of recovery of TPA is 88.62 ~ 89.19%, and when Alkali reduction waste residue add-on surpasses 3g, increase Alkali reduction waste residue add-on further, the rate of recovery of TPA declines gradually.This be due to TPA meltage do not reach capacity time, the rate of recovery of TPA is constant; After TPA meltage reaches capacity, because the meltage of TPA is constant, and the initial incremental amount of Alkali reduction waste residue increases, and therefore the rate of recovery of TPA declines.
Embodiment 3
Preparation DMF and MEK mass ratio is the DMF/MEK mixed solvent 50g of 4:1, the Alkali reduction waste residue taking 3g is added in described mixed solvent, at 25 DEG C, after abundant stirring 60min, filter, in filtrate after filtration, add the Yttrium trinitrate of 3g, the gac of 3g respectively, after reacting completely, through secondary filtration, separate out and recycling, obtain product.By calculating, after Yttrium trinitrate process, in product, the rate of recovery of TPA is 89.21%, and after activated carbon treatment, in product, the rate of recovery of TPA is 79.16%.
Analyze reason: with gac as discoloring agent, when carrying out heavy metal ion adsorbed, can absorbed portion TPA effective constituent, cause the minimizing of reclaiming TPA.When carrying out electrostatic adhesion with yttrium oxide heavy metal ion, can not adsorb TPA effective constituent, the rate of recovery of TPA is higher.
The foregoing is only the preferred embodiment of the invention; not in order to limit the invention; the any amendment done within all spirit in the invention and principle, equivalently to replace and improvement etc., within the protection domain that all should be included in the invention.

Claims (8)

1. reclaim a method for terephthalic acid in Alkali Weight Reduction Treatment of Polyester waste residue with mixed solvent, it is characterized in that: Alkali reduction waste residue is dissolved in mixed solvent, through stirring, filtration, adjust pH, decolouring, precipitation and recycling, obtain product; Described mixed solvent comprises DMF, MEK, and described decolorization phase uses rare earth material as discoloring agent.
2. a kind of mixed solvent according to claim 1 reclaims the method for terephthalic acid in Alkali Weight Reduction Treatment of Polyester waste residue, it is characterized in that: in described mixed solvent, the massfraction of DMF is 70% ~ 90%, and that remaining is MEK.
3. a kind of mixed solvent according to claim 1-2 reclaims the method for terephthalic acid in Alkali Weight Reduction Treatment of Polyester waste residue, it is characterized in that: the mass ratio of described mixed solvent and Alkali reduction waste residue is 1:5 ~ 15.
4. a kind of mixed solvent according to claim 1 reclaims the method for terephthalic acid in Alkali Weight Reduction Treatment of Polyester waste residue, it is characterized in that: described rare earth material is yttrium oxide or cerium oxide or lanthanum trioxide.
5. a kind of mixed solvent according to claim 4 reclaims the method for terephthalic acid in Alkali Weight Reduction Treatment of Polyester waste residue, it is characterized in that: described rare earth material is yttrium oxide.
6. a kind of mixed solvent according to claim 4-5 reclaims the method for terephthalic acid in Alkali Weight Reduction Treatment of Polyester waste residue, it is characterized in that: described yttrium oxide is 0.1 ~ 2:1 with described slag quality ratio.
7. a kind of mixed solvent according to claim 1 or 2 or 4 or 5 reclaims the method for terephthalic acid in Alkali Weight Reduction Treatment of Polyester waste residue, it is characterized in that: carry out as follows, described DMF is mixed with described MEK, prepare described mixing solutions, described Alkali reduction waste residue is added in described mixing solutions, at 20 ~ 30 DEG C, after abundant stirring 30 ~ 90min, filter, appropriate yttrium oxide is added in filtrate after filtration, after reacting completely, through secondary filtration, precipitation and recycling, obtain product.
8. a kind of mixed solvent according to claim 7 reclaims the method for terephthalic acid in Alkali Weight Reduction Treatment of Polyester waste residue, and it is characterized in that: described churning time is 60min, whipping temp is 25 DEG C.
CN201510557599.3A 2015-09-02 2015-09-02 Method for recycling terephthalic acid in terylene alkali peeling waste residue using mixed solvent Pending CN105085230A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20020193630A1 (en) * 2001-06-04 2002-12-19 Robert Lin Process for the production of purified terephthalic acid
CN101041616A (en) * 2007-03-22 2007-09-26 钱胜文 Method for purifying terephthalic acid from waste material
CN101503353A (en) * 2009-03-05 2009-08-12 浙江大学 Technique for purifying crude terephthalic acid from alkali deweighting wastewater
CN103570110A (en) * 2012-07-24 2014-02-12 上海纳米技术及应用国家工程研究中心有限公司 Efficient composite absorbing and flocculating agent used for printing and dyeing waste water treatment, preparation method thereof and applications thereof
CN103922926A (en) * 2014-04-17 2014-07-16 绍兴县远程树脂科技有限公司 Process for purifying residual solid waste generated after alkali peeling wastewater treatment

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20020193630A1 (en) * 2001-06-04 2002-12-19 Robert Lin Process for the production of purified terephthalic acid
CN101041616A (en) * 2007-03-22 2007-09-26 钱胜文 Method for purifying terephthalic acid from waste material
CN101503353A (en) * 2009-03-05 2009-08-12 浙江大学 Technique for purifying crude terephthalic acid from alkali deweighting wastewater
CN103570110A (en) * 2012-07-24 2014-02-12 上海纳米技术及应用国家工程研究中心有限公司 Efficient composite absorbing and flocculating agent used for printing and dyeing waste water treatment, preparation method thereof and applications thereof
CN103922926A (en) * 2014-04-17 2014-07-16 绍兴县远程树脂科技有限公司 Process for purifying residual solid waste generated after alkali peeling wastewater treatment

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
王国庆等: "仿真丝生产中碱减量及染整废水的治理", 《污染防治技术》 *
贺永林等: "有机溶剂对回收涤纶碱减量废渣中苯二甲酸的影响", 《纺织学报》 *

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