CN105085229A - Method for recovering TPA (terephthalic acid) from polyester alkali deweighting waste residues with limitation on rare earth materials - Google Patents
Method for recovering TPA (terephthalic acid) from polyester alkali deweighting waste residues with limitation on rare earth materials Download PDFInfo
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- CN105085229A CN105085229A CN201510556606.8A CN201510556606A CN105085229A CN 105085229 A CN105085229 A CN 105085229A CN 201510556606 A CN201510556606 A CN 201510556606A CN 105085229 A CN105085229 A CN 105085229A
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- tpa
- mixed solvent
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- alkali deweighting
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/47—Separation; Purification; Stabilisation; Use of additives by solid-liquid treatment; by chemisorption
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- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a method for recovering TPA (terephthalic acid) from polyester alkali deweighting waste residues with limitation on rare earth materials. The method comprises steps as follows: the alkali deweighting waste residues are dissolved in a DMF/MEK (dimethyl formamide/methyl ethyl ketone) mixed solvent, stirring, filtration, pH value adjustment, decolorization, precipitation and recovery treatment are performed, and a product is obtained. Experiments prove that with the gradual increase of the mass fraction of the DMF in the mixed solvent, the amount of the recovered TPA is gradually increased, and when the DMF in the mixed solvent is excessive, the amount of the recovered TPA tends to stability; with the increase of the mass ratio of the mixed solvent to the alkali deweighting waste residues, the amount of the recovered TPA is gradually increased, when the mass ratio of the mixed solvent to the alkali deweighting waste residues reaches a balance value, the amount of the recovered TPA is maximum, and when the mass ratio of the mixed solvent to the alkali deweighting waste residues is continuously increased, the amount of the recovered TPA has a trend of decrease. The method has the advantages that the amount of the recovered TPA is high, the toxicity of the solvent is low, the technology is safe, and the like and is mainly applied to the application field of recovery of the TPA in the polyester alkali deweighting waste residues.
Description
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 the method for terephthalic acid in the recovery Alkali Weight Reduction Treatment of Polyester waste residue limiting rare earth material.
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 the method for terephthalic acid in the recovery Alkali Weight Reduction Treatment of Polyester waste residue of open restriction rare earth material.
The present invention solves the problems of the technologies described above by the following technical solutions: the method limiting terephthalic acid in the recovery Alkali Weight Reduction Treatment of Polyester waste residue of rare earth material, 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, and described rare earth material is yttrium oxide or cerium oxide or lanthanum trioxide.
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 (1)
1. limit the method for terephthalic acid in the recovery Alkali Weight Reduction Treatment of Polyester waste residue of rare earth material, 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, and described rare earth material is yttrium oxide or cerium oxide or lanthanum trioxide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510556606.8A CN105085229A (en) | 2015-09-02 | 2015-09-02 | Method for recovering TPA (terephthalic acid) from polyester alkali deweighting waste residues with limitation on rare earth materials |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510556606.8A CN105085229A (en) | 2015-09-02 | 2015-09-02 | Method for recovering TPA (terephthalic acid) from polyester alkali deweighting waste residues with limitation on rare earth materials |
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| Publication Number | Publication Date |
|---|---|
| CN105085229A true CN105085229A (en) | 2015-11-25 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510556606.8A Pending CN105085229A (en) | 2015-09-02 | 2015-09-02 | Method for recovering TPA (terephthalic acid) from polyester alkali deweighting waste residues with limitation on rare earth materials |
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Citations (5)
| 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 |
-
2015
- 2015-09-02 CN CN201510556606.8A patent/CN105085229A/en active Pending
Patent Citations (5)
| 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 (1)
| Title |
|---|
| 贺永林: "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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Application publication date: 20151125 |