WO2009127117A1 - A process for resource processing purified terephthalic acid waste residue - Google Patents
A process for resource processing purified terephthalic acid waste residue Download PDFInfo
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- WO2009127117A1 WO2009127117A1 PCT/CN2009/000338 CN2009000338W WO2009127117A1 WO 2009127117 A1 WO2009127117 A1 WO 2009127117A1 CN 2009000338 W CN2009000338 W CN 2009000338W WO 2009127117 A1 WO2009127117 A1 WO 2009127117A1
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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
- C07C51/487—Separation; Purification; Stabilisation; Use of additives by treatment giving rise to chemical modification
- C07C51/493—Separation; Purification; Stabilisation; Use of additives by treatment giving rise to chemical modification whereby carboxylic acid esters are formed
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- 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
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts
Definitions
- the invention relates to a resource treatment method for chemical waste residue, in particular to a resource treatment method for purified terephthalic acid waste residue.
- Purified terephthalic acid is the basic raw material for the production of polyester fibers and PET resins.
- the terephthalic acid residue is a chemical waste discharged from the production of purified terephthalic acid. Its composition is complex.
- the main components are benzoic acid, terephthalic acid, p-phenylbenzoic acid, p-carboxybenzaldehyde, ortho-benzene.
- Most of the major purified terephthalic acid producers in foreign countries treat the purified terephthalic acid waste residue by incineration.
- the organic acid in the waste residue is burned by adding coal or fuel oil.
- the residue treatment method is for resources and energy. It causes great waste; some domestic terephthalic acid production enterprises wash the purified terephthalic acid waste residue, and recover the cobalt acetate and manganese acetate, and the waste residue is stacked in the open air or diluted with a large amount of water. The environment causes serious pollution and wastes valuable resources.
- the method for recycling the purified terephthalic acid waste residue comprises the following steps: a. heating the PTA waste residue to 60-100 ° C, and the obtained fraction is crude monobasic acid;
- step a The crude monobasic acid described in step a is controlled at 50-80 ° C to remove light components, and then subjected to distillation at 180-280 ° C and a negative pressure of 0.6-0.95 Mpa to obtain benzoic acid;
- step d The crude dibasic acid described in step b is input into the reaction vessel, and the reaction is carried out by adding alcohol and sulfuric acid, titanium series, aluminum series, or cobalt series catalyst, and the reaction temperature is controlled to be 60-100 ° C, and the reaction time is 2 ⁇ 10h; e.
- the reaction mixture obtained in step d is decolorized with activated carbon at 50 ⁇ 95 ° C for 2 ⁇ 5h;
- step e and bleaching tank Set the input material in step e and bleaching tank, at 50 ⁇ 95 ° C conditions, NaHC0 3 or NaOH to neutralize, and then cooled to room temperature, washed with water, controlling the pH at 5. 5 ⁇ 7.0 ° C ;
- step f The material obtained in step f is input into the fine column, at 180 ⁇ 28 (TC, negative pressure 0.77 ⁇ 0.98Mpa) Distillation to obtain terephthalate products;
- step h The wastewater obtained after de-lighting in step c, the residue after rectification, and the residue after rectification in step g are separately sent to a fuel-free incinerator for incineration treatment;
- a panel filter press or a centrifuge is used.
- the alcohol added in step d may be methanol or ethanol or octanol or ethylene glycol.
- the chemical products such as purified terephthalic acid, terephthalic acid and the rare metals cobalt and manganese can be extracted; the waste residue without use value is incinerated without any fuel condition.
- the waste residue can be used as a fuel, and the heat energy generated by the incineration can be recycled, and the chemical waste residue treatment can be resourced, harmless, reduced, and meet the requirements of circular economy and environmental protection.
- Figure 1 shows an industrial flow diagram of the present invention.
- the PTA waste residue was placed in a kettle, heated to 80 ° C, stirred while the benzoic acid was dissolved, and centrifuged by a centrifuge.
- the filtrate obtained was a crude monobasic acid (the mass was 43% of the original slag), and the filter residue was a crude dibasic acid (mass was 56% of the original slag).
- the fineness is about 0. 8Mpa, the fine is carried out. Distillate, worth 98.5% of benzoic acid.
- the residue of crude dibasic acid (acid value 568.46gK0H/kg, content 80%) was placed in the reaction vessel, and ethanol (920 g of ethanol per kg of crude dibasic acid) and concentrated sulfuric acid were added (the amount added was coarse).
- ethanol 920 g of ethanol per kg of crude dibasic acid
- concentrated sulfuric acid were added (the amount added was coarse).
- Activated carbon was introduced into the reaction thick mixture, and the amount was added in an amount of three thousandths, and the temperature was kept at 80 ° C for 3 hours. Then, the bleaching and thick road was boring and input into the kettle, and NaOH was added (the amount added was 1.5% of the mass of the crude dibasic acid).
- the water-washed material is input into a fine column, and refined at 200-210 ° C, 0.74-0. 76 Mpa to obtain a terephthalate. , the recovery rate reached 99%.
- Waste water obtained by removing light components from crude dibasic acid, residue after rectification, residue after crude diacid distillation They are sent to the incinerator for incineration.
- the ash obtained after incineration is put into the solution NH 4 HC0 3 solution for precipitation reaction.
- the resulting precipitate was washed by dosing, then dissolved in excess acetic acid, and dehydrated by adding two-thousandths of activated carbon. Filtration method for removing the activated carbon was added was allowed to stand 02 standing 3-4h after removal of iron ions, the liquid evaporated to give the cobalt acetate, manganese salts.
Abstract
Disclosed is a process for resource processing purified terephthalic acid waste residue, which comprises: heating purified terephthalic acid waste residue and separating to get crude monoacid and binary acid; cutting light component out of the crude monoacid and then rectifying to get benzoic acid; feeding the crude binary acid into a reactor, adding alcohol and sulfuric acid or titanium series, aluminum series or cobalt series catalyst and reacting; decoloring with active carbon, neutralizing, washing with water and rectifying to get esters of terephthalic acid; sending the residue from rectification into an incinerator exempting fuel, and extracting cobalt, manganese and other rare metals from the residue produced by burning. The process can extract chemical industrial products of benzoic acid and esters of terephthalic acid, as well as cobalt, manganese and other rare metals, and burn the unavailable residue without any burning condition.
Description
精对苯二甲酸废渣的资源化处理方法 Resource treatment method for purified terephthalic acid waste residue
技术领域 Technical field
本发明涉及一种化工废渣的资源化处理方法，具体涉及一种精对苯二甲酸废 渣的资源化处理方法。 The invention relates to a resource treatment method for chemical waste residue, in particular to a resource treatment method for purified terephthalic acid waste residue.
背景技术 Background technique
精对苯二甲酸（ purified terephthalic acid , PTA) 是生产聚酯纤维和 PET 树脂的基本原料。精对苯二甲酸残渣是精对苯二甲酸生产过程中排出的化工废弃 物， 其成分比较复杂， 主要成分有苯甲酸、 对苯二甲酸、 对苯基苯甲酸、 对羧基 苯甲醛、 邻苯二甲酸、 间苯二甲酸、 苯二甲酸及缩合物等。 国外主要精对苯二甲 酸生产企业对精对苯二甲酸废渣的处理方法大多是通过焚烧法来处理，采用加煤 或燃油烧掉废渣中的有机酸，这样的残渣处理方法对资源、能源均造成极大浪费； 国内一些精对苯二甲酸生产企业，则是对精对苯二甲酸废渣进行水洗处理，将其 中的醋酸钴、醋酸锰回收， 而废渣露天堆放或用大量水稀释排放既对环境造成严 重污染， 有浪费了可贵资源。 Purified terephthalic acid (PTA) is the basic raw material for the production of polyester fibers and PET resins. The terephthalic acid residue is a chemical waste discharged from the production of purified terephthalic acid. Its composition is complex. The main components are benzoic acid, terephthalic acid, p-phenylbenzoic acid, p-carboxybenzaldehyde, ortho-benzene. Dicarboxylic acid, isophthalic acid, phthalic acid, condensate, and the like. Most of the major purified terephthalic acid producers in foreign countries treat the purified terephthalic acid waste residue by incineration. The organic acid in the waste residue is burned by adding coal or fuel oil. The residue treatment method is for resources and energy. It causes great waste; some domestic terephthalic acid production enterprises wash the purified terephthalic acid waste residue, and recover the cobalt acetate and manganese acetate, and the waste residue is stacked in the open air or diluted with a large amount of water. The environment causes serious pollution and wastes valuable resources.
发明内容 Summary of the invention
本发明的目的在于提供一种既可有效提取资源，同时又符合环保要求的对精 对苯二甲酸废渣的资源化处理方法。 It is an object of the present invention to provide a resource treatment method for purified terephthalic acid waste residue which can effectively extract resources while complying with environmental protection requirements.
本发明提供的一种精对苯二甲酸废渣的资源化处理方法， 包括下列步骤： a.将 PTA废渣加热至 60~100°C， 得到的馏分为粗一元酸； The method for recycling the purified terephthalic acid waste residue provided by the invention comprises the following steps: a. heating the PTA waste residue to 60-100 ° C, and the obtained fraction is crude monobasic acid;
b.分离步骤 a所得废渣， 得到粗二元酸； b. separation step a obtained waste residue to obtain a crude dibasic acid;
c.将步骤 a所述的粗一元酸控制在 50~80°C脱轻组分， 再经 180~280°C、 负 压 0. 6~0.95Mpa进行精馏得苯甲酸； c. The crude monobasic acid described in step a is controlled at 50-80 ° C to remove light components, and then subjected to distillation at 180-280 ° C and a negative pressure of 0.6-0.95 Mpa to obtain benzoic acid;
d.步骤 b中所述的粗二元酸输入反应釜中， 加入醇以及硫酸、 钛系列、 铝系 列、 或钴系列催化剂进行反应， 控制反应温度为 60~100°C， 反应时间为 2~10h; e.将步骤 d得到的反应混合物在 50~95°C条件下用活性炭脱色， 维持时间 2~5h; d. The crude dibasic acid described in step b is input into the reaction vessel, and the reaction is carried out by adding alcohol and sulfuric acid, titanium series, aluminum series, or cobalt series catalyst, and the reaction temperature is controlled to be 60-100 ° C, and the reaction time is 2~ 10h; e. The reaction mixture obtained in step d is decolorized with activated carbon at 50~95 ° C for 2~5h;
f.将步骤 e脱色后的物料输入中和釜，在 50~95°C条件下，以 NaOH或 NaHC03 进行中和， 然后冷却至常温进行水洗， 控制 pH值在 5. 5〜7.0°C ; f. Set the input material in step e and bleaching tank, at 50 ~ 95 ° C conditions, NaHC0 3 or NaOH to neutralize, and then cooled to room temperature, washed with water, controlling the pH at 5. 5~7.0 ° C ;
g.将步骤 f所得物料输入精熘塔， 在 180~28(TC、负压 0. 7~0.98Mpa条件下
精馏， 得到对苯二甲酸酯类产品； g. The material obtained in step f is input into the fine column, at 180~28 (TC, negative pressure 0.77~0.98Mpa) Distillation to obtain terephthalate products;
h.将步骤 c所述脱轻后得到的废水、 精馏后的残渣， 步骤 g所述精馏后的残 渣分别送入免燃料焚烧炉中焚烧处理； h. The wastewater obtained after de-lighting in step c, the residue after rectification, and the residue after rectification in step g are separately sent to a fuel-free incinerator for incineration treatment;
i.从步骤 h所得焚烧产生的灰渣中提取稀有金属钴、 锰。 i. Extracting rare metals such as cobalt and manganese from the ash produced by incineration in step h.
为实现步骤 b 中分离废渣的过程， 采用板柜压滤机或离心机。 In order to carry out the process of separating the waste in step b, a panel filter press or a centrifuge is used.
步骤 d中加入的醇类可以为甲醇或乙醇或辛醇或乙二醇。 The alcohol added in step d may be methanol or ethanol or octanol or ethylene glycol.
为了提取稀有金属钴、 锰， 采用 N HC03溶液同时沉淀钴、 锰， 然后用过 来的醋酸溶解， 再多次精制最终得到醋酸钴锰盐。 In order to extract rare metals cobalt, manganese, N HC0 3 solution using simultaneous precipitation of cobalt, manganese, and then dissolved in acetic acid over, and then repeatedly purified to obtain the final cobalt-manganese acetate salts.
采用本发明精对苯二甲酸废渣的资源化处理方法，可提取精对苯二甲酸，对 苯二甲酸等的化工产品及稀有金属钴、锰；无利用价值的废渣在无需任何燃料条 件下焚烧处理， 即可将废渣做燃料使用， 又能将焚烧产生的热能回收利用， 可以 实现化学废渣处理资源化、 无害化、 减量化、 符合循环经济要求和环保要求。 附图说明 By adopting the resource treatment method of the purified terephthalic acid waste residue of the invention, the chemical products such as purified terephthalic acid, terephthalic acid and the rare metals cobalt and manganese can be extracted; the waste residue without use value is incinerated without any fuel condition. After the treatment, the waste residue can be used as a fuel, and the heat energy generated by the incineration can be recycled, and the chemical waste residue treatment can be resourced, harmless, reduced, and meet the requirements of circular economy and environmental protection. DRAWINGS
图 1表示本发明的工业流程图。 Figure 1 shows an industrial flow diagram of the present invention.
具体实施方式 detailed description
将 PTA废渣投入釜中， 加热至 80°C， 同时搅拌， 使苯甲酸溶解， 采用离心 机趁热进行离心。 所得滤液为粗一元酸 （质量为原渣的 43%)， 滤渣为粗二元酸 (质量为原渣的 56%)。 The PTA waste residue was placed in a kettle, heated to 80 ° C, stirred while the benzoic acid was dissolved, and centrifuged by a centrifuge. The filtrate obtained was a crude monobasic acid (the mass was 43% of the original slag), and the filter residue was a crude dibasic acid (mass was 56% of the original slag).
将粗一元酸输入釜中， 调整温度为 60-70Ό， 将轻组分蒸发并冷凝为废水； 将轻组分去除后剩余的液体升温至 200-220Ό , 压力控制在 0. 8Mpa左右， 进行 精馏， 值得纯度为 98. 5%的苯甲酸。 The fineness is about 0. 8Mpa, the fine is carried out. Distillate, worth 98.5% of benzoic acid.
将粗二元酸（酸值为 568. 46gK0H/kg， 含量为 80%)残渣置于反应釜中， 加 入乙醇 （每千克粗二元酸中加入乙醇 920克）和浓硫酸（加入量为粗二元酸的 4%), 在 75-85°C条件下反应 5h， 酯化率达到 97%。 向反应厚道混合物中投入活 性炭， 加入量为千分之三， 在 80°C下保温 3h。 然后将脱色厚道无聊输入釜中， 加入 NaOH (加入量为粗二元酸质量的 1. 5%)。 然后冷却至常温， 进行水洗后 pH 值达到 6. 5.将水洗后的物料输入精熘塔， 在 200-210°C， 0. 74-0. 76Mpa下精镏， 得到对苯二甲酸酯， 回收率达到 99%。 The residue of crude dibasic acid (acid value 568.46gK0H/kg, content 80%) was placed in the reaction vessel, and ethanol (920 g of ethanol per kg of crude dibasic acid) and concentrated sulfuric acid were added (the amount added was coarse). 4% of the dibasic acid, reacted at 75-85 ° C for 5 h, and the esterification rate reached 97%. Activated carbon was introduced into the reaction thick mixture, and the amount was added in an amount of three thousandths, and the temperature was kept at 80 ° C for 3 hours. Then, the bleaching and thick road was boring and input into the kettle, and NaOH was added (the amount added was 1.5% of the mass of the crude dibasic acid). Then, it is cooled to normal temperature, and after washing with water, the pH value reaches 6. 5. The water-washed material is input into a fine column, and refined at 200-210 ° C, 0.74-0. 76 Mpa to obtain a terephthalate. , the recovery rate reached 99%.
将粗二元酸脱轻组分后得到的废水、精馏后的残渣，粗二元酸精馏后的残渣
分别送入免焚烧炉中焚烧处理。为了回收稀有金属钴锰，将焚烧后所得灰渣投入 溶液 NH4HC03溶液中进行沉淀反应。 将所得沉淀采用睡洗涤， 然后用过量的醋酸 溶解，加入千分之二的活性炭进行脱色。采用过滤的方法除去该活性炭， 加入静 置 02静置 3-4h除去铁离子后， 对液体进行蒸发结晶， 得到醋酸钴锰盐。
Waste water obtained by removing light components from crude dibasic acid, residue after rectification, residue after crude diacid distillation They are sent to the incinerator for incineration. In order to recover the rare metal cobalt manganese, the ash obtained after incineration is put into the solution NH 4 HC0 3 solution for precipitation reaction. The resulting precipitate was washed by dosing, then dissolved in excess acetic acid, and dehydrated by adding two-thousandths of activated carbon. Filtration method for removing the activated carbon was added was allowed to stand 02 standing 3-4h after removal of iron ions, the liquid evaporated to give the cobalt acetate, manganese salts.
Claims
1. 一种精对苯二甲酸废渣的资源化处理方法，其特征在于：采取下列步骤: a.将 PTA废渣加热至 60~100°C， 得到的熘分为粗一元酸； A method for recycling a purified terephthalic acid waste residue, characterized in that the following steps are taken: a. heating the PTA waste residue to 60-100 ° C, and the obtained mash is divided into crude monobasic acid;
b.分离步骤 a所得废渣， 得到粗二元酸； b. separation step a obtained waste residue to obtain a crude dibasic acid;
c.将步骤 a所述的粗一元酸控制在 50~80°C脱轻组分， 再经 180~280°C、 负压c. The crude monobasic acid described in step a is controlled at 50~80 °C to remove light components, and then subjected to 180~280 ° C, negative pressure.
0. 6~0.95Mpa进行精馏得苯甲酸； 0. 6~0.95Mpa for rectification to obtain benzoic acid;
d.步骤 b中所述的粗二元酸输入反应釜中， 加入醇以及硫酸、 钛系列、 铝系列、 或钴系列催化剂进行反应， 控制反应温度为 60〜100°C， 反应时间为 2~10h;e.将步骤 d得到的反应混合物在 50~95°C条件下用活性炭脱色， 维持时间 2~5h; f.将步骤 e脱色后的物料输入中和釜， 在 50~95°C条件下， 以 NaOH或 NaHC03进 行中和， 然后冷却至常温进行水洗， 控制 pH值在 5. 5~7.0°C ; d. The crude dibasic acid described in step b is input into the reaction vessel, and the reaction is carried out by adding alcohol and sulfuric acid, titanium series, aluminum series, or cobalt series catalyst, and the reaction temperature is controlled to be 60 to 100 ° C, and the reaction time is 2~ 10h; e. The reaction mixture obtained in step d is decolorized with activated carbon at 50-95 ° C for 2~5 h; f. The material decolored after step e is input into the neutralization kettle at 50-95 ° C. under NaHC0 3 or NaOH to neutralize, and then cooled to room temperature, washed with water, controlling the pH at 5. 5 ~ 7.0 ° C;
g.将步骤 f所得物料输入精馏塔，在 180~280°C、负压 0. 7~0.98Mpa条件下精馏， 得到对苯二甲酸酯类产品； g. The material obtained in step f is input into a rectification column, and is subjected to rectification under conditions of 180 to 280 ° C and a negative pressure of 0.7 to 0.98 Mpa to obtain a terephthalate product;
h.将步骤 c所述脱轻后得到的废水、 精馏后的残渣， 步骤 g所述精馏后的残渣分 别送入免燃料焚烧炉中焚烧处理； h. The waste water obtained after de-lighting in step c, the residue after rectification, and the residue after rectification in step g are separately sent to a fuel-free incinerator for incineration treatment;
1.从步骤 h所得焚烧产生的灰渣中提取稀有金属钴、 猛。 1. Extract the rare metal cobalt and fierce from the ash produced by the incineration obtained in step h.
2.根据权利要求 1所述的精对二苯甲酸废渣的资源化处理方法， 其特征在 于： 所述步骤 b采用板柜压滤机或离心机分离废渣。 The method for recycling a purified p-dibenzoic acid waste residue according to claim 1, wherein the step b is performed by using a panel filter press or a centrifuge to separate the waste residue.
3.根据权利要求 1所述的精对二苯甲酸废渣的资源化处理方法，其特征在于： 步骤 d中加入的醇类为甲醇或乙醇或辛醇或乙二醇。 The method for recycling a purified p-dibenzoate waste according to claim 1, wherein the alcohol added in the step d is methanol or ethanol or octanol or ethylene glycol.
4.根据权利要求 1所述的精对二苯甲酸废渣的资源化处理方法， 其特征在 于： 步骤 i所述提取稀有金属钴、锰的方法为： 采用 N HC03溶液同时沉淀钴、 锰， 然后用过来的醋酸溶解， 再多次精制最终得到醋酸钴锰盐。
The method for recycling the purified p-dibenzoic acid waste residue according to claim 1, wherein: the method for extracting the rare metal cobalt and manganese in the step i is: simultaneously depositing cobalt and manganese by using the N HC0 3 solution; Then, it is dissolved in acetic acid and then refined a plurality of times to finally obtain a cobalt manganese acetate salt.
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| CNA2008100235548A CN101255107A (en) | 2008-04-03 | 2008-04-03 | Resourceful treatment method of purified terephthalic acid waste residue |
| CN200810023554.8 | 2008-04-03 |
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| CN101255107A (en) * | 2008-04-03 | 2008-09-03 | 沈福昌 | Resourceful treatment method of purified terephthalic acid waste residue |
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| CN101255107A (en) * | 2008-04-03 | 2008-09-03 | 沈福昌 | Resourceful treatment method of purified terephthalic acid waste residue |
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| WO2016023958A1 (en) * | 2014-08-12 | 2016-02-18 | Invista Technologies S.À R.L. | Process for recovering an aromatic monocarboxylic acid |
| CN113151686A (en) * | 2020-12-08 | 2021-07-23 | 南通百川新材料有限公司 | Equipment and method for recovering cobalt-manganese mixture in trimellitic anhydride production residues |
| CN112876357A (en) * | 2021-01-20 | 2021-06-01 | 江苏福昌环保科技集团有限公司 | Production process for producing plasticizer from PTA oxidation residues |
Also Published As
| Publication number | Publication date |
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| CN101513641B (en) | 2012-10-31 |
| CN101255107A (en) | 2008-09-03 |
| CN101513641A (en) | 2009-08-26 |
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