CN105503605A - Method for preparing dimethyl terephthalate from polybutylene terephthalate waste material - Google Patents
Method for preparing dimethyl terephthalate from polybutylene terephthalate waste material Download PDFInfo
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- CN105503605A CN105503605A CN201510929412.8A CN201510929412A CN105503605A CN 105503605 A CN105503605 A CN 105503605A CN 201510929412 A CN201510929412 A CN 201510929412A CN 105503605 A CN105503605 A CN 105503605A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/03—Preparation of carboxylic acid esters by reacting an ester group with a hydroxy group
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Abstract
The invention belongs to the field of polybutylene terephthalate, and particularly relates to a method for preparing dimethyl terephthalate from the polybutylene terephthalate waste material. The method includes the following steps of firstly, making the polybutylene terephthalate waste material and monohydric alcohol react in a closed reactor under the condition of titanate catalysis to obtain reaction liquid, wherein the polybutylene terephthalate waste material is one or more of the polyethylene glycol terephthalate waste material, the polytrimethylene terephthalate waste material and the polybutylene terephthalate waste material, monohydric alcohol is one or more of butyl alcohol, amyl alcohol, hexyl alcohol, heptanol, capryl alcohol, nonyl alcohol and decyl alcohol, and the reaction temperature is 200-220 DEG C; secondly, processing the reaction liquid to obtain dimethyl terephthalate. Experiment results show that when dimethyl terephthalate is prepared through the method with the polybutylene terephthalate waste material as the reaction raw material, the product yield of dimethyl terephthalate is larger than 90%.
Description
Technical field
The invention belongs to poly terephthalic acid diol ester field, particularly relate to a kind of method utilizing poly terephthalic acid diol ester waste material to prepare terephthalate.
Background technology
Polyester is the polymkeric substance general name obtained by polyvalent alcohol and polyprotonic acid polycondensation, is a class excellent performance, broad-spectrum engineering plastics.Along with the development of petrochemical complex, the polyester industry achievement of China is remarkable, has now become polyester product manufacture base maximum in the world.
At present, the polyester material be most widely used is poly terephthalic acid diol ester, polyethylene terephthalate particularly in poly terephthalic acid diol ester, because it has excellent physical and mechanical properties and electrical insulating property in wide temperature range, be widely used in the fields such as packing business, electronic apparatus, health care, building, automobile.
Along with the extensive application in daily life of poly terephthalic acid naphthalate material goods, As time goes on incident be, goods enter the date of retirement, and a large amount of poly terephthalic acid naphthalate material goods become waste material.For the disposal of poly terephthalic acid diol ester waste material, traditional disposal options has burial biodegradation and burning.But because poly terephthalic acid diol ester belongs to difficult degradation material, if rely on natural degradation these wastes to need more than 100 years, and burned and can be produced a large amount of toxic and harmfuls, huge pollution is caused to environment.
For the disposal of poly terephthalic acid diol ester waste material, optimal mode carries out recycling to it exactly, so not only can avoid landfill and burn the problems brought, can also turn waste into wealth, bring economic benefit.Therefore, the recycling how realizing poly terephthalic acid diol ester waste material is current problem demanding prompt solution.
Summary of the invention
In view of this, the object of the present invention is to provide a kind of method utilizing poly terephthalic acid diol ester waste material to prepare terephthalate, method provided by the invention not only can realize the recycling of poly terephthalic acid diol ester waste material, and the yield of the phthalic acid ester prepared is higher.
The invention provides a kind of method utilizing poly terephthalic acid diol ester waste material to prepare terephthalate, comprise the following steps:
A), poly terephthalic acid diol ester waste material and monohydroxy-alcohol react under titanic acid ester catalytic condition in closed reactor, obtains reaction solution;
Described poly terephthalic acid diol ester waste material is one or more in polyethylene terephthalate waste material, Poly(Trimethylene Terephthalate) waste material and polybutylene terephthalate waste material;
Described monohydroxy-alcohol is one or more in butanols, amylalcohol, hexanol, enanthol, octanol, nonyl alcohol and decyl alcohol;
The temperature of described reaction is 200 ~ 220 DEG C;
B), described reaction solution carries out aftertreatment, obtains terephthalate.
Preferably, the described number of ester groups of poly terephthalic acid diol ester waste material and the mol ratio of monohydroxy-alcohol are 1:(1 ~ 2).
Preferably, described titanic acid ester comprises tetrabutyl titanate and/or titanium isopropylate.
Preferably, the mass ratio of described poly terephthalic acid diol ester waste material and titanic acid ester is (200 ~ 500): 1.
Preferably, step a) in, the time of described reaction is 2 ~ 10h.
Preferably, the number-average molecular weight of described poly terephthalic acid diol ester waste material is 70000 ~ 110000.
Preferably, described step b) specifically comprise:
B1), described reaction solution distills, and obtains terephthalate crude product and alcohol mixture;
Described alcohol mixture comprises ethylene glycol and described monohydroxy-alcohol;
B2), described terephthalate crude product carries out washing and decolouring successively, obtains terephthalate.
Preferably, step b1) in, described reaction solution first filters, then distills filtering the filtrate obtained.
Preferably in, also comprise: described alcohol mixture is separated, obtain ethylene glycol and monohydroxy-alcohol.
Preferably, step a) in, described poly terephthalic acid diol ester waste material first successively through washing, dry and after pulverizing, then reacts under titanic acid ester catalytic condition with monohydroxy-alcohol in closed reactor.
Compared with prior art, the invention provides a kind of method utilizing poly terephthalic acid diol ester waste material to prepare terephthalate.Method provided by the invention comprises the following steps: a), poly terephthalic acid diol ester waste material and monohydroxy-alcohol react under titanic acid ester catalytic condition in closed reactor, obtains reaction solution; Described poly terephthalic acid diol ester waste material is one or more in polyethylene terephthalate waste material, Poly(Trimethylene Terephthalate) waste material and polybutylene terephthalate waste material; Described monohydroxy-alcohol is one or more in butanols, amylalcohol, hexanol, enanthol, octanol, nonyl alcohol and decyl alcohol; The temperature of described reaction is 200 ~ 220 DEG C; B), described reaction solution carries out aftertreatment, obtains terephthalate.Method provided by the invention with poly terephthalic acid diol ester waste material and monohydroxy-alcohol for reaction raw materials, using titanic acid ester as catalysts, simultaneously by selecting specific temperature of reaction, prepare terephthalic acid ester articles, and goods yield is higher, the method can be applicable to the recycling of poly terephthalic acid diol ester waste material.Experimental result shows, using poly terephthalic acid diol ester waste material as reaction raw materials, when adopting method provided by the invention to prepare terephthalate, its product yield is greater than 90%.
Embodiment
Be clearly and completely described the technical scheme in the embodiment of the present invention below, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
The invention provides a kind of method utilizing poly terephthalic acid diol ester waste material to prepare terephthalate, comprise the following steps:
A), poly terephthalic acid diol ester waste material and monohydroxy-alcohol react under titanic acid ester catalytic condition in closed reactor, obtains reaction solution;
Described poly terephthalic acid diol ester waste material is one or more in polyethylene terephthalate waste material, Poly(Trimethylene Terephthalate) waste material and polybutylene terephthalate waste material;
Described monohydroxy-alcohol is one or more in butanols, amylalcohol, hexanol, enanthol, octanol, nonyl alcohol and decyl alcohol;
The temperature of described reaction is 200 ~ 220 DEG C;
B), described reaction solution carries out aftertreatment, obtains terephthalate.
In method provided by the invention, first poly terephthalic acid diol ester waste material and monohydroxy-alcohol are reacted under titanic acid ester catalytic condition in closed reactor.Wherein, described poly terephthalic acid diol ester waste material is one or more in polyethylene terephthalate waste material, Poly(Trimethylene Terephthalate) waste material and polybutylene terephthalate waste material.In the present invention, the number-average molecular weight of described poly terephthalic acid diol ester waste material is preferably 70000 ~ 110000.In the present invention, described polyethylene terephthalate waste material has formula (I-1) structure, described Poly(Trimethylene Terephthalate) waste material preferably has formula (I-2) structure, and described polybutylene terephthalate waste material preferably has formula (I-3) structure:
In the present invention, described poly terephthalic acid diol ester waste material preferably first successively after washing, drying and pulverizing, then reacts under titanic acid ester catalytic condition with monohydroxy-alcohol in closed reactor.
In the present invention, described poly terephthalic acid diol ester waste material and monohydroxy-alcohol carry out in the process of reacting under titanic acid ester catalytic condition in closed reactor, and described monohydroxy-alcohol is one or more in butanols, amylalcohol, hexanol, enanthol, octanol, nonyl alcohol and decyl alcohol.Wherein, described butanols preferably includes propyl carbinol and/or isopropylcarbinol; Described octanol preferably includes isooctyl alcohol.In the present invention, the described number of ester groups of poly terephthalic acid diol ester waste material and the mol ratio of monohydroxy-alcohol are preferably 1:(1 ~ 2), be more preferably 1:(1 ~ 1.5), most preferably be 1:(1.1 ~ 1.3), be the most preferably 1:(1 ~ 1.2).
In the present invention, described poly terephthalic acid diol ester waste material and monohydroxy-alcohol carry out in the process of reacting under titanic acid ester catalytic condition in closed reactor, and described titanic acid ester preferably includes tetrabutyl titanate and/or titanium isopropylate.In the present invention, the mass ratio of described poly terephthalic acid diol ester waste material and titanic acid ester is preferably (200 ~ 500): 1, is more preferably (300 ~ 400): 1, most preferably is (350 ~ 400): 1.
In the present invention, described poly terephthalic acid diol ester waste material and monohydroxy-alcohol carry out in the process of reacting under titanic acid ester catalytic condition in closed reactor, and the temperature of described reaction is 200 ~ 220 DEG C, is more preferably 200 ~ 210 DEG C; The time of described reaction is preferably 2 ~ 10h, is more preferably 4 ~ 8h, most preferably is 5 ~ 6h.In the present invention, described closed reactor is preferably high-temperature high-pressure reaction kettle well known to those skilled in the art.After reaction terminates, obtain reaction solution.Described reaction solution comprises poly terephthalic acid diol ester waste material and monohydroxy-alcohol reacts the phthalic acid ester and ethylene glycol that generate, also may comprise the poly terephthalic acid diol ester waste material not carrying out reacting and monohydroxy-alcohol.
In the present invention, after obtaining described reaction solution, described reaction solution carries out aftertreatment, and this process specifically comprises:
B1), described reaction solution distills, and obtains terephthalate crude product and alcohol mixture;
Described alcohol mixture comprises ethylene glycol and described monohydroxy-alcohol;
B2), described terephthalate crude product carries out washing and decolouring successively, obtains terephthalate.
In the process of above-mentioned reaction solution aftertreatment provided by the invention, first described reaction solution distills.In still-process, by collecting the distillate under different distillation temperature, achieve the separation of the different each component of described reaction solution mid-boiling point.In the present invention, the mode of described distillation is preferably vacuum distilling.After distillation terminates, obtain terephthalate crude product and alcohol mixture, described alcohol mixture comprises ethylene glycol and does not carry out the described monohydroxy-alcohol that reacts.In the present invention, the product of distillation collected under low temperature is generally alcohol mixture, and the product of distillation collected under high temperature is generally phthalic acid ester crude product.In an embodiment provided by the invention, described reaction solution comprises terephthalic acid dibutyl ester and alcohol mixture, and described alcohol mixture is isooctyl alcohol and ethylene glycol.In this embodiment, in still-process, what below 225 DEG C, distillation was collected is alcohol mixture, and what more than 225 DEG C, distillation was collected is terephthalate crude product.
In the present invention, described reaction solution preferably first filters, then distills filtering the filtrate obtained.In the present invention, the object of filtering reaction solution is the solid impurity in filtering reaction solution, improves the purity of goods.
In the process of above-mentioned reaction solution aftertreatment provided by the invention, after obtaining described terephthalate crude product, described terephthalate crude product carries out washing and decolouring successively.Wherein, the mode of described washing is preferably washing.After the present invention preferably first carries out neutralizing treatment to described terephthalate crude product, then wash.In the present invention, the mode of described decolouring preferably includes stripping decolouring and/or activated carbon decolorizing.In an embodiment provided by the invention, described terephthalate crude product after washing carries out stripping decolouring and activated carbon decolorizing successively, this process specifically comprises: first carry out stripping to the described terephthalate crude product after washing, terephthalate crude product after stripping dewaters, and namely completes stripping bleaching process after dehydration terminates; Terephthalate crude product after dehydration mixes with gac, and gac adsorbs the pigment in described terephthalate crude product, afterwards filtering gac, completes activated carbon decolorizing operation.After decolouring terminates, obtain terephthalate.
In the process of above-mentioned reaction solution aftertreatment provided by the invention, after obtaining described alcohol mixture, preferably described alcohol mixture is separated, obtains ethylene glycol and monohydroxy-alcohol.In the present invention, the mode that described alcohol mixture carries out being separated is preferably: first by described mixing alcohol and water mixing, leave standstill, separatory, obtains aqueous phase and organic phase, and wherein, be dissolved with ethylene glycol in described aqueous phase, described organic phase is monohydroxy-alcohol; Then described aqueous phase is distilled, obtain ethylene glycol.In the present invention, after obtaining ethylene glycol and monohydroxy-alcohol, described ethylene glycol is preferred for preparing PEGylation chemical product, and described monohydroxy-alcohol is preferably used for again preparing terephthalate as reaction raw materials.
Method provided by the invention with poly terephthalic acid diol ester waste material and monohydroxy-alcohol for reaction raw materials, using titanic acid ester as catalysts, simultaneously by selecting specific temperature of reaction, prepare terephthalic acid ester articles, and goods yield is higher, speed of response is very fast, and the method can be applicable to the recycling of poly terephthalic acid diol ester waste material.
In preferred implementation provided by the invention, using polyethylene terephthalate waste material and isooctyl alcohol as reaction raw materials, prepared Di-2-ethylhexyl terephthalate goods, these goods are softening agent of a kind of excellent property, have wide market application foreground.
Experimental result shows, using poly terephthalic acid diol ester waste material as reaction raw materials, when adopting method provided by the invention to prepare terephthalate, its product yield is greater than 90%.
For the purpose of clearer, be described in detail below by following examples.
Embodiment 1
Polyethylene terephthalate waste material (number-average molecular weight is preferably 70000 ~ 110000) is rinsed well with water, puts into baking oven, and temperature controls to dry 0.8h at 130 ~ 140 DEG C, and the waste material pulverizer after oven dry is ground into powder.Accurately take wasted powder 384g, isooctyl alcohol 624g puts into the high-temperature high-pressure reaction kettle of 2000mL, adds 1g tetrabutyl titanate, be warmed up to 200 ~ 210 DEG C, the reaction times is 6h, and reaction terminates rear vacuum pump suction filtration, filtrate is carried out vacuum distilling, collects distillate.Wherein, what collect before 225 DEG C is the mixture of isooctyl alcohol and ethylene glycol; More than 225 DEG C collect be Di-2-ethylhexyl terephthalate crude product.
The mixture of described isooctyl alcohol and ethylene glycol is mixed with water, the mixed solution be mixed to get leaves standstill, separatory, obtain aqueous phase and organic phase, wherein, be dissolved with ethylene glycol in described aqueous phase, described organic phase is isooctyl alcohol, aqueous phase obtains ethylene glycol finished product after distillation and concentration, and organic phase uses as the feedstock circulation preparing Di-2-ethylhexyl terephthalate.
Described Di-2-ethylhexyl terephthalate crude product carried out successively neutralize, wash, after stripping and dehydration, then through charcoal absorption and filtering sorbent material, obtain Di-2-ethylhexyl terephthalate goods.
Carry out mass spectroscopy to described Di-2-ethylhexyl terephthalate goods, result shows that the goods that the present embodiment obtains are Di-2-ethylhexyl terephthalate.
Carry out gas chromatographic analysis to described Di-2-ethylhexyl terephthalate goods, calculate the purity of Di-2-ethylhexyl terephthalate in goods according to gas chromatographic analysis result, result is: 97 ~ 99%.
The yield of Di-2-ethylhexyl terephthalate goods calculates, and result is that yield reaches 91%.
Embodiment 2
Polyethylene terephthalate waste material (number-average molecular weight is preferably 70000 ~ 110000) is rinsed well with water, puts into baking oven, and temperature controls to dry 0.8h at 130 ~ 140 DEG C, and the waste material pulverizer after oven dry is ground into powder.Accurately take wasted powder 384g, isooctyl alcohol 624g puts into the high-temperature high-pressure reaction kettle of 2000mL, adds 1g tetrabutyl titanate, be warmed up to 200 ~ 210 DEG C, the reaction times is 6h, and reaction terminates rear vacuum pump suction filtration, filtrate is carried out vacuum distilling, collects distillate.Wherein, what collect before 225 DEG C is the mixture of isooctyl alcohol and ethylene glycol; More than 225 DEG C collect be Di-2-ethylhexyl terephthalate crude product.
The mixture of described isooctyl alcohol and ethylene glycol is mixed with water, the mixed solution be mixed to get leaves standstill, separatory, obtain aqueous phase and organic phase, wherein, be dissolved with ethylene glycol in described aqueous phase, described organic phase is isooctyl alcohol, aqueous phase obtains ethylene glycol finished product after distillation and concentration, and organic phase uses as the feedstock circulation preparing Di-2-ethylhexyl terephthalate.
Described Di-2-ethylhexyl terephthalate crude product carried out successively neutralize, wash, after stripping and dehydration, then through charcoal absorption and filtering sorbent material, obtain Di-2-ethylhexyl terephthalate goods.
Carry out mass spectroscopy to described Di-2-ethylhexyl terephthalate goods, result shows that the goods that the present embodiment obtains are Di-2-ethylhexyl terephthalate.
Carry out gas chromatographic analysis to described Di-2-ethylhexyl terephthalate goods, calculate the purity of Di-2-ethylhexyl terephthalate in goods according to gas chromatographic analysis result, result is: 97 ~ 99%.
The yield of Di-2-ethylhexyl terephthalate goods calculates, and result is that yield reaches 91.8%.
Embodiment 3
Polyethylene terephthalate waste material (number-average molecular weight is preferably 70000 ~ 110000) is rinsed well with water, puts into baking oven, and temperature controls to dry 0.8h at 130 ~ 140 DEG C, and the waste material pulverizer after oven dry is ground into powder.Accurately take wasted powder 384g, isooctyl alcohol 624g puts into the high-temperature high-pressure reaction kettle of 2000mL, adds 1g tetrabutyl titanate, be warmed up to 200 ~ 210 DEG C, the reaction times is 6h, and reaction terminates rear vacuum pump suction filtration, filtrate is carried out vacuum distilling, collects distillate.Wherein, what collect before 225 DEG C is the mixture of isooctyl alcohol and ethylene glycol; More than 225 DEG C collect be Di-2-ethylhexyl terephthalate crude product.
The mixture of described isooctyl alcohol and ethylene glycol is mixed with water, the mixed solution be mixed to get leaves standstill, separatory, obtain aqueous phase and organic phase, wherein, be dissolved with ethylene glycol in described aqueous phase, described organic phase is isooctyl alcohol, aqueous phase obtains ethylene glycol finished product after distillation and concentration, and organic phase uses as the feedstock circulation preparing Di-2-ethylhexyl terephthalate.
Described Di-2-ethylhexyl terephthalate crude product carried out successively neutralize, wash, after stripping and dehydration, then through charcoal absorption and filtering sorbent material, obtain Di-2-ethylhexyl terephthalate goods.
Carry out mass spectroscopy to described Di-2-ethylhexyl terephthalate goods, result shows that the goods that the present embodiment obtains are Di-2-ethylhexyl terephthalate.
Carry out gas chromatographic analysis to described Di-2-ethylhexyl terephthalate goods, calculate the purity of Di-2-ethylhexyl terephthalate in goods according to gas chromatographic analysis result, result is: 97 ~ 99%.
The yield of Di-2-ethylhexyl terephthalate goods calculates, and result is that yield reaches 91.5%.
Embodiment 4
Polyethylene terephthalate waste material (number-average molecular weight is preferably 70000 ~ 110000) is rinsed well with water, puts into baking oven, and temperature controls to dry 0.8h at 130 ~ 140 DEG C, and the waste material pulverizer after oven dry is ground into powder.Accurately take wasted powder 384g, isooctyl alcohol 624g puts into the high-temperature high-pressure reaction kettle of 2000mL, adds 1g tetrabutyl titanate, be warmed up to 200 ~ 210 DEG C, the reaction times is 6h, and reaction terminates rear vacuum pump suction filtration, filtrate is carried out vacuum distilling, collects distillate.Wherein, what collect before 225 DEG C is the mixture of isooctyl alcohol and ethylene glycol; More than 225 DEG C collect be Di-2-ethylhexyl terephthalate crude product.
The mixture of described isooctyl alcohol and ethylene glycol is mixed with water, the mixed solution be mixed to get leaves standstill, separatory, obtain aqueous phase and organic phase, wherein, be dissolved with ethylene glycol in described aqueous phase, described organic phase is isooctyl alcohol, aqueous phase obtains ethylene glycol finished product after distillation and concentration, and organic phase uses as the feedstock circulation preparing Di-2-ethylhexyl terephthalate.
Described Di-2-ethylhexyl terephthalate crude product carried out successively neutralize, wash, after stripping and dehydration, then through charcoal absorption and filtering sorbent material, obtain Di-2-ethylhexyl terephthalate goods.
Carry out mass spectroscopy to described Di-2-ethylhexyl terephthalate goods, result shows that the goods that the present embodiment obtains are Di-2-ethylhexyl terephthalate.
Carry out gas chromatographic analysis to described Di-2-ethylhexyl terephthalate goods, calculate the purity of Di-2-ethylhexyl terephthalate in goods according to gas chromatographic analysis result, result is: 97 ~ 99%.
The yield of Di-2-ethylhexyl terephthalate goods calculates, and result is that yield reaches 92.0%.
Can be found out by above-mentioned 4 embodiments, when adopting method provided by the invention to prepare phthalic acid di-isooctyl goods, the goods purity of 4 embodiments is suitable with yield, illustrates that method provided by the invention has satisfactory stability.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (10)
1. utilize poly terephthalic acid diol ester waste material to prepare a method for terephthalate, comprise the following steps:
A), poly terephthalic acid diol ester waste material and monohydroxy-alcohol react under titanic acid ester catalytic condition in closed reactor, obtains reaction solution;
Described poly terephthalic acid diol ester waste material is one or more in polyethylene terephthalate waste material, Poly(Trimethylene Terephthalate) waste material and polybutylene terephthalate waste material;
Described monohydroxy-alcohol is one or more in butanols, amylalcohol, hexanol, enanthol, octanol, nonyl alcohol and decyl alcohol;
The temperature of described reaction is 200 ~ 220 DEG C;
B), described reaction solution carries out aftertreatment, obtains terephthalate.
2. method according to claim 1, is characterized in that, the described number of ester groups of poly terephthalic acid diol ester waste material and the mol ratio of monohydroxy-alcohol are 1:(1 ~ 2).
3. method according to claim 1, is characterized in that, described titanic acid ester comprises tetrabutyl titanate and/or titanium isopropylate.
4. method according to claim 3, is characterized in that, the mass ratio of described poly terephthalic acid diol ester waste material and titanic acid ester is (200 ~ 500): 1.
5. method according to claim 1, is characterized in that, step a) in, the time of described reaction is 2 ~ 10h.
6. method according to claim 1, is characterized in that, the number-average molecular weight of described poly terephthalic acid diol ester waste material is 70000 ~ 110000.
7. method according to claim 1, is characterized in that, described step b) specifically comprise:
B1), described reaction solution distills, and obtains terephthalate crude product and alcohol mixture;
Described alcohol mixture comprises ethylene glycol and described monohydroxy-alcohol;
B2), described terephthalate crude product carries out washing and decolouring successively, obtains terephthalate.
8. method according to claim 7, is characterized in that, step b1) in, described reaction solution first filters, then distills filtering the filtrate obtained.
9. method according to claim 7, is characterized in that, also comprises: described alcohol mixture is separated, and obtains ethylene glycol and monohydroxy-alcohol.
10. the method according to any one of claim 1 ~ 9, it is characterized in that, step a) in, described poly terephthalic acid diol ester waste material first successively through washing, dry and after pulverizing, then reacts under titanic acid ester catalytic condition with monohydroxy-alcohol in closed reactor.
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| CN201510929412.8A CN105503605A (en) | 2015-12-14 | 2015-12-14 | Method for preparing dimethyl terephthalate from polybutylene terephthalate waste material |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109311798A (en) * | 2016-06-27 | 2019-02-05 | 沙特基础工业全球技术有限公司 | For the method by recycling raw material preparation dimethyl terephthalate ester |
| CN112724014A (en) * | 2019-10-28 | 2021-04-30 | 南亚塑胶工业股份有限公司 | Preparation method and decoloring method of dioctyl terephthalate |
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| CN1073164A (en) * | 1991-12-13 | 1993-06-16 | 化学工业部成都有机硅应用研究技术服务中心 | Produce softening agent with the polyester waste material single stage method |
| JP2000256274A (en) * | 1999-03-11 | 2000-09-19 | Hokoku Seiyu Kk | Production of terephthalic acid diester and its composition |
| CN101531594A (en) * | 2008-03-14 | 2009-09-16 | 长春人造树脂厂股份有限公司 | Method for preparing high-purity diesters of terephthalate acid from polyethylene terephthalate wastes |
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- 2015-12-14 CN CN201510929412.8A patent/CN105503605A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1073164A (en) * | 1991-12-13 | 1993-06-16 | 化学工业部成都有机硅应用研究技术服务中心 | Produce softening agent with the polyester waste material single stage method |
| JP2000256274A (en) * | 1999-03-11 | 2000-09-19 | Hokoku Seiyu Kk | Production of terephthalic acid diester and its composition |
| CN101531594A (en) * | 2008-03-14 | 2009-09-16 | 长春人造树脂厂股份有限公司 | Method for preparing high-purity diesters of terephthalate acid from polyethylene terephthalate wastes |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109311798A (en) * | 2016-06-27 | 2019-02-05 | 沙特基础工业全球技术有限公司 | For the method by recycling raw material preparation dimethyl terephthalate ester |
| CN112724014A (en) * | 2019-10-28 | 2021-04-30 | 南亚塑胶工业股份有限公司 | Preparation method and decoloring method of dioctyl terephthalate |
| CN112724014B (en) * | 2019-10-28 | 2024-01-09 | 南亚塑胶工业股份有限公司 | Preparation method and decoloring method of dioctyl terephthalate |
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