CN105111063A - Method for preparing terephthalic acid by using waste polyester and cotton fiber - Google Patents
Method for preparing terephthalic acid by using waste polyester and cotton fiber Download PDFInfo
- Publication number
- CN105111063A CN105111063A CN201510458505.7A CN201510458505A CN105111063A CN 105111063 A CN105111063 A CN 105111063A CN 201510458505 A CN201510458505 A CN 201510458505A CN 105111063 A CN105111063 A CN 105111063A
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- China
- Prior art keywords
- autoclave
- terephthalic acid
- waste
- polyester fiber
- old polyester
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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
- C07C51/09—Preparation of carboxylic acids or their salts, halides or anhydrides from carboxylic acid esters or lactones
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/09—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by hydrolysis
- C07C29/095—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by hydrolysis of esters of organic acids
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a method for preparing terephthalic acid by using waste polyester and cotton fiber. Aiming at the condition that waste polyester and cotton fiber is large in stock, severe in pollution and hard to recover, the method uses the waste polyester and cotton fiber as raw materials and performs washing, disinfection, high pressure degradation and separation to strip color, drying and grinding to prepare a terephthalic acid product. Meanwhile, a byproduct ethylene glycol is further separated. The preparation method is advanced in process and accurate, full and accurate in data, and the prepared and separated product is good in quality and high in purity. The purity can reach 99.973%. The product is powdery, the diameter of the powdery particles is less than or equal to 2[mu]m, and the terephthalic acid can be recycled as chemical raw materials, so that the method is the very advanced method for preparing terephthalic acid by using waste polyester and cotton fiber.
Description
Technical field
The present invention relates to a kind of method preparing terephthalic acid with waste and old polyester fiber, belong to the technical field of the recycling of waste and old polyester fiber, preparative chemistry material.
Background technology
Polyester cotton is the fabric that terylene short fiber peacekeeping cotton fibre mix spinning is made into, and conventional blending ratio is terylene: cotton fibre=70:30, and in polyester-cotton fabric, major part is terylene; Terylene is with terephthalic acid and ethylene glycol for raw material, the superpolymer-polyethylene terephthalate made through esterification and polycondensation, makes polyster fibre, then make polyester cotton through synthesis spinning.
In textile industry, polyester cotton occupies very large ratio, because polyester cotton intensity is good, good toughness, wear-resisting durable, not easy to wear, long service life, be commonly used to make polyester cotton blending clothing, industrial drop cloth, travelling belt, rope for traction etc., in industrial application and daily life, application is more and more.
Because polyester cotton is more and more in industry and daily use, the waste and old polyester cotton produced also increases thereupon, the waste and old polyester cotton that China produces every year is greatly about 3,000 ten thousand tons, recovery utilization rate is less than 10%, due to the backwardness of recovery technology, waste and old polyester cotton is buried or burning often, causes the serious wasting of resources and environmental pollution, how to have become important research topic to waste and old polyester fiber recycling.
Summary of the invention
Goal of the invention
The object of the invention is the situation for background technology, with waste and old polyester fiber for raw material, be separated through washing, rinsing, sterilization, High Temperature High Pressure strip, dry, grinding, make terephthalic acid, to reach the object with waste and old polyester fiber recycling.
Technical scheme
The chemical substance material that the present invention uses is: waste and old polyester fiber, manganese acetate, high-carbon fatty alcohol polyoxyethylene ether, activated carbon, DMF, dehydrated alcohol, deionized water, and it is as follows that it prepares consumption: with gram, milliliter for measure unit
Waste and old polyester fiber: (C
39h
44o
22)
nn=6000-15000,10g ± 0.01g
Activated carbon: C, 10g ± 0.01g
Manganese acetate: C
4h
6mnO
4, 0.1g ± 0.01g
DMF: C
3h
7nO, 50mL ± 0.01mL
Dehydrated alcohol: C
2h
5o, 100mL ± 5mL
High-carbon fatty alcohol polyoxyethylene ether: C
14o (CH
2cH
2o)
9h, 2mL ± 0.01mL
Deionized water: H
2o, 3000mL ± 50mL
Preparation method is as follows:
(1) the waste and old polyester fiber of pre-treatment
1. wash, waste and old polyester fiber 10g ± 0.01g is placed in washer, add deionized water 200mL, high-carbon fatty alcohol polyoxyethylene ether 2mL ± 0.01mL;
Turn on agitator, agitator treating 12min;
2. rinsing, is placed in beaker by the waste and old polyester fiber after washing, adds deionized water 200mL, stirs rinsing 3min;
Stir rinsing and repeat 4 times;
3. dry, the waste and old polyester fiber after rinsing is placed in loft drier dry, drying temperature 100 DEG C, time of drying 60min;
4. sterilize, dried waste and old polyester fiber is placed in ultraviolet disinfection case, carries out airtight sterilization, voltage 220V, power 40W, disinfecting time 30min;
5. shear, the waste and old polyester fiber after sterilization is cut into bulk, lumpy sizes≤10mm × 10mm;
(2) degrading waste polyester fiber
The degraded of waste and old polyester fiber is carried out in autoclave, completes in heating, whipping process;
1. clean autoclave, open autoclave, add deionized water 200mL, cleaning autoclave inwall, makes it clean;
Cleaning repeats 3 times, dries after cleaning;
2. prepare reaction solution, take waste and old polyester fiber 10g ± 0.01g, activated carbon 10g ± 0.01g, manganese acetate 0.1g ± 0.01g, measure deionized water 100mL ± 1mL, add in beaker, stir 10min, become mixed solution;
3. mixed solution is added in autoclave, and airtight;
4. open autoclave, and heat, Heating temperature 240 DEG C ± 1 DEG C, autoclave internal pressure is 3.3MPa, autoclave agitation revolution 100r/min, reaction times 7h;
To there is physical-chemical reaction in mixing solutions, cotton fibre carbonization, terylene hydrolysis, color divest in heating, reaction process;
Stop heating after reaction, mixed solution is cooled to 25 DEG C with still, obtains suspension liquid;
(3) product separation
1. solid-liquid separation, is placed in the Büchner funnel of filter flask by suspension liquid, carry out suction filtration with millipore filtration, filter cake retained by filter membrane, filtrate is evacuated in filter flask, and collects respectively;
2. extract ethylene glycol, filtrate is placed in distilling flask, be placed in by distilling flask on electric heating agitator, Heating temperature 197 DEG C ± 1 DEG C, heated and stirred, obtains liquid fraction, i.e. ethylene glycol, and collects;
3. prepare parting liquid, filter cake is placed in beaker, then add DMF 50mL ± 0.01mL, stir 5min;
Then beaker is placed in heated and stirred on electric heating agitator, Heating temperature 70 DEG C ± 1 DEG C, heats and stirs, and terephthalic acid is fully dissolved in the solution, becomes parting liquid;
4. suction filtration, is placed in the Büchner funnel of filter flask by parting liquid, carry out suction filtration with millipore filtration, filter membrane is retained filter cake, filtrate suction filtration in filter flask, and is collected respectively;
5. wash and reclaim activated carbon, filter cake is placed in beaker, adding dehydrated alcohol 100mL ± 5mL, stirring 10min;
Then carry out suction filtration with millipore filtration, obtain filter cake;
Then filter cake deionized water is carried out washing, suction filtration, obtain filter cake;
Filter cake is placed in loft drier dry, drying temperature 120 DEG C, time of drying, 2h, reclaimed activated carbon after drying;
6. separation and Extraction terephthalic acid, adds filtrate in beaker, then adds deionized water 50mL, stirs 5min, becomes suspension liquid;
Added by suspension liquid in centrifuge tube, whizzer carries out centrifugation, be separated revolution 8000r/min, disengaging time 8min, retains throw out after separation, abandoning supernatant;
Throw out is placed in beaker, adds deionized water 200mL, agitator treating 5min, then filter with three layers of middling speed qualitative filter paper, retain filter cake, discard washings;
Filter cake is placed in vacuum drying oven dry, drying temperature 110 DEG C, vacuum tightness 10Pa, time of drying, 6h, obtained solid matter, i.e. terephthalic acid after drying;
(4) grind, sieve
Dried solid matter terephthalic acid agate mortar, pestle are ground, then sieves with 600 eye mesh screens;
Grind, sieve and repeatedly carry out, obtain end product terephthalic acid white powder;
(5) detect, analyze, characterize
The color and luster of terephthalic acid of preparation, pattern, chemical physics performance, purity are detected, analyze, characterized;
The micromorphology analysis of terephthalic acid is carried out by scanning electronic microscope;
The image structural analysis of terephthalic acid is carried out with X-ray diffractometer;
Conclusion: terephthalic acid is white powder, powder granule diameter≤2 μm, and product purity reaches 99.973%;
(6) product storage
Be stored in respectively in the Glass Containers of amber transparent the terephthalic acid prepared, ethylene glycol, airtight shading is preserved, and moistureproof, sun-proof, anti-acid-alkali salt to corrode, storing temp 20 DEG C, relative humidity≤10%.
Beneficial effect
The present invention has obvious advance compared with background technology, many for waste and old polyester fiber storage, seriously polluted, reclaim difficult situation, waste and old polyester fiber is washed, sterilization, high pressure degraded separation is stripped, dry, grinding, make terephthalic acid product, also isolated by product ethylene glycol simultaneously, this preparation method's technique is advanced, data are accurately full and accurate, the product quality that preparative separation goes out is good, purity is high, purity can reach 99.973%, product is powder, powder granule diameter≤2 μm, chemical feedstocks can be made re-use, it is the very advanced method preparing terephthalic acid and by product with waste and old polyester fiber.
Accompanying drawing explanation
Fig. 1, waste and old polyester fiber degraded state graph
The terephthalic acid shape appearance figure of Fig. 2, preparation
The terephthalic acid diffracted intensity collection of illustrative plates of Fig. 3, preparation
Shown in figure, list of numerals is as follows:
1, agitator, 2, bolt, 3, kettle cover, 4, thermal insulation layer, 5, autoclave, 6, resistance heater, 7, reaction solution, 8, still seat, 9, wire, 10, agitator motor, 11, feed belt, 12, tensimeter, 13, thermopair, 14, electric control box, 15, agitation revolution display screen, 16, temperature in the kettle display screen, 17, stir switch, 18, power switch, 19, Heating temperature modulator, 20, agitation revolution modulator.
Embodiment
Once the invention will be further described by reference to the accompanying drawings:
Shown in Fig. 1, be waste and old polyester fiber degraded state graph, each position wants correct, and proportioning according to quantity, operates according to the order of sequence.
The value preparing the chemical substance used first is determined by the scope pre-set, with gram, milliliter, millimeter for measure unit.
Autoclave 5 is rectangle, is resistance heater 6 in the outside of autoclave 5, is thermal insulation layer 4, the bottom of autoclave 5 is still seat 8, top is kettle cover 3, and is fixed by bolt 2, is reaction solution 7 in autoclave 5 in resistance heater 6 outside; Be provided with agitator 1 in the mid-way of kettle cover 3, and go deep in autoclave 5; Be provided with thermopair 13, tensimeter 12 at the sidepiece of kettle cover 3, and go deep in autoclave 5; Be provided with agitator motor 10 at the right part of autoclave 5, agitator motor 10 connects agitator 1 by travelling belt 11; Be provided with electric control box 14 in the right side of autoclave 5, electric control box 14 be provided with agitation revolution display screen 15, temperature in the kettle display screen 16, stir switch 17, power switch 18, Heating temperature modulator 19, agitation revolution modulator 20; Be connected by wire 9 between autoclave 5 with electric control box 14.
Shown in Fig. 2, be the terephthalic acid shape appearance figure of preparation, shown in figure, product terephthalic acid is powder, in irregular stacking.
Shown in Fig. 3, be the terephthalic acid diffracted intensity collection of illustrative plates of preparation, shown in figure, product diffraction peak is terephthalic acid characteristic peak.
Claims (2)
1. prepare a method for terephthalic acid with waste and old polyester fiber, it is characterized in that:
The chemical substance material used is: waste and old polyester fiber, manganese acetate, high-carbon fatty alcohol polyoxyethylene ether, activated carbon, DMF, dehydrated alcohol, deionized water, and it is as follows that it prepares consumption: with gram, milliliter for measure unit
Waste and old polyester fiber: (C
39h
44o
22)
nn=6000-15000,10g ± 0.01g
Activated carbon: C, 10g ± 0.01g
Manganese acetate: C
4h
6mnO
4, 0.1g ± 0.01g
DMF: C
3h
7nO, 50mL ± 0.01mL
Dehydrated alcohol: C
2h
5o, 100mL ± 5mL
High-carbon fatty alcohol polyoxyethylene ether: C
14o (CH
2cH
2o)
9h, 2mL ± 0.01mL
Deionized water: H
2o, 3000mL ± 50mL
Preparation method is as follows:
(1) the waste and old polyester fiber of pre-treatment
1. wash, waste and old polyester fiber 10g ± 0.01g is placed in washer, add deionized water 200mL, high-carbon fatty alcohol polyoxyethylene ether 2mL ± 0.01mL;
Turn on agitator, agitator treating 12min;
2. rinsing, is placed in beaker by the waste and old polyester fiber after washing, adds deionized water 200mL, stirs rinsing 3min;
Stir rinsing and repeat 4 times;
3. dry, the waste and old polyester fiber after rinsing is placed in loft drier dry, drying temperature 100 DEG C, time of drying 60min;
4. sterilize, dried waste and old polyester fiber is placed in ultraviolet disinfection case, carries out airtight sterilization, voltage 220V, power 40W, disinfecting time 30min;
5. shear, the waste and old polyester fiber after sterilization is cut into bulk, lumpy sizes≤10mm × 10mm;
(2) degrading waste polyester fiber
The degraded of waste and old polyester fiber is carried out in autoclave, completes in heating, whipping process;
1. clean autoclave, open autoclave, add deionized water 200mL, cleaning autoclave inwall, makes it clean;
Cleaning repeats 3 times, dries after cleaning;
2. prepare reaction solution, take waste and old polyester fiber 10g ± 0.01g, activated carbon 10g ± 0.01g, manganese acetate 0.1g ± 0.01g, measure deionized water 100mL ± 1mL, add in beaker, stir 10min, become mixed solution;
3. mixed solution is added in autoclave, and airtight;
4. open autoclave, and heat, Heating temperature 240 DEG C ± 1 DEG C, autoclave internal pressure is 3.3MPa, autoclave agitation revolution 100r/min, reaction times 7h;
To there is physical-chemical reaction in mixing solutions, cotton fibre carbonization, terylene hydrolysis, color divest in heating, reaction process;
Stop heating after reaction, mixed solution is cooled to 25 DEG C with still, obtains suspension liquid;
(3) product separation
1. solid-liquid separation, is placed in the Büchner funnel of filter flask by suspension liquid, carry out suction filtration with millipore filtration, filter cake retained by filter membrane, filtrate is evacuated in filter flask, and collects respectively;
2. extract ethylene glycol, filtrate is placed in distilling flask, be placed in by distilling flask on electric heating agitator, Heating temperature 197 DEG C ± 1 DEG C, heated and stirred, obtains liquid fraction, i.e. ethylene glycol, and collects;
3. prepare parting liquid, filter cake is placed in beaker, then add DMF 50mL ± 0.01mL, stir 5min;
Then beaker is placed in heated and stirred on electric heating agitator, Heating temperature 70 DEG C ± 1 DEG C, heats and stirs, and terephthalic acid is fully dissolved in the solution, becomes parting liquid;
4. suction filtration, is placed in the Büchner funnel of filter flask by parting liquid, carry out suction filtration with millipore filtration, filter membrane is retained filter cake, filtrate suction filtration in filter flask, and is collected respectively;
5. wash and reclaim activated carbon, filter cake is placed in beaker, adding dehydrated alcohol 100mL ± 5mL, stirring 10min;
Then carry out suction filtration with millipore filtration, obtain filter cake;
Then filter cake deionized water is carried out washing, suction filtration, obtain filter cake;
Filter cake is placed in loft drier dry, drying temperature 120 DEG C, time of drying, 2h, reclaimed activated carbon after drying;
6. separation and Extraction terephthalic acid, adds filtrate in beaker, then adds deionized water 50mL, stirs 5min, becomes suspension liquid;
Added by suspension liquid in centrifuge tube, whizzer carries out centrifugation, be separated revolution 8000r/min, disengaging time 8min, retains throw out after separation, abandoning supernatant;
Throw out is placed in beaker, adds deionized water 200mL, agitator treating 5min, then filter with three layers of middling speed qualitative filter paper, retain filter cake, discard washings;
Filter cake is placed in vacuum drying oven dry, drying temperature 110 DEG C, vacuum tightness 10Pa, time of drying, 6h, obtained solid matter, i.e. terephthalic acid after drying;
(4) grind, sieve
Dried solid matter terephthalic acid agate mortar, pestle are ground, then sieves with 600 eye mesh screens;
Grind, sieve and repeatedly carry out, obtain end product terephthalic acid white powder;
(5) detect, analyze, characterize
The color and luster of terephthalic acid of preparation, pattern, chemical physics performance, purity are detected, analyze, characterized;
The micromorphology analysis of terephthalic acid is carried out by scanning electronic microscope;
The image structural analysis of terephthalic acid is carried out with X-ray diffractometer;
Conclusion: terephthalic acid is white powder, powder granule diameter≤2 μm, and product purity reaches 99.973%;
(6) product storage
Be stored in respectively in the Glass Containers of amber transparent the terephthalic acid prepared, ethylene glycol, airtight shading is preserved, and moistureproof, sun-proof, anti-acid-alkali salt to corrode, storing temp 20 DEG C, relative humidity≤10%.
2. a kind of method preparing terephthalic acid with waste and old polyester fiber according to claim 1, is characterized in that:
Autoclave (5) is rectangle, be resistance heater (6) in the outside of autoclave (5), be thermal insulation layer (4) in resistance heater (6) outside, the bottom of autoclave (5) is still seat (8), top is kettle cover (3), and fixed by bolt (2), be reaction solution (7) in autoclave (5); Be provided with agitator (1) in the mid-way of kettle cover (3), and go deep in autoclave (5); Be provided with thermopair (13), tensimeter (12) at the sidepiece of kettle cover (3), and go deep in autoclave (5); Be provided with agitator motor (10) at the right part of autoclave (5), agitator motor (10) connects agitator (1) by travelling belt (11); Be provided with electric control box (14) in the right side of autoclave (5), electric control box (14) be provided with agitation revolution display screen (15), temperature in the kettle display screen (16), stir switch (17), power switch (18), Heating temperature modulator (19), agitation revolution modulator (20); Be connected by wire (9) between autoclave (5) with electric control box (14).
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510458505.7A CN105111063B (en) | 2015-07-30 | 2015-07-30 | A kind of method that terephthalic acid (TPA) is prepared with waste and old polyester fiber |
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|---|---|---|---|
| CN201510458505.7A CN105111063B (en) | 2015-07-30 | 2015-07-30 | A kind of method that terephthalic acid (TPA) is prepared with waste and old polyester fiber |
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| CN105111063A true CN105111063A (en) | 2015-12-02 |
| CN105111063B CN105111063B (en) | 2017-05-31 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106000230A (en) * | 2016-07-27 | 2016-10-12 | 升华集团德清华源颜料有限公司 | High-pressure reaction vessel special for preparation of low-length/diameter-ratio iron oxide yellow |
| CN110237888A (en) * | 2019-05-13 | 2019-09-17 | 杭州谈笑电子商务有限公司 | A kind of alcohol extraction procedure |
| WO2022047843A1 (en) * | 2020-09-07 | 2022-03-10 | 苏州贤辉新纺织科技有限公司 | Technological method for regenerating flame retardant polyester fiber by recycling polyester fiber |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106000230A (en) * | 2016-07-27 | 2016-10-12 | 升华集团德清华源颜料有限公司 | High-pressure reaction vessel special for preparation of low-length/diameter-ratio iron oxide yellow |
| CN110237888A (en) * | 2019-05-13 | 2019-09-17 | 杭州谈笑电子商务有限公司 | A kind of alcohol extraction procedure |
| WO2022047843A1 (en) * | 2020-09-07 | 2022-03-10 | 苏州贤辉新纺织科技有限公司 | Technological method for regenerating flame retardant polyester fiber by recycling polyester fiber |
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|---|---|
| CN105111063B (en) | 2017-05-31 |
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