CN105111063B - A kind of method that terephthalic acid (TPA) is prepared with waste and old polyester fiber - Google Patents
A kind of method that terephthalic acid (TPA) is prepared with waste and old polyester fiber Download PDFInfo
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- CN105111063B CN105111063B CN201510458505.7A CN201510458505A CN105111063B CN 105111063 B CN105111063 B CN 105111063B CN 201510458505 A CN201510458505 A CN 201510458505A CN 105111063 B CN105111063 B CN 105111063B
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- terephthalic acid
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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
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- 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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- 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 present invention relates to a kind of method that terephthalic acid (TPA) is prepared with waste and old polyester fiber, it is directed to waste and old polyester fiber storage many, it is seriously polluted, reclaim difficult situation, waste and old polyester fiber is washed, sterilization, high pressure degraded separation is stripped, dry, grinding, it is made terephthalic acid product, accessory substance ethylene glycol is also isolated simultaneously, this preparation method technique is advanced, data are accurately full and accurate, the product quality that preparative separation goes out is good, purity is high, purity is up to 99.973%, product is powder, powder granule diameter≤2 μm, chemical raw material re-using can be made, it is the highly advanced method that terephthalic acid (TPA) is prepared with waste and old polyester fiber.
Description
Technical field
The present invention relates to a kind of method that terephthalic acid (TPA) is prepared with waste and old polyester fiber, belong to waste and old polyester fiber and reclaim profit
With, prepare chemical substance technical field.
Background technology
Polyester cotton is the fabric that terylene short fiber peacekeeping cotton fiber mix spinning is made into, and conventional mixed proportion is to wash
Synthetic fibre:Cotton fiber=70:30, major part is terylene in polyester-cotton fabric；Terylene is with terephthalic acid (TPA) and ethylene glycol as raw material, through ester
Change and polycondensation reaction and high polymer-polyethylene terephthalate for being made, be made polyster fibre through synthesizing spinning, then
It is made polyester cotton.
In textile industry, polyester cotton occupies very big ratio, because polyester cotton intensity is good, toughness
Good, wear-resisting durable, not easy to wear, long service life, is commonly used to make polyester cotton blending clothing, industrial drop cloth, conveyer belt, drawing
Using more and more in rope etc., commercial Application and daily life.
Because polyester cotton is more and more in industry and daily use, the waste and old polyester cotton of generation also with
Increase, China every year produce waste and old polyester cotton about at 30,000,000 tons, recovery utilization rate is less than 10%, due to
The backwardness of recovery technology, waste and old polyester cotton is often buried or burns, and causes the serious wasting of resources and environmental pollution,
How waste and old polyester fiber is recycled has turned into important research topic.
The content of the invention
Goal of the invention
The purpose of the present invention is directed to the situation of background technology, scrubbed, rinse, disappear with waste and old polyester fiber as raw material
Poison, HTHP separate and strip, dry, grinding, and terephthalic acid (TPA) are made, to reach with waste and old polyester fiber recycling
Purpose.
Technical scheme
The chemical substance material that the present invention is used is：Waste and old polyester fiber, manganese acetate, high-carbon fatty alcohol polyoxyethylene ether,
Activated carbon, DMF, absolute ethyl alcohol, deionized water, it is as follows that it prepares consumption：It is measurement unit with gram, milliliter
Waste and old polyester fiber：(C39H44O22)nN=6000-15000,10g ± 0.01g
Activated carbon：C, 10g ± 0.01g
Manganese acetate：C4H6MnO4, 0.1g ± 0.01g
N,N-dimethylformamide：C3H7NO, 50mL ± 0.01mL
Absolute ethyl alcohol：C2H5O, 100mL ± 5mL
High-carbon fatty alcohol polyoxyethylene ether：C14O(CH2CH2O)9H, 2mL ± 0.01mL
Deionized water：H2O, 3000mL ± 50mL
Preparation method is as follows：
(1) waste and old polyester fiber is pre-processed
1. wash, waste and old polyester fiber 10g ± 0.01g are placed in washer, add deionized water 200mL, high-carbon fat
Fat alcohol APEO 2mL ± 0.01mL；
Turn on agitator, agitator treating 12min；
2. rinse, by washing after waste and old polyester fiber be placed in beaker, add deionized water 200mL, stirring rinsing
3min；
Stirring rinsing repeats 4 times；
3. dry, by rinsing after waste and old polyester fiber be placed in drying box dry, 100 DEG C of drying temperature, drying time
60min；
4. sterilize, dried waste and old polyester fiber is placed in ultraviolet disinfection case, carry out closed sterilization, voltage
220V, power 40W, disinfecting time 30min；
5. shear, by sterilization after waste and old polyester fiber 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, is completed in heating, whipping process；
1. autoclave is cleaned, autoclave is opened, deionized water 200mL is added, autoclave inwall is cleaned,
Make it clean；
Cleaning repeats 3 times, is dried after cleaning；
2. prepare reaction solution, weigh waste and old polyester fiber 10g ± 0.01g, activated carbon 10g ± 0.01g, manganese acetate 0.1g ±
0.01g, measures deionized water 100mL ± 1mL, adds in beaker, 10min is stirred, into mixed liquor；
3. mixed liquor is added in autoclave, and it is closed；
4. autoclave is opened, and is heated, 240 DEG C ± 1 DEG C of heating-up temperature, pressure is 3.3MPa in autoclave,
Autoclave agitation revolution 100r/min, reaction time 7h；
Mixed solution will occur physical-chemical reaction, cotton fiber carbonization, terylene hydrolysis, color in heating, course of reaction
Divest；
Stop heating after reaction, mixed liquor is cooled to 25 DEG C, obtains suspension with kettle；
(3) product is separated
1. separation of solid and liquid, suspension is placed in the Buchner funnel of bottle,suction, and suction filtration is carried out with miillpore filter, is stayed on filter membrane
Filter cake is deposited, filtrate is evacuated in filter flask, and is collected respectively；
2. ethylene glycol is extracted, filtrate is placed in distilling flask, distilling flask is placed on electric heating agitator, heating-up temperature
197 DEG C ± 1 DEG C, heating stirring obtains liquid fraction, i.e. ethylene glycol, and collect；
3. separating liquid is prepared, filter cake is placed in beaker, be subsequently adding DMF 50mL ± 0.01mL, stirred
Mix 5min；
Then beaker is placed in heating stirring on electric heating agitator, 70 DEG C ± 1 DEG C of heating-up temperature is heated and stirred, and it is right to make
Phthalic acid is substantially dissolved in solution, into separating liquid；
4. suction filtration, separating liquid is placed in the Buchner funnel of bottle,suction, and suction filtration is carried out with miillpore filter, and filter is retained on filter membrane
In cake, filtrate suction filtration to filter flask, and collect respectively；
5. activated carbon is washed and is reclaimed, filter cake is placed in beaker, add absolute ethyl alcohol 100mL ± 5mL, stir 10min；
Then suction filtration is carried out with miillpore filter, obtains filter cake；
Then filter cake is washed with deionized water, suction filtration, obtain filter cake；
Filter cake is placed in drying box and is dried, 120 DEG C of drying temperature, drying time 2h reclaims activated carbon after drying；
6. separation and Extraction terephthalic acid (TPA), by filtrate addition beaker, is subsequently adding deionized water 50mL, stirs 5min,
Into suspension；
Suspension is added in centrifuge tube, is centrifuged on centrifuge, revolution 8000r/min is separated, during separation
Between 8min, sediment, abandoning supernatant are retained after separation；
Put the precipitate in beaker, add deionized water 200mL, agitator treating 5min, it is then qualitative with three layers of middling speed
Filter paper is filtered, and retains filter cake, discards cleaning solution；
Filter cake is placed in vacuum drying chamber and is dried, 110 DEG C of drying temperature, vacuum 10Pa, drying time 6h, after drying
Obtain solid matter, i.e. terephthalic acid (TPA)；
(4) grind, sieve
Dried solid matter terephthalic acid (TPA) agate mortar, pestle are ground, then with 600 eye mesh screen mistakes
Sieve；
Grinding, sieving are repeated, and obtain end-product terephthalic acid (TPA) white powder；
(5) detect, analyze, characterize
The color and luster of the terephthalic acid (TPA) to preparing, pattern, Chemical Physics performance, purity are detected, analyzed, characterized；
The micromorphology analysis of terephthalic acid (TPA) are carried out with SEM；
The image structural analysis of terephthalic acid (TPA) is carried out with X-ray diffractometer；
Conclusion：Terephthalic acid (TPA) is white powder, powder granule diameter≤2 μm, and product purity is up to 99.973%；
(6) product storage
Terephthalic acid (TPA), ethylene glycol to preparation are separately stored in the glass container of amber transparent, and closed shading is preserved,
Moistureproof, sun-proof, anti-acid-alkali salt corrodes, 20 DEG C of storage temperature, relative humidity≤10%.
Beneficial effect
The present invention has obvious advanced with background technology compared with, is directed to that waste and old polyester fiber storage is more, pollutes sternly
Weight, difficult situation is reclaimed, waste and old polyester fiber is washed, is sterilized, high pressure degraded separation is stripped, dries, ground, it is right to be made
Terephthalic acid product, while also having isolated accessory substance ethylene glycol, this preparation method technique is advanced, data are accurately full and accurate, prepares
The product quality isolated is good, purity is high, and up to 99.973%, product is powder to purity, and powder granule diameter≤2 μm can be made
Chemical raw material is re-used, and is the highly advanced method that terephthalic acid (TPA) and accessory substance are prepared with waste and old polyester fiber.
Brief description of the drawings
Fig. 1, the degraded state diagram of waste and old polyester fiber
Fig. 2, the terephthalic acid (TPA) shape appearance figure for preparing
Fig. 3, the terephthalic acid (TPA) diffracted intensity collection of illustrative plates for preparing
Shown in figure, list of numerals is as follows：
1st, agitator, 2, bolt, 3, kettle cover, 4, heat-insulation layer, 5, autoclave, 6, resistance heater, 7, reaction solution, 8,
Kettle seat, 9, wire, 10, stirring motor, 11, feed belt, 12, pressure gauge, 13, thermocouple, 14, electric cabinet, 15, agitation revolution
Display screen, 16, temperature in the kettle display screen, 17, stirring switch, 18, power switch, 19, heating-up temperature modulator, 20, stirring turns
Number modulator.
Specific embodiment
Once with reference to accompanying drawing, the invention will be further described：
It is waste and old polyester fiber degraded state diagram shown in Fig. 1, each portion position is correct, matches according to quantity, sequentially operates.
What the value of the chemical substance that preparation is used first was determined by the scope for pre-setting, be metering with gram, milliliter, millimeter
Unit.
Autoclave 5 is rectangle, is resistance heater 6 in the outside of autoclave 5, outside resistance heater 6
It is heat-insulation layer 4, the bottom of autoclave 5 is that kettle seat 8, top is kettle cover 3, and is fixed by bolt 2, is in autoclave 5
Reaction solution 7；Agitator 1 is provided with the centre position of kettle cover 3, and is goed deep into autoclave 5；Heat is provided with the sidepiece of kettle cover 3
Galvanic couple 13, pressure gauge 12, and go deep into autoclave 5；Stirring motor 10, stirring electricity are provided with the right part of autoclave 5
Machine 10 connects agitator 1 by conveyer belt 11；Electric cabinet 14 is provided with the right side of autoclave 5, is set on electric cabinet 14
There are agitation revolution display screen 15, temperature in the kettle display screen 16, stirring to switch 17, power switch 18, heating-up temperature modulator 19, stir
Mix revolution modulator 20；Connected by wire 9 between autoclave 5 and electric cabinet 14.
It is the terephthalic acid (TPA) shape appearance figure for preparing shown in Fig. 2, shown in figure, product terephthalic acid is powder, in not advising
Then pile up.
It is the terephthalic acid (TPA) diffracted intensity collection of illustrative plates for preparing shown in Fig. 3, shown in figure, product diffraction maximum is terephthaldehyde
Sour characteristic peak.
Claims (2)
1. a kind of method that terephthalic acid (TPA) is prepared with waste and old polyester fiber, it is characterised in that：
The chemical substance material for using is：Waste and old polyester fiber, manganese acetate, high-carbon fatty alcohol polyoxyethylene ether, activated carbon, N, N-
Dimethylformamide, absolute ethyl alcohol, deionized water, it is as follows that it prepares consumption：It is measurement unit with gram, milliliter
Waste and old polyester fiber：(C39H44O22)nN=6000-15000,10g ± 0.01g
Activated carbon：C, 10g ± 0.01g
Manganese acetate：C4H6MnO4, 0.1g ± 0.01g
N,N-dimethylformamide：C3H7NO, 50mL ± 0.01mL
Absolute ethyl alcohol：C2H6O, 100mL ± 5mL
High-carbon fatty alcohol polyoxyethylene ether：C14O(CH2CH2O)9H, 2mL ± 0.01mL
Deionized water：H2O, 3000mL ± 50mL
Preparation method is as follows：
(1) waste and old polyester fiber is pre-processed
1. wash, waste and old polyester fiber 10g ± 0.01g are placed in washer, add deionized water 200mL, high-carbon fatty alcohol
APEO 2mL ± 0.01mL；
Turn on agitator, agitator treating 12min；
2. rinse, by washing after waste and old polyester fiber be placed in beaker, add deionized water 200mL, stirring rinsing 3min；
Stirring rinsing repeats 4 times；
3. dry, by rinsing after waste and old polyester fiber be placed in drying box dry, 100 DEG C of drying temperature, drying time
60min；
4. sterilize, dried waste and old polyester fiber is placed in ultraviolet disinfection case, carry out closed sterilization, voltage 220V, work(
Rate 40W, disinfecting time 30min；
5. shear, by sterilization after waste and old polyester fiber cut into bulk, block planar dimension≤(10mm × 10mm)；
(2) degrading waste polyester fiber
The degraded of waste and old polyester fiber is carried out in autoclave, is completed in heating, whipping process；
1. autoclave is cleaned, autoclave is opened, deionized water 200mL is added, autoclave inwall is cleaned, makes it
It is clean；
Cleaning repeats 3 times, is dried after cleaning；
2. prepare reaction solution, weigh waste and old polyester fiber 10g ± 0.01g, activated carbon 10g ± 0.01g, manganese acetate 0.1g ±
0.01g, measures deionized water 100mL ± 1mL, adds in beaker, 10min is stirred, into mixed liquor；
3. mixed liquor is added in autoclave, and it is closed；
4. autoclave is opened, and is heated, 240 DEG C ± 1 DEG C of heating-up temperature, pressure is 3.3MPa, high pressure in autoclave
Reactor agitation revolution 100r/min, reaction time 7h；
Mixed solution will occur physical-chemical reaction in heating, course of reaction, and cotton fiber carbonization, terylene hydrolysis, color are divested；
Stop heating after reaction, mixed liquor is cooled to 25 DEG C, obtains suspension with kettle；
(3) product is separated
1. separation of solid and liquid, suspension is placed in the Buchner funnel of bottle,suction, and suction filtration is carried out with miillpore filter, and filter is retained on filter membrane
Cake, filtrate is evacuated in filter flask, and is collected respectively；
2. ethylene glycol is extracted, filtrate is placed in distilling flask, distilling flask is placed on electric heating agitator, heating-up temperature 197
DEG C ± 1 DEG C, heating stirring obtains liquid fraction, i.e. ethylene glycol, and collect；
3. separating liquid is prepared, filter cake is placed in beaker, be subsequently adding DMF 50mL ± 0.01mL, stirred
5min；
Then beaker is placed in heating stirring on electric heating agitator, 70 DEG C ± 1 DEG C of heating-up temperature is heated and stirred, makes to benzene two
Formic acid is substantially dissolved in solution, into separating liquid；
4. suction filtration, separating liquid is placed in the Buchner funnel of bottle,suction, and suction filtration is carried out with miillpore filter, on filter membrane retain filter cake,
In filtrate suction filtration to filter flask, and collect respectively；
5. activated carbon is washed and is reclaimed, filter cake is placed in beaker, add absolute ethyl alcohol 100mL ± 5mL, stir 10min；
Then suction filtration is carried out with miillpore filter, obtains filter cake；
Then filter cake is washed with deionized water, suction filtration, obtain filter cake；
Filter cake is placed in drying box and is dried, 120 DEG C of drying temperature, drying time 2h reclaims activated carbon after drying；
6. separation and Extraction terephthalic acid (TPA), during filtrate added into beaker, is subsequently adding deionized water 50mL, stirs 5min, into outstanding
Turbid liquid；
Suspension is added in centrifuge tube, is centrifuged on centrifuge, separate revolution 8000r/min, disengaging time
8min, retains sediment, abandoning supernatant after separation；
Put the precipitate in beaker, deionized water 200mL, agitator treating 5min are added, then with three layers of middling speed qualitative filter paper
Filtering, retains filter cake, discards cleaning solution；
Filter cake is placed in vacuum drying chamber and is dried, 110 DEG C of drying temperature, vacuum 10Pa, drying time 6h must consolidate after drying
Body material, i.e. terephthalic acid (TPA)；
(4) grind, sieve
Dried solid matter terephthalic acid (TPA) agate mortar, pestle are ground, are then sieved with 600 eye mesh screens；
Grinding, sieving are repeated, and obtain end-product terephthalic acid (TPA) white powder；
(5) detect, analyze, characterize
The color and luster of the terephthalic acid (TPA) to preparing, pattern, purity are detected, analyzed, characterized；
The micromorphology analysis of terephthalic acid (TPA) are carried out with SEM；
The image structural analysis of terephthalic acid (TPA) is carried out with X-ray diffractometer；
Conclusion：Terephthalic acid (TPA) is white powder, powder granule diameter≤2 μm, and product purity is up to 99.973%；
(6) product storage
Terephthalic acid (TPA), ethylene glycol to preparation are separately stored in the glass container of amber transparent, and closed shading is preserved, and to be prevented
Damp, sun-proof, anti-acid-alkali salt corrodes, 20 DEG C of storage temperature, relative humidity≤10%.
2. a kind of method that terephthalic acid (TPA) is prepared with waste and old polyester fiber according to claim 1, it is characterised in that：
Autoclave (5) is rectangle, is resistance heater (6) in the outside of autoclave (5), in resistance heater (6)
Outside is heat-insulation layer (4), and the bottom of autoclave (5) is kettle seat (8), top is kettle cover (3), and fixed by bolt (2), high
It is reaction solution (7) in pressure reactor (5)；Agitator (1) is provided with the centre position of kettle cover (3), and gos deep into autoclave (5)
It is interior；Thermocouple (13), pressure gauge (12) are provided with the sidepiece of kettle cover (3), and are goed deep into autoclave (5)；In reaction under high pressure
The right part of kettle (5) is provided with stirring motor (10), and stirring motor (10) connects agitator (1) by conveyer belt (11)；It is anti-in high pressure
Answer the right side of kettle (5) to be provided with electric cabinet (14), agitation revolution display screen (15), temperature in the kettle are provided with electric cabinet (14) and are shown
Display screen (16), stirring switch (17), power switch (18), heating-up temperature modulator (19), agitation revolution modulator (20)；High pressure
It is connected by wire (9) between reactor (5) and electric cabinet (14).
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| CN110237888B (en) * | 2019-05-13 | 2021-10-01 | 嘉兴卓十生物科技有限公司 | Ethanol extraction method |
| CN112251870A (en) * | 2020-09-07 | 2021-01-22 | 苏州贤辉新纺织科技有限公司 | Process method for regenerating flame-retardant polyester fiber by adopting recycled polyester fiber |
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