CN109467739A - Recovery method of waste polyester blended fabric containing natural base fiber - Google Patents
Recovery method of waste polyester blended fabric containing natural base fiber Download PDFInfo
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- CN109467739A CN109467739A CN201710806957.9A CN201710806957A CN109467739A CN 109467739 A CN109467739 A CN 109467739A CN 201710806957 A CN201710806957 A CN 201710806957A CN 109467739 A CN109467739 A CN 109467739A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J11/00—Recovery or working-up of waste materials
- C08J11/04—Recovery or working-up of waste materials of polymers
- C08J11/06—Recovery or working-up of waste materials of polymers without chemical reactions
- C08J11/08—Recovery or working-up of waste materials of polymers without chemical reactions using selective solvents for polymer components
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2367/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2401/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2401/02—Cellulose; Modified cellulose
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2489/00—Characterised by the use of proteins; Derivatives thereof
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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
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/62—Plastics recycling; Rubber recycling
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- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)
- Artificial Filaments (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention provides a method for recovering waste polyester blended fabrics containing natural base fibers, which comprises the steps of placing the waste polyester blended fabrics in a water-soluble tertiary amine oxide solution containing an antioxidant so as to dissolve the natural base fibers to form a fiber solution and solid insoluble substances, then recovering the fiber solution to obtain regenerated natural base cellulose fibers, and sequentially adding an ester solvent and fatty alcohol into the solid insoluble substances to recover polyester solids. The recovery method can separate the terylene from other natural base fibers, is suitable for all terylene blended fabrics, fills the blank of the prior art, has high recovery rate of the terylene and the regenerated natural base cellulose fibers, avoids using chemical reagents with high toxicity and irritation, and can recycle the used reagents. The recovery method provided by the invention has the advantages of high efficiency, low cost, environmental friendliness, wide application range and the like, and has the potential of industrial application.
Description
Technical field
The invention belongs to resource regeneration fields of weaving, and in particular to a kind of waste and old terylene containing natural based cellulose is blended to be knitted
The recovery method of object.
Background technique
Terylene is an important species in synthetic fibers, is to pass through polyethylene terephthalate high polymer (PET)
Fiber made of spinning and post-processing.Polyester blended fabric is that polyester fiber is mixed spinning with fibers such as other cottons, hair, silk, fiber crops
The textile product that yarn is made into, main polyester blended fabric include polyester cotton, wool-polyester blended fabric, wash fiber crops and blended knit
(fabric of terylene and two kinds of fiber blends such as washs Maoma, washs numb cotton, washs for object, polyester-viscose blended fabric, " three-in-one " blended fabric
Adhesive hair, polyester-cotton blend are viscous etc.).After the polyester blended fabric of such multiple types becomes waste textile, need to find a kind of ring
Guarantor, energy conservation, efficient method are by terylene therein and other blended natural based cellulose recycling and reusings as far as possible, with reality
Now certain economic well-being of workers and staff reaches the sustainable development of resource.
Existing research focuses mostly in the recycling and reusing of polyester cotton, is seldom related to other fibers and blend polyester
The recycling and reusing of fabric, especially natural based cellulose and polyester blended fabric.Typically, the recycling of polyester blended fabric is again
It is to separate terylene and other compositions such as cotton fiber etc. using method, then pointedly recycles respectively.But it is existing
The solvent that method uses is mostly the higher type of toxicity, at high cost and endanger environment, in addition, existing method is difficult to realize mostly
Regenerant is completely separated, and influences to recycle purity.
Summary of the invention
To overcome blank and defect present in existing waste and old terylene blended fabric recovery technology, the purpose of the present invention is mention
For a kind of recovery method of efficiently waste and old terylene blended fabric containing natural based cellulose.
The recovery method of waste and old terylene blended fabric provided by the invention containing natural based cellulose the following steps are included:
S1: the waste and old terylene blended fabric containing natural based cellulose is placed in the oxidation of the water-soluble tertiary amine containing antioxidant
In object solution, so that natural based cellulose dissolves to form fiber solution and solid insoluble；
S2: the resulting fiber solution of step S1 is passed through into wet spinning reclaiming natural based cellulose cellulose fiber；And
S3: the resulting solid insoluble of step S1 is immersed in esters solvent and is reacted at a temperature of 150~210 DEG C to molten
Solution, the fatty alcohol that C1~C3 is then added are recycled so that terylene solid is precipitated；
Wherein, water-soluble tertiary amine oxide used in the step S1 is selected from cacodyl oxide ethylethanolamine, oxidation front three
One of amine, N-methylmorpholine-N- oxide, N- methylpiperidine-N-oxide, N- methylpyrrolidin- N- oxide are more
The combination of kind；
Esters solvent used in the step S3 has formula (1) structure:
In formula (1), R indicates the linear or branched alkyl group of C1~C5, and n indicates 1~3 integer.
In recovery method of the invention, the waste and old terylene blended fabric is 10%~90% containing the amount of washing by weight,
Water content is lower than 10% by weight.
In recovery method of the invention, the natural based cellulose in the waste and old terylene blended fabric includes protein fiber
And/or cellulose-based fiber, wherein the protein fiber includes silk and/or wool, and the cellulose-based fiber includes
One of cotton fiber, flaxen fiber, viscose rayon, Modal fibre, Lyocell fiber, copper ammonia fiber, acetate fiber are a variety of
Combination.
In recovery method of the invention, the protein fiber content in the waste and old terylene blended fabric is by weight low
In 30%.
In recovery method of the invention, the moisture content of the water-soluble tertiary amine oxide solution in the step S1 is by weight
It is 10%~15%.
In recovery method of the invention, the antioxidant is selected from catechol, Pyrogallol acid, gallic acid third
Ester, 2,6-di-tert-butyl p-cresol, gallic acid, the first, second of gallic acid, third or one of isopropyl ester or a variety of groups
It closes, the weight ratio of the antioxidant is 0.5%~3%.
The waste and old terylene blended fabric and water containing natural based cellulose in recovery method of the invention, in the step S1
The weight ratio of dissolubility tertiary amino oxides solution is 1 ﹕, 99~15 ﹕ 85.
In recovery method of the invention, the process that natural based cellulose dissolves in the step S1 includes prior at 60~75 DEG C
It is swollen 20~30min, is warming up to 80~130 DEG C of 50~90min of dissolution later.
In recovery method of the invention, the wet spinning process in the step S2 includes that the resulting fiber of step S1 is molten
Liquid spinneret is into water and/or ethyl alcohol, and 3~10 times of mechanical stretching, regeneration natural based cellulose cellulose fiber is made.
In recovery method of the invention, esters solvent used in the step S3 is selected from methyl benzoate, benzoic acid second
Ester, propyl benzoate, isopropyl benzoate, butyl benzoate, isobutyl benzoate, dimethyl terephthalate (DMT), isophthalic diformazan
One of dimethyl phthalate or a variety of combinations；Terylene weight and the esters solvent in the waste and old terylene blended fabric
Weight ratio is 1 ﹕, 1.1~1 ﹕ 50.
In recovery method of the invention, the reaction time in the step S3 is 3~30min.
In recovery method of the invention, in the step S3, the volume ratio of dissolved terylene solution and the fatty alcohol
For 1 ﹕, 15~1 ﹕ 50, after the fatty alcohol is added, 45~65 DEG C are cooled to so that terylene solid is precipitated.
In recovery method of the invention, the fatty alcohol is selected from methanol or ethyl alcohol.
In recovery method of the invention, the step S3 further includes being viscosified resulting terylene solid to reaching spinning
The requirement of slice.
In recovery method of the invention, the step S3 further includes that will return respectively again after terylene solid separation and recovery
Receive the fatty alcohol and the esters solvent.
The recovery method of waste and old terylene blended fabric containing natural based cellulose of the invention has the advantage that
(1) recovery method of the invention can completely, thoroughly separate terylene and other natural based celluloses, the terylene of recycling
With regeneration natural based cellulose cellulose fiber purity is high, the rate of recovery is high, and original physics, chemistry can be retained substantially by recycling resulting terylene
Performance, economic advantages are obvious.
(2) recovery method technical process of the invention is advanced, only can obtain high quality by once dissolution-regenerative process
Regenerated protein/cellulose fibre.
(3) recovery method of the invention is applicable to the polyester blended fabric containing terylene of all kinds, the scope of application
Extensively, blank of the existing technology has been filled up.
(4) recovery method of the invention avoids chemical reagent big using toxicity, that irritation is big, and used examination
Agent is also recyclable, further reduces process costs, and alleviates the harm to environment.
In short, recovery method provided by the invention has many advantages, such as that high efficiency, low cost, environmental-friendly, applicability is wide, tool
There are the potentiality of industrial applications.
Detailed description of the invention
Fig. 1 is the process flow of the waste and old terylene blended fabric recovery method of the present invention containing natural based cellulose
Figure.
Specific embodiment
The recovery method for the waste and old terylene blended fabric containing natural based cellulose that the present invention provides a kind of, including following step
It is rapid:
S1: the waste and old terylene blended fabric containing natural based cellulose is placed in the oxidation of the water-soluble tertiary amine containing antioxidant
In object solution, so that natural based cellulose dissolves to form fiber solution and solid insoluble；
S2: the resulting fiber solution of step S1 is passed through into wet spinning reclaiming natural based cellulose cellulose fiber；And
S3: the resulting solid insoluble of step S1 is immersed in esters solvent and is reacted at a temperature of 150~210 DEG C to molten
Solution, the fatty alcohol that C1~C3 is then added are recycled so that terylene solid is precipitated；
Wherein, water-soluble tertiary amine oxide used in step S1 is selected from cacodyl oxide ethylethanolamine, trimethylamine oxide, N-
One of methyhnorpholine-N-oxide, N- methylpiperidine-N-oxide, N- methylpyrrolidin- N- oxide or a variety of groups
It closes；
Esters solvent used in step S3 has formula (1) structure:
In formula (1), R indicates the linear or branched alkyl group of C1~C5, and n indicates 1~3 integer.
Referring to Fig.1, the recovery method of the waste and old terylene blended fabric of the invention containing natural based cellulose is first using containing
There is the water-soluble tertiary amine oxide solution of antioxidant to dissolve natural based cellulose to form fiber solution and terylene solid is insoluble
Object achievees the purpose that be completely separated polyester fiber (insoluble matter) and natural based cellulose (being dissolved in solution), then by being separated by solid-liquid separation
Specific aim recovery processing is carried out to resulting terylene solid insoluble and natural based cellulose solution again.The water solubility that the present invention uses
Tertiary amino oxides toxicity is extremely low, and the ingredients such as energy solubilising protein, cellulose can be made again without being converted into derivative
TModified Cellulose Fibers are obtained, water-soluble tertiary amine oxide is reused after also can be recycled.
Further, natural based cellulose solution can handle to obtain regeneration natural based cellulose cellulose fiber progress by wet spinning
Recycling.Terylene solid insoluble is dissolved using esters solvent first, and resulting terylene solution reuses C1 after removing impurity
The lower aliphatic alcohols of~C3 are handled, so that terylene solid is precipitated and recycles.The esters solvent that recovery method of the invention uses is
The solvent of benzoic acid derived ester, small toxicity is at low cost, is also convenient to recycling and reusing.
What recovery method of the present invention obtained is regenerated protein/cellulose fibre of high quality, is contained on protein side chain
Ion-COO-With-NH3 +, hydrophilic ability is better than the polarity-OH on cellulose, can improve the water-swellable of pure cellulose regenerated fiber
The defects of property and fibrillation characteristic, and bring excellent feel.
In practical applications, step S2, S3 can be handled by different sequencings according to the actual situation, and sequence is not
Limit, can also be handled simultaneously.
In recovery method of the invention, the waste and old terylene blended fabric containing natural based cellulose can be existing any
The polyester blended fabric of type, including but not limited to polyester cotton, wool-polyester blended fabric wash numb blended fabric, wash viscous mix
Textile fabric, " three-in-one " blended fabric etc., recovery method of the invention can obtain high-purity, the recycling effect of high-recovery
Fruit.In one embodiment according to the present invention, waste and old terylene blended fabric containing the amount of washing by weight can for 10%~
90%, in one preferred embodiment, waste and old terylene blended fabric can be 30%~70% containing the amount of washing by weight.
In one embodiment according to the present invention, the water content of waste and old terylene blended fabric is lower than 10% by weight.
In recovery method of the invention, the natural based cellulose in the waste and old terylene blended fabric containing natural based cellulose can
Think existing any kind, for example, may include protein fiber, cellulose-based fiber or simultaneously comprising both.According to this
In one embodiment of invention, protein fiber includes but is not limited to silk, wool etc., or is a combination thereof.According to this
In the another embodiment of invention, cellulose-based fiber includes but is not limited to cotton fiber, flaxen fiber, viscose rayon, Modal
Fiber, Lyocell fiber, copper ammonia fiber, acetate fiber etc., or be any combination.In one preferred embodiment, when useless
When in old polyester blended fabric including protein fiber such as silk, wool, protein fiber content is lower than by weight
30%.
In recovery method of the invention, tertiary amino oxides packet that the water-soluble tertiary amine oxide solution in step S1 uses
Include but be not limited to cacodyl oxide ethylethanolamine, trimethylamine oxide, N-methylmorpholine-N- oxide, N- methyl piperidine-N- oxidation
Object, N- methylpyrrolidin- N- oxide etc., or be any combination.In one preferred embodiment, water-soluble tertiary amine aoxidizes
Object can be N-methylmorpholine-N- oxide.In one embodiment according to the present invention, water-soluble tertiary amine oxide solution
Moisture content by weight can be 10%~15%, in one preferred embodiment, water-soluble tertiary amine oxide solution
Moisture content by weight can be 12%~14%.
In recovery method of the invention, antioxidant can select common antioxidant type for example tannins, phenols,
Aromatics polyol etc., specifically, including but not limited to catechol, Pyrogallol acid, propylgallate, 2,6-
Di-tert-butyl p-cresol, gallic acid, the first, second of gallic acid, third or isopropyl ester etc. can also be the combination of any kind,
In one preferred embodiment, antioxidant can be propylgallate or Propylgallate.According to the present invention
In one embodiment, the weight of antioxidant can be the 0.5%~3% of water-soluble tertiary amine oxide solution weight, one
In a preferred embodiment, the weight of antioxidant can be the 1%~2% of water-soluble tertiary amine oxide solution weight.
In recovery method of the invention, the waste and old terylene blended fabric containing natural based cellulose and water-soluble tertiary amine are aoxidized
The weight ratio of object solution can be 1 ﹕, 99~15 ﹕ 85, in one preferred embodiment, waste and old terylene blended fabric with it is water-soluble
The weight ratio of property tertiary amino oxides solution can be 10 ﹕, 90~13 ﹕ 87.
In recovery method of the invention, the course of dissolution of natural based cellulose can be performed under heating conditions, such as with
Lower process: being swollen 20~30min at prior to 60~75 DEG C, is warming up to 80~130 DEG C of dissolution 50~90min later, excellent at one
In the embodiment of choosing, Fibrinolysis can also be following procedure: being swollen 20~30min at prior to 60~75 DEG C, heat up later
To 90~100 DEG C of 60~80min of dissolution.
In recovery method of the invention, the wet spinning process in step S2 can be existing wet spinning technology.
In one preferred embodiment, it can be following procedure: the resulting fiber solution of step S1 is continuously squeezed by spinning head
Enter in water and/or ethyl alcohol, 3~10 times of mechanical stretching, make molecularly oriented, the regeneration natural based cellulose element for being thus made recyclable is fine
Dimension.
In recovery method of the invention, as shown in Figure 1, after step S2 reclaiming natural based cellulose cellulose fiber, also
It can be recycled the remaining water-soluble tertiary amine oxide solution containing antioxidant, after the purification process by such as ion exchange column etc.,
It can be with cycling and reutilization.
In recovery method of the invention, the esters solvent that step S3 is used has above-mentioned formula (1) structure, wherein R can table
Show methyl, ethyl, propyl, isopropyl, normal-butyl, isobutyl group, sec-butyl, tert-butyl, n-pentyl, isopentyl, neopentyl, uncle penta
Base etc. preferably can be methyl, ethyl, propyl, isopropyl, normal-butyl.N can indicate 1,2 or 3 integer, preferably 1 or 2
Integer has one or two carboxylate groups that is, on phenyl ring, when n indicates not to be 1 integer, two or more substitutions
Group can be located at any possible the position of substitution on phenyl ring.In one embodiment according to the present invention, esters solvent packet
Include but be not limited to methyl benzoate, ethyl benzoate, propyl benzoate, isopropyl benzoate, butyl benzoate, anhydride
Ester, dimethyl terephthalate (DMT), dimethyl isophthalate etc. can also be the combination of any kind.
In recovery method of the invention, calculated according to the weight of terylene in waste and old terylene blended fabric, it is molten with esters
The dosage of agent can be the weight ratio of 1 ﹕, 1.1~1 ﹕ 50, can also be adjusted according to the actual situation by those skilled in the art.?
In a preferred embodiment according to the present invention, the weight ratio of terylene and esters solvent can be 1 ﹕, 15~1 ﹕ 20.
In recovery method of the invention, the terylene dissolution reaction in step S3 should generally make the dissolution of terylene solid completely,
It can be by those skilled in the art adjusting reaction time and temperature according to the actual situation.According to embodiment of the present invention
In, the reaction time can be 3~60 minutes, and in one preferred embodiment, the reaction time can be 5~15 minutes.?
According to embodiment of the present invention, reaction temperature can be 150~210 DEG C, in one preferred embodiment, instead
Answering temperature can be 170~190 DEG C.Terylene dissolves after the reaction was completed, can be filtered removing impurity, obtain terylene solution.
In recovery method of the invention, C1~C3 fatty alcohol in step S3 can be methanol, ethyl alcohol, propyl alcohol, isopropyl
The common lower aliphatic alcohols such as alcohol.In one embodiment according to the present invention, fatty alcohol can be methanol or ethyl alcohol.In root
According in an embodiment of the invention, the volume ratios of the lower aliphatic alcohols such as dissolved terylene solution and methanol, ethyl alcohol can be with
For 1 ﹕, 15~1 ﹕ 50, in one preferred embodiment, the volume ratios of terylene solution and lower aliphatic alcohols can for 1 ﹕ 20~
1 ﹕ 25.In one embodiment according to the present invention, fatty alcohol can be added in dissolved terylene solution, can also will be molten
Terylene solution after solution pours into fatty alcohol.In one embodiment according to the present invention, the rudimentary rouge such as methanol, ethyl alcohol are added
After fat alcohol, terylene solution can be cooled to 45~65 DEG C so that terylene solid is precipitated.
In recovery method of the invention, to reach higher recycling requirement, the terylene solid of precipitation can also be passed through
Granulation, pre-crystallized, dry, solid-phase tack producing etc. are handled to improve the number-average molecular weight of terylene, can such as be viscosified to number-average molecular weight and be reached
20000 or more, to reach the requirement of spinning chips.
In recovery method of the invention, as shown in Figure 1, collecting the lower aliphatic alcohols after processing terylene solid, may be used also
It is recycled or is purified to recycle respectively for esters solvent and fatty alcohol itself contained therein.Since the present invention makes
Esters solvent boiling point is much higher than lower aliphatic alcohols, therefore can pass through this fields normal methods such as cooling crystallization, distillation, rectifying
Recycle esters solvent and fatty alcohol.In one embodiment according to the present invention, after isolating terylene solid, then will be remaining
Fatty alcohol solution continues to be cooled to 20~40 DEG C so that esters solvent crystal is precipitated, and in one preferred embodiment, is cooled to
20~25 DEG C to be precipitated esters solvent crystal, after recycling esters solvent crystal, remaining fatty alcohol is purified by modes such as distillations
After can be recycled.In an alternative embodiment of the process according to the invention, can also be used distillation or rectifying mode to recycle esters molten
Agent and fatty alcohol.
In recovery method of the invention, it is common that this field can be selected in the operation of the separating steps such as separation of solid and liquid, filtering
Operation, including but not limited to suction method, (high speed) centrifugal process, the precipitation method or their combination.
To make the object, technical solutions and advantages of the present invention clearer, it will be further described below example of the invention
The technical solution of property embodiment.
Chemical reagent used in following embodiment is then unless otherwise instructed commercial goods, used in following embodiment
Operation or instrument are then this field common operation or instrument unless otherwise instructed.Ratio described in following embodiment, ratio,
Content etc. is then weight ratio unless otherwise instructed.
Embodiment 1
By water content 5%, containing the amount of washing 50%, the waste and old of wool content 10% velvet apple blended fabric 10g is washed, is placed in 65 DEG C and contains
It is swollen 30min in 0.5g propylgallate and the 4- methyhnorpholine-N-oxide solution 45ml of 12% deionized water, is then risen
Temperature makes natural based cellulose therein sufficiently dissolve 60min to 100 DEG C.Mixture is separated by solid-liquid separation using vacuum filtration method,
Obtained protein/cellulose spin dope is continuously squeezed into water from spinning head, 3 times of mechanical stretching, obtained regenerated protein/
Cellulose fibre, is recycled and to purify the 4- methyhnorpholine-N-oxide containing propylgallate with ion exchange column molten
Liquid.And the solid insoluble isolated then is immersed in 170 DEG C, in the dimethyl terephthalate (DMT) of 50ml after 15min, then slowly
It pours into methanol, when temperature is down to 50 DEG C, the terylene particle being precipitated is collected using supercentrifugal process, is further continued for being cooled to 25 DEG C
When, the dimethyl terephthalate (DMT) particle of precipitation is collected, and remaining methanol solution is recycled by the way of distillation again.
Embodiment 2
By water content 8%, containing the amount of washing 30%, the waste and old of wool content 15% adhesive hair blended fabric 10g is washed, is placed in 75 DEG C and contains
It is swollen 20min in 1g Propylgallate and the 4- methyhnorpholine-N-oxide solution 50ml of 14% deionized water, is then heated up
To 90 DEG C, natural based cellulose therein is made sufficiently to dissolve 80min.Mixture is separated by solid-liquid separation using vacuum filtration method, it will
Obtained protein/cellulose spin dope is continuously squeezed into water from spinning head, and 8 times of mechanical stretching, regenerated protein/fibre is made
Cellulose fiber, recycling and the 4- methyhnorpholine-N-oxide solution containing Propylgallate of being purified with ion exchange column.
And the solid insoluble isolated then is immersed in 190 DEG C, in the butyl benzoate of 60ml after 5min, is then poured slowly into ethyl alcohol
In, when temperature is down to 60 DEG C, the terylene particle being precipitated is collected using supercentrifugal process, then carry out at distillation to ethanol solution
Reason, obtains product of distillation ethyl alcohol, residue is butyl benzoate.
Although the preferred embodiments of the invention, those skilled in the art has been disclosed in order to illustrate the present invention
Member can be the present invention it should be appreciated that in the case where not departing from present inventive concept defined by claims and range
Various modifications, addition and replacement out.
Claims (15)
1. a kind of recovery method of the waste and old terylene blended fabric containing natural based cellulose, which comprises the following steps:
S1: it is molten that the waste and old terylene blended fabric containing natural based cellulose is placed in the water-soluble tertiary amine oxide containing antioxidant
In liquid, so that natural based cellulose dissolves to form fiber solution and solid insoluble；
S2: the resulting fiber solution of step S1 is passed through into wet spinning reclaiming natural based cellulose cellulose fiber；And
S3: immersing the reaction extremely dissolution at a temperature of 150~210 DEG C in esters solvent for the resulting solid insoluble of step S1,
Then the fatty alcohol for C1~C3 being added is recycled so that terylene solid is precipitated；
Wherein, water-soluble tertiary amine oxide used in the step S1 is selected from cacodyl oxide ethylethanolamine, trimethylamine oxide, N-
One of methyhnorpholine-N-oxide, N- methylpiperidine-N-oxide, N- methylpyrrolidin- N- oxide or a variety of groups
It closes；
Esters solvent used in the step S3 has formula (1) structure:
In formula (1), R indicates the linear or branched alkyl group of C1~C5, and n indicates 1~3 integer.
2. recovery method according to claim 1, which is characterized in that the waste and old terylene blended fabric contains the amount of washing by weight
For amount than being 10%~90%, water content is lower than 10% by weight.
3. recovery method according to claim 2, which is characterized in that the natural base in the waste and old terylene blended fabric is fine
Dimension includes protein fiber and/or cellulose-based fiber, wherein the protein fiber includes silk and/or wool, institute
Stating cellulose-based fiber includes cotton fiber, flaxen fiber, viscose rayon, Modal fibre, Lyocell fiber, copper ammonia fiber, acetic acid
One of fiber or a variety of combinations.
4. recovery method according to claim 3, which is characterized in that the protein base in the waste and old terylene blended fabric
Fiber content is lower than 30% by weight.
5. recovery method according to claim 1, which is characterized in that the water-soluble tertiary amine oxide in the step S1 is molten
The moisture content of liquid is 10%~15% by weight.
6. recovery method according to claim 1, which is characterized in that the antioxidant is selected from catechol, 1,2,3-
In benzenetriol, propylgallate, 2,6-di-tert-butyl p-cresol, gallic acid, the first, second of gallic acid, third or isopropyl ester
One or more combinations, the weight ratio of the antioxidant is 0.5%~3%.
7. recovery method according to claim 1, which is characterized in that useless containing natural based cellulose in the step S1
The weight ratio of old polyester blended fabric and water-soluble tertiary amine oxide solution is 1 ﹕, 99~15 ﹕ 85.
8. recovery method according to claim 1, which is characterized in that the process that natural based cellulose dissolves in the step S1
Including being swollen 20~30min at prior to 60~75 DEG C, it is warming up to 80~130 DEG C of 50~90min of dissolution later.
9. recovery method according to claim 1, which is characterized in that the wet spinning process in the step S2 includes will
The resulting fiber solution spinneret of step S1 is into water and/or ethyl alcohol, and 3~10 times of mechanical stretching, regeneration natural based cellulose element is made
Fiber.
10. recovery method according to claim 1, which is characterized in that esters solvent used in the step S3 is selected from
Methyl benzoate, ethyl benzoate, propyl benzoate, isopropyl benzoate, butyl benzoate, isobutyl benzoate, to benzene two
One of formic acid dimethyl ester, dimethyl isophthalate or a variety of combinations；Terylene in the waste and old terylene blended fabric
Weight and the weight ratio of the esters solvent are 1 ﹕, 1.1~1 ﹕ 50.
11. recovery method according to claim 1, which is characterized in that reaction time in the step S3 is 3~
30min。
12. recovery method according to claim 1, which is characterized in that in the step S3, dissolved terylene solution with
The volume ratio of the fatty alcohol is 1 ﹕, 15~1 ﹕ 50, after the fatty alcohol is added, is cooled to 45~65 DEG C so that terylene solid is precipitated.
13. recovery method according to claim 12, which is characterized in that the fatty alcohol is selected from methanol or ethyl alcohol.
14. recovery method according to claim 1, which is characterized in that the step S3 further includes by resulting terylene solid
Body is viscosified to the requirement for reaching spinning chips.
15. recovery method according to claim 1, which is characterized in that the step S3 further includes by the terylene solid
The fatty alcohol and the esters solvent is separately recovered after separation and recovery again.
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