A kind of discarded polyester-cotton textiles degraded recovery process and system
Technical field
The invention belongs to polyester-cotton blend recovery technology field, and in particular to a kind of discarded polyester-cotton textiles degraded recovery process and be
System.
Background technology
Into 21 century since, with economic, industry and the fast development of population, available natural resources is passed day by day
Subtract.Meanwhile, environmental pollution caused by greenhouse gases, pollutant and the disposition of solid waste that combustion of fossil fuel is discharged is improper
Also it is on the rise.Therefore, whole world various countries are while renewable new energy is sought, to the process of solid waste from mistake
Landfill, burning or the simple recycling disposal for going turns to the recycling of full constituent or the recycling of high added value.
More than 40,000,000 tons, the blend fabric of wherein terylene, cotton and both accounts for fiber and disappears the fiber of Chinese annual production
More than half of consumption.According to the key task of " 12 " textile industry scientific and technological progress, from now on by Man-made Fibre and day
The recovery and reuse technology of right fiber waste textile.But due to technology and cost reason, the discarded cotton-terylene of the overwhelming majority
Blend fabric is still processed by landfill, burning electricity generation, or even simple burning.At present both at home and abroad for terylene, cotton and
The recovery of its blend fibre, be by terylene component therein is separated with cotton component after recycled.With reference to discarded
The component feature of bafta, for terylene, it is most useful that being recycled terylene hydrolysis or alcoholysis into monomer by chemical reagent
These monomers remanufacture new polyster fibre;And cotton thread therein is made up of 100% cellulose, can be used as enzyme hydrolysis
Raw material is produced and can be fermented monose, and then by by bio-baseds such as monose production of ethanol from microbial fermentation, butanol, bacteria celluloses
Fuel or bio-based materials.But in discarded bafta, the crystalline texture of cotton base fiber height changes into fermentable sugars to enzyme hydrolysis has
Very big inhibition.Therefore, for the recycling of cotton fiber, the method for adopting at present is will to re-work after its opening picking
Into regeneration cotton yarn, due to the chopped fiber produced in removal process it is more, so reclaim cotton fiber in can be used for spin amount compared with
It is few, cause regeneration cotton yarn quality not high, be simply possible to use in the relatively low textile of productive value.
In prior art, also have and the terylene in polyester cotton is dissolved, again by terylene chemical degradation after separation
The way that realization is utilized.But above-mentioned these methods, due to the detached reaction mechanism of heterogeneity it is different, and different separation
Method can not be carried out by successive reaction, in prior art often be a kind of composition of separated and dissolved, and using residue as
Another kind of composition, is not separated respectively to each composition, causes the purity of final product poor, is not easy to circulation profit
With.
The content of the invention
In order to solve the problems referred to above of prior art presence, the invention provides a kind of discarded polyester-cotton textiles degraded is reclaimed
Technique and system.The discarded polyester-cotton textiles degraded recovery process, is respectively adopted difference to the terylene and cotton fiber in polyester-cotton blend
Recovery method processed, obtain that purity is higher, be easy to continue cycling through cotton fiber and the polyethylene terephthalate for utilizing
Ester.The discarded polyester-cotton textiles degraded recovery process not only can alleviate the present situation of textile industry shortage of resources, and can be with
Textile pollution on the environment is reduced, with very big economic benefit and social benefit, is benefited the nation and the people.In addition, described useless
Abandon polyester-cotton textiles degraded recovery system efficiently to complete entirely to discard polyester-cotton textiles degraded recovery process.
The technical solution adopted in the present invention is:A kind of discarded polyester-cotton textiles degraded recovery process, comprises the following steps:
A, polyester-cotton textiles are crushed, as raw material;
B, in raw material add mass fraction for 75-80% SPA, 0.5-1.5h is reacted at 70-80 DEG C, react
After the completion of filter, obtain filtrate I and filtered fluid I;
C, take the stirring that adds water of filtered fluid I and be hydrolyzed, stop adding water when solids is separated out until there is no longer;Filter, obtain
Filtrate II, filtrate II are cotton fiber;
D, filtrate I is taken, mass fraction is added for the sodium hydroxide solution of 20-25%, sodium hydroxide solution and filtrate I
Mass ratio be 3-5:1,4-6h is reacted at 90-100 DEG C, is filtered after reaction, is taken filtrate and obtain filtered fluid II;
E, take the stirring that adds water of filtered fluid II and be diluted, stop adding water when solids is separated out until there is no longer, filter to take filter
Liquid, obtains filtered fluid III;
F, take filtrate III and carry out acid out and dry, obtain terephthalic acid (TPA);
G, take terephthalic acid (TPA) add ethylene glycol dissolving, carry out esterification, obtain polyethylene terephthalate.
The discarded polyester-cotton textiles degraded recovery process, first the phosphoric acid using high concentration is anti-with the cotton fiber in polyester-cotton blend
Should, generation is dissolved in the cellulose phosphate of water, so as to complete the initial gross separation of terylene and cotton fiber;Hydrolyze again and cotton fiber is analysed
Go out, obtain more pure cotton fiber;Then alkali lye is added in the reactant liquor Jing after acidolysis, carry out alkaline hydrolysis, NaOH energy
Enough and terylene generates the para-phthalic sodium for being dissolved in water, and para-phthalic sodium further hydrolyzes generation terephthalic acid (TPA), while
During alkaline hydrolysis and hydrolysis, the cotton fiber (such as β-cellulose and gamma cellulose) of part residual can be separated out, and filtration can rise
To the effect of removal of impurities;The terephthalic acid (TPA) for obtaining is carried out into direct esterification using ethylene glycol, polyethylene terephthalate is obtained
Ester, i.e. PET, are easy to following cycle to utilize.
The broken contact area in order to increase polyester-cotton textiles and process solvent, so as to be beneficial to smoothly entering for recovery process
OK;Parameter in the step, is able to preferably realize the smooth of the discarded polyester-cotton textiles degraded recovery process
Carry out.
In step A, polyester-cotton textiles are broken into into the cloth of 2-8cm, facilitate subsequent operation.
To accelerate the reaction rate of acidolysis, preferred technical scheme is, in step B, the mass ratio of SPA and raw material is
4-6:1, and be stirred in reaction.
To ensure good filter effect, preferred technical scheme is, in step C and step E, filter operation is:Make
Suction filtration is carried out as screen pack with polyester fiber or polypropylene fibre.
During hydrolysis, the addition of water can affect the amount of final hydrolysate, according to present inventor to mechanism and test
Learn, in step C, the volume ratio of the water and filtered fluid I of addition is 3:1;In step E, the volume of the water and filtered fluid II of addition
Than for 4:1.
In step F, add hydrochloric acid to carry out acid out, and drying operation is carried out at 160-200 DEG C, drying time is 2-4h.
At a temperature of 160-200 DEG C, terephthalic acid (TPA) is highly stable, will not degrade because of drying, so as to obtain purity it is higher to benzene
Dioctyl phthalate.
To improve the reactivity of terephthalic acid (TPA), present inventor improves the consumption of ethylene glycol, specifically, step
In rapid G, ethylene glycol is 2 with the mass ratio of terephthalic acid (TPA):1.
Present invention also offers a kind of discarded polyester-cotton textiles for realizing the discarded polyester-cotton textiles degraded recovery process
Degraded recovery system, including disintegrating machine, conveyer belt, acidolysis reaction kettle, cotton fiber reclaim reactor, Basic fluxing raction kettle, just carry anti-
Answer kettle and reaction kettle of the esterification;The discharging opening of the disintegrating machine is connected with the charging aperture of the acidolysis reaction kettle by conveyer belt,
Terylene filter cloth or nylon filtering cloth made by filter medium, the acidolysis are provided with the liquid outlet of the acidolysis reaction kettle removably
The liquid outlet of reactor and cotton fiber are reclaimed the inlet of reactor and are connected by pipeline, the Basic fluxing raction kettle, just carry anti-
Kettle and reaction kettle of the esterification is answered to be sequentially communicated, the cotton fiber reclaims reactor, Basic fluxing raction kettle, just puies forward reactor and esterification
Screen pack made by polyester fiber or polypropylene fibre is equipped with the liquid outlet of kettle;The acidolysis reaction kettle, Basic fluxing raction kettle
With heater, and the inside of acidolysis reaction kettle, Basic fluxing raction kettle and reaction kettle of the esterification are equipped with the side wall of reaction kettle of the esterification
It is equipped with agitator.
Since it is considered that in filtration step after acidolysis, filtrate and filtrate are the product for needing to stay, so
Removable filter medium is set in acidolysis reaction kettle, after the completion of filtration, filter medium is pulled down, you can easily remove and be deposited in
Filtrate on filter medium.
In view of the controllability and treating capacity of recovery process, the acidolysis reaction kettle, Basic fluxing raction kettle and reaction kettle of the esterification
Volume be 50-100L, the heater is located on acidolysis reaction kettle, Basic fluxing raction kettle or reaction kettle of the esterification side wall for disk
Electric heating coil, the pitch of the electric heating coil is 2-4cm.Electrically heated mode of heating, is easy to control heating power, 2-4cm
Pitch, also ensure that the uniformity of heating.
In view of the corrosivity of acidolysis, alkaline hydrolysis and esterification to reaction equipment, it is to ensure the discarded polyester-cotton textiles
Degraded recovery process is smoothed out, and preferred technical scheme is, the acidolysis reaction kettle, Basic fluxing raction kettle and reaction kettle of the esterification
Made using 304 stainless steels or 316L stainless steels.304 stainless steels or 316L stainless steels are resistant to below acid and 30%
Alkali, disclosure satisfy that the needs of recovery process.
Certainly, in the present invention, the pressure that the power of pipeline transportation and suction filtration need is both from the pump for being arranged on pipeline, right
Species, quantity and installation site in pump, those skilled in the art are needed by existing hydrodynamics, Principles of Chemical Engineering and technique,
Can be readily available, here is not just being repeated.
Beneficial effects of the present invention are:
1st, the recovery process the invention provides a kind of discarded polyester-cotton textiles are degraded, to the terylene and cotton fiber in polyester-cotton blend point
Do not processed using different recovery methods, obtained that purity is higher, be easy to continue cycling through the cotton fiber that utilizes and poly- to benzene two
Formic acid glycol ester.The discarded polyester-cotton textiles degraded recovery process not only can alleviate showing for textile industry shortage of resources
Shape, and textile pollution on the environment can be reduced, with very big economic benefit and social benefit, benefit the nation and the people.
2nd, the recovery system present invention also offers a kind of discarded polyester-cotton textiles are degraded, using the discarded polyester-cotton textiles
Degraded recovery system can be efficiently completed discarded polyester-cotton textiles degraded recovery process, and it is higher to obtain purity, is easy to continue to follow
Cotton fiber and polyethylene terephthalate that ring is utilized.
Description of the drawings
Fig. 1 is the structural representation of embodiment 4 in the present invention;
Fig. 2 is the partial sectional view of acidolysis reaction kettle in embodiment 4;
Fig. 3 is the partial sectional view of Basic fluxing raction kettle in embodiment 4.
In figure:1st, disintegrating machine;2nd, conveyer belt;3rd, acidolysis reaction kettle;31st, filter medium;4th, cotton fiber reclaims reactor;5、
Basic fluxing raction kettle;6th, just carry reactor;7th, reaction kettle of the esterification;8th, electric heating coil;9th, agitator.
Specific embodiment
With reference to embodiment, present disclosure is further illustrated.It should be appreciated that the enforcement of the present invention is not limited to
In the following examples, any pro forma flexible and/or change made to the present invention falls within the scope of the present invention.
In the present invention, if not refering in particular to, all of part, percentage are unit of weight, and all of equipment and raw material etc. are
It is commercially available or the industry is conventional.Method in following embodiments, if no special instructions, is the routine of this area
Method.
Embodiment 1
A kind of discarded polyester-cotton textiles degraded recovery process, comprises the following steps:
A, the cloth that discarded polyester-cotton textiles are broken into 2cm, as raw material;
B, add the SPA that mass fraction is 80% in raw material, the mass ratio of SPA and raw material is 4:1,80
DEG C, react 0.5h under stirring, filter after the completion of reaction, obtain filtrate I and filtered fluid I;
C, take the stirring that adds water of filtered fluid I and be hydrolyzed, the volume ratio of the water and filtered fluid I of addition is 3:1;It is fine using polyester
Dimension carries out suction filtration as screen pack and takes filtrate, obtains filtrate II, and filtrate II is cotton fiber;
D, filtrate I is taken, add the sodium hydroxide solution that mass fraction is 25%, sodium hydroxide solution and filtrate I
Mass ratio is 3:1,4h is reacted at 100 DEG C, is filtered after reaction, is taken filtrate and obtain filtered fluid II;
E, take the stirring that adds water of filtered fluid II and be diluted, the volume ratio of the water and filtered fluid II of addition is 4:1, using poly- third
Alkene fiber carries out suction filtration as screen pack and takes filtrate, obtains filtered fluid III;
F, filtrate III is taken, add hydrochloric acid to carry out acid out, and drying operation is carried out at 200 DEG C, drying time is 2h, is obtained
To terephthalic acid (TPA);
G, take terephthalic acid (TPA) and add ethylene glycol dissolving, the mass ratio of ethylene glycol and terephthalic acid (TPA) is 2:1, it is esterified
Reaction, obtains polyethylene terephthalate.
By the discarded polyester-cotton textiles degraded recovery process, discarded polyester-cotton textiles are progressively decomposed and obtains cotton fiber
And polyethylene terephthalate, it is easy to following cycle to utilize.
Embodiment 2
A kind of discarded polyester-cotton textiles degraded recovery process, comprises the following steps:
A, the cloth that discarded polyester-cotton textiles are broken into 8cm, as raw material;
B, add the SPA that mass fraction is 75% in raw material, the mass ratio of SPA and raw material is 6:1,70
DEG C, react 1.5h under stirring, filter after the completion of reaction, obtain filtrate I and filtered fluid I;
C, take the stirring that adds water of filtered fluid I and be hydrolyzed, the volume ratio of the water and filtered fluid I of addition is 3:1;It is fine using polyester
Dimension carries out suction filtration as screen pack and takes filtrate, obtains filtrate II, and filtrate II is cotton fiber;
D, filtrate I is taken, add the sodium hydroxide solution that mass fraction is 20%, sodium hydroxide solution and filtrate I
Mass ratio is 5:1,6h is reacted at 90 DEG C, is filtered after reaction, is taken filtrate and obtain filtered fluid II;
E, take the stirring that adds water of filtered fluid II and be diluted, the volume ratio of the water and filtered fluid II of addition is 4:1, using poly- third
Alkene fiber carries out suction filtration as screen pack and takes filtrate, obtains filtered fluid III;
F, filtrate III is taken, add hydrochloric acid to carry out acid out, and drying operation is carried out at 160 DEG C, drying time is 4h, is obtained
To terephthalic acid (TPA);
G, take terephthalic acid (TPA) and add ethylene glycol dissolving, the mass ratio of ethylene glycol and terephthalic acid (TPA) is 2:1, it is esterified
Reaction, obtains polyethylene terephthalate.
By the discarded polyester-cotton textiles degraded recovery process, discarded polyester-cotton textiles are progressively decomposed and obtains cotton fiber
And polyethylene terephthalate, it is easy to following cycle to utilize.
Embodiment 3
A kind of discarded polyester-cotton textiles degraded recovery process, comprises the following steps:
A, the cloth that discarded polyester-cotton textiles are broken into 5cm, as raw material;
B, add the SPA that mass fraction is 78% in raw material, the mass ratio of SPA and raw material is 5:1,75
DEG C, react 1h under stirring, filter after the completion of reaction, obtain filtrate I and filtered fluid I;
C, take the stirring that adds water of filtered fluid I and be hydrolyzed, the volume ratio of the water and filtered fluid I of addition is 3:1;Using polypropylene
Fiber carries out suction filtration as screen pack and takes filtrate, obtains filtrate II, and filtrate II is cotton fiber;
D, filtrate I is taken, add the sodium hydroxide solution that mass fraction is 22%, sodium hydroxide solution and filtrate I
Mass ratio is 4:1,5h is reacted at 95 DEG C, is filtered after reaction, is taken filtrate and obtain filtered fluid II;
E, take the stirring that adds water of filtered fluid II and be diluted, the volume ratio of the water and filtered fluid II of addition is 4:1, using polyester
Fiber carries out suction filtration as screen pack and takes filtrate, obtains filtered fluid III;
F, filtrate III is taken, add hydrochloric acid to carry out acid out, and drying operation is carried out at 180 DEG C, drying time is 3h, is obtained
To terephthalic acid (TPA);
G, take terephthalic acid (TPA) and add ethylene glycol dissolving, the mass ratio of ethylene glycol and terephthalic acid (TPA) is 2:1, it is esterified
Reaction, obtains polyethylene terephthalate.
By the discarded polyester-cotton textiles degraded recovery process, discarded polyester-cotton textiles are progressively decomposed and obtains cotton fiber
And polyethylene terephthalate, it is easy to following cycle to utilize.
Embodiment 4
As Figure 1-3, for one kind, the present embodiment realizes that the arbitrary discarded polyester-cotton textiles degraded of embodiment 1-3 is reclaimed
The discarded polyester-cotton textiles degraded recovery system of technique, including the recovery of disintegrating machine 1, conveyer belt 2, acidolysis reaction kettle 3, cotton fiber is instead
Answer kettle 4, Basic fluxing raction kettle 5, just carry reactor 6 and reaction kettle of the esterification 7;The discharging opening of the disintegrating machine 1 passes through conveyer belt 2 and institute
The charging aperture for stating acidolysis reaction kettle 3 is connected, and is removably provided with terylene filter cloth or Buddhist nun at the liquid outlet of the acidolysis reaction kettle 3
Filter medium 31 made by imperial filter cloth, the liquid outlet of the acidolysis reaction kettle 3 and cotton fiber reclaim the inlet of reactor 4 and pass through
Pipeline is connected, and the Basic fluxing raction kettle 5, just carries reactor 6 and reaction kettle of the esterification 7 is sequentially communicated, and the cotton fiber reclaims anti-
Answer kettle 4, Basic fluxing raction kettle 5, just carry that polyester fiber or polypropylene are equipped with the liquid outlet of reactor 6 and reaction kettle of the esterification 7 is fine
Screen pack made by dimension (is not marked in figure);The volume of the acidolysis reaction kettle 3, Basic fluxing raction kettle 5 and reaction kettle of the esterification 7 is optional
For 50,75 or 100L, the electricity that disk sets is equipped with the side wall of the acidolysis reaction kettle 3, Basic fluxing raction kettle 5 and reaction kettle of the esterification 7
Hot coil 8, the pitch of the electric heating coil 8 are chosen as 2,3 or 4cm;Acidolysis reaction kettle 3, Basic fluxing raction kettle 5 and reaction kettle of the esterification
7 inside is equipped with agitator 9.
In view of the corrosivity of acidolysis, alkaline hydrolysis and esterification to reaction equipment, it is to ensure the discarded polyester-cotton textiles
Degraded recovery process is smoothed out, and the acidolysis reaction kettle 3, Basic fluxing raction kettle 5 and reaction kettle of the esterification 7 are stainless using 304
Steel or 316L stainless steels are made.
It should be noted last that, above example is only unrestricted to illustrate technical scheme, although ginseng
The present invention is described in detail according to preferred embodiment, it is be should be understood that to the foregoing is only being embodied as the present invention
Mode, the protection domain being not intended to limit the present invention, it is all within the spirit and principles in the present invention, done any repair
Change, equivalent, improvement etc., should be included within the scope of the present invention.