CN110947733A - Synthetic leather rectification residue recovery process - Google Patents
Synthetic leather rectification residue recovery process Download PDFInfo
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- CN110947733A CN110947733A CN201911228570.5A CN201911228570A CN110947733A CN 110947733 A CN110947733 A CN 110947733A CN 201911228570 A CN201911228570 A CN 201911228570A CN 110947733 A CN110947733 A CN 110947733A
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- synthetic leather
- fiber treating
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- 238000011084 recovery Methods 0.000 title claims abstract description 34
- 239000002649 leather substitute Substances 0.000 title claims abstract description 27
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 97
- 238000005086 pumping Methods 0.000 claims abstract description 31
- 239000000843 powder Substances 0.000 claims abstract description 27
- 239000007788 liquid Substances 0.000 claims abstract description 25
- 238000011049 filling Methods 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 21
- 238000006243 chemical reaction Methods 0.000 claims abstract description 19
- 239000000203 mixture Substances 0.000 claims abstract description 17
- 238000003860 storage Methods 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000012065 filter cake Substances 0.000 claims abstract description 13
- 238000010438 heat treatment Methods 0.000 claims abstract description 10
- 238000003825 pressing Methods 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims abstract description 9
- 239000000706 filtrate Substances 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 239000006228 supernatant Substances 0.000 claims abstract description 5
- 239000000835 fiber Substances 0.000 claims description 75
- 229920006221 acetate fiber Polymers 0.000 claims description 48
- 239000002351 wastewater Substances 0.000 claims description 44
- 239000004952 Polyamide Substances 0.000 claims description 41
- 229920002647 polyamide Polymers 0.000 claims description 41
- QPFMBZIOSGYJDE-UHFFFAOYSA-N 1,1,2,2-tetrachloroethane Chemical compound ClC(Cl)C(Cl)Cl QPFMBZIOSGYJDE-UHFFFAOYSA-N 0.000 claims description 30
- 239000004743 Polypropylene Substances 0.000 claims description 28
- -1 polypropylene Polymers 0.000 claims description 28
- 229920001155 polypropylene Polymers 0.000 claims description 28
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 21
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 claims description 20
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 18
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 18
- RHQDFWAXVIIEBN-UHFFFAOYSA-N Trifluoroethanol Chemical compound OCC(F)(F)F RHQDFWAXVIIEBN-UHFFFAOYSA-N 0.000 claims description 12
- 239000003153 chemical reaction reagent Substances 0.000 claims description 5
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims description 4
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 claims description 4
- 239000011976 maleic acid Substances 0.000 claims description 4
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 claims description 4
- 238000011085 pressure filtration Methods 0.000 claims description 3
- 230000000694 effects Effects 0.000 abstract description 9
- 239000004744 fabric Substances 0.000 description 19
- 230000000052 comparative effect Effects 0.000 description 15
- 150000002978 peroxides Chemical class 0.000 description 9
- 239000007790 solid phase Substances 0.000 description 8
- 239000007791 liquid phase Substances 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 7
- 210000002268 wool Anatomy 0.000 description 7
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 6
- DHKHKXVYLBGOIT-UHFFFAOYSA-N acetaldehyde Diethyl Acetal Natural products CCOC(C)OCC DHKHKXVYLBGOIT-UHFFFAOYSA-N 0.000 description 6
- 150000001241 acetals Chemical class 0.000 description 6
- 238000000926 separation method Methods 0.000 description 5
- 210000004209 hair Anatomy 0.000 description 4
- 239000010985 leather Substances 0.000 description 4
- 239000011259 mixed solution Substances 0.000 description 4
- 239000002893 slag Substances 0.000 description 4
- 229920002284 Cellulose triacetate Polymers 0.000 description 3
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- NNLVGZFZQQXQNW-ADJNRHBOSA-N [(2r,3r,4s,5r,6s)-4,5-diacetyloxy-3-[(2s,3r,4s,5r,6r)-3,4,5-triacetyloxy-6-(acetyloxymethyl)oxan-2-yl]oxy-6-[(2r,3r,4s,5r,6s)-4,5,6-triacetyloxy-2-(acetyloxymethyl)oxan-3-yl]oxyoxan-2-yl]methyl acetate Chemical compound O([C@@H]1O[C@@H]([C@H]([C@H](OC(C)=O)[C@H]1OC(C)=O)O[C@H]1[C@@H]([C@@H](OC(C)=O)[C@H](OC(C)=O)[C@@H](COC(C)=O)O1)OC(C)=O)COC(=O)C)[C@@H]1[C@@H](COC(C)=O)O[C@@H](OC(C)=O)[C@H](OC(C)=O)[C@H]1OC(C)=O NNLVGZFZQQXQNW-ADJNRHBOSA-N 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 239000000945 filler Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000004064 recycling Methods 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 229920006304 triacetate fiber Polymers 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- IKHGUXGNUITLKF-UHFFFAOYSA-N Acetaldehyde Chemical compound CC=O IKHGUXGNUITLKF-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 description 2
- 229920006239 diacetate fiber Polymers 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 229920005610 lignin Polymers 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 241000282414 Homo sapiens Species 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 125000003158 alcohol group Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 229920002301 cellulose acetate Polymers 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000004745 nonwoven fabric Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 125000000864 peroxy group Chemical group O(O*)* 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
- B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
- B09B5/00—Operations not covered by a single other subclass or by a single other group in this subclass
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C231/00—Preparation of carboxylic acid amides
- C07C231/22—Separation; Purification; Stabilisation; Use of additives
- C07C231/24—Separation; Purification
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The invention relates to a synthetic leather rectification residue recovery process, which comprises the following process steps: s1: pumping the rectification residues in the rectification tower into a recovery pot for temporary storage, and pumping the rectification residues temporarily stored in the recovery pot into a reaction kettle when the rectification residues in the recovery pot need to be treated; s2: pumping clear water into the reaction kettle in the step S1, mixing the clear water with the rectification residues, and adding a treating agent for treatment in the heating and stirring process to obtain a turbid liquid; s3: pumping the turbid liquid obtained in the step S2 into a middle tank for standing to obtain a supernatant and a lower solid-liquid mixture; s4: pumping the lower-layer solid-liquid mixture obtained in the step S3 into a filter press for filter pressing to obtain a filter cake and a filtrate; s5: and (5) drying the filter cake obtained in the step (S4), and crushing the dried filter cake by a crusher to obtain the regenerated filling powder. The method has the effect of recovering the filling powder in the synthetic leather rectification residues.
Description
Technical Field
The invention relates to the technical field of waste residue treatment processes, in particular to a synthetic leather rectification residue recovery process.
Background
Along with the increase of world population and the rapid development of economy of all countries, the demand of human beings on leather is multiplied, the animal skin resources are totally deficient, the processing cost is rapidly increased and serious environmental pollution is accompanied, so that the natural leather cannot meet the normal demand of people, and under the condition, the appearance and the development of the synthetic leather make up the shortage of the natural leather in quantity.
Synthetic leather is a material that is formed by artificially synthesizing a base cloth made of a material such as woven cloth, nonwoven cloth, or double-layered leather, and forming a natural leather-like appearance on the base cloth. With the advent of new technology and technology, synthetic leather has incomparable advantages in the aspects of variety, style, design and color, performance and the like.
The rapid development of the synthetic leather industry generates a series of non-negligible environmental pollution problems, wherein the waste residue pollution is mainly residue generated in the process of DMF recycling and rectification, and more than 300 kg of residue can be generated in one production line. Besides part of DMF which is not completely rectified and recycled, the residue also contains a large amount of filling powder added in the artificial leather manufacturing process, such as lignin fiber powder and the like, and the filling powder is insoluble in water and not easy to dissolve in organic solvents and finally becomes a solid phase in the residue to form viscous rectification residue together with liquid-phase DMF.
For example, the patent of Chinese invention with the publication number of CN103130670A discloses a synthetic leather DMF recycling residue treatment process, which comprises the steps of A), generating negative pressure for drying DMF raffinate; B) stirring and heating the entering DMF residual liquid; C) collecting the gas evaporated by heating the DMF residual liquid, condensing the gas, and sending the condensed liquid to a DMF recovery device; D) stopping heating after the DMF residual liquid is evaporated, and cooling dry slag by introducing water; E) and after the dry slag is cooled, exhausting until the dry slag is balanced with the environmental pressure, and then removing the dry slag.
The above prior art solutions have the following drawbacks: in the technical scheme, the rectification residue of DMF is further treated to further recover the residual DMF in the rectification residue, but solid residue still can be generated, the residue belongs to solid dangerous waste and cannot be directly discharged, but the filling powder such as lignin fiber and the like contained in the rectification residue has a certain recovery value, and the treatment modes such as direct incineration, solid waste landfill and the like not only pollute the environment, but also cannot recover the filling powder in the rectification residue, so that a rectification residue recovery process capable of recovering the filling powder in the synthetic leather rectification residue is required.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a synthetic leather rectification residue recovery process which has the effect of recovering filling powder in synthetic leather rectification residues.
The above object of the present invention is achieved by the following technical solutions:
a synthetic leather rectification residue recovery process is characterized in that: the method comprises the following process steps:
s1: pumping the rectification residues in the rectification tower into a recovery pot for temporary storage, and pumping the rectification residues temporarily stored in the recovery pot into a reaction kettle when the rectification residues in the recovery pot need to be treated;
s2: pumping clear water into the reaction kettle in the step S1, mixing the clear water with the rectification residues, and adding a treating agent for treatment in the heating and stirring process to obtain a turbid liquid;
s3: pumping the turbid liquid obtained in the step S2 into a middle tank for standing to obtain a supernatant and a lower solid-liquid mixture;
s4: pumping the lower-layer solid-liquid mixture obtained in the step S3 into a filter press for filter pressing to obtain a filter cake and a filtrate;
s5: and (5) drying the filter cake obtained in the step (S4), and crushing the dried filter cake by a crusher to obtain the regenerated filling powder.
By adopting the technical scheme, because the rectifying tower discharges discontinuously, the rectifying residues obtained by discharging each time need to be pumped into the recovery pot for temporary storage. When the rectification residues are treated, the rectification residues temporarily stored in the recovery pot need to be pumped into the reaction kettle, and then clear water is pumped into the reaction kettle, so that the solid phase in the rectification residues is fully stirred and dispersed in the liquid phase.
Subsequently, a treating agent is added to the reaction vessel, and the cloth fluff which is inevitably present in the rectification residue is treated under the conditions of stirring and heating, so that the solid phase in the mixed solution in step S2 is substantially the filler powder. In order to process more rectification residues, mixed liquor after the reaction in the reaction kettle is finished can be pumped into the intermediate tank for standing, and then the reaction kettle can be used for processing the rectification residues of the next batch. In addition, the solid-liquid phase separation can be caused in the standing process, so that the subsequent solid-liquid separation is convenient.
The solid phase in the mixed liquid with higher solid phase content at the bottom of the middle tank can be subjected to filter pressing separation by carrying out filter pressing on the rectification residue at the bottom of the middle tank. And the filter cake obtained by filter pressing separation is dried and crushed to obtain the regenerated filling powder. Because the output of the rectification residue is large, the pollution of the rectification residue to the environment is reduced by treating and recovering the rectification residue, and a large amount of regenerated filling powder can be recovered by the process, so that the production cost is reduced.
The invention is further configured to: step S6 is further performed after step S5 to recycle wastewater, and step S6 specifically includes the following steps:
step a: pumping the supernatant liquid obtained in the step S3 into a wastewater tank, and pumping the filtrate obtained by pressure filtration in the step S4 into the wastewater tank;
step b: pumping the wastewater in the wastewater tank into a wastewater storage tank;
step c: the wastewater in the wastewater storage tank is pumped into the rectifying tower in step S1.
By adopting the technical scheme, the mixed liquor in the intermediate tank is kept stand, the solid phase content of the mixed liquor on the upper layer is lower, and the mixed liquor can be directly pumped into a wastewater tank as wastewater, so that the workload of the filter press is reduced, and the production efficiency is also improved; and the filtrate obtained by filter pressing of the filter press can be directly pumped into a wastewater tank as wastewater.
Because the rectification recovery of DMF is the discontinuous feeding of multistep, the waste water in the waste water tank can not be transferred to the rectifying tower for rectification once again, therefore, the waste water in the waste water tank is pumped into the waste water storage tank for temporary storage. When the rectifying tower feeds, pumping the wastewater in the wastewater storage tank into the rectifying tower to rectify the wastewater again so as to further recover DMF in the wastewater, thereby recovering DMF and filling powder in the rectification residues.
The invention is further configured to: the treating agent in the step S2 comprises the following components in percentage by weight:
60-80% of polyamide fiber treating agent;
10-20% of acetate fiber treating agent;
10-20% of polypropylene fiber treating agent.
By adopting the technical scheme, in the conventional medium-high-end artificial leather product, the base fabric mostly adopts polyamide fibers as a main body and is obtained by blending with other fibers. In addition to polyamide fibers, acetate fibers and polypropylene fibers are often blended into the base fabric. Among them, acetate fiber has a large water permeability and is easy for the wet production process of artificial leather, while polypropylene fiber is a conventional material of non-woven fabric. Similarly, the fluff falling from the base fabric is mainly the three fibers, and the three fibers are removed.
The invention is further configured to: the polyamide fiber treating agent is selected from one of trifluoroethanol and a mixed reagent, and the mixed reagent is a mixture of phenol and tetrachloroethane.
By adopting the technical scheme, wherein,
when the polyamide fiber treating agent is a mixed reagent, that is, a mixture of phenol and tetrachloroethane, phenol and tetrachloroethane are mixed, and although the mixture of phenol and tetrachloroethane is insoluble in water, DMF is present in the mixed liquid in the reaction kettle, and the mixture of phenol and tetrachloroethane can be dissolved in DMF, so that the mixture of phenol and tetrachloroethane can be well dispersed in the mixed liquid, and the polyamide fibers dispersed in the mixed liquid can be well dissolved.
When the polyamide fiber treating agent is trifluoroethanol, the trifluoroethanol has good water solubility, so that the trifluoroethanol has good dispersibility in the mixed solution, and when the trifluoroethanol is used as a good solvent of the polyamide fiber, the reaction conditions such as high temperature and high pressure are not needed when the trifluoroethanol is dissolved, the polyamide fiber can be dissolved only at normal temperature, and therefore, the energy consumption can be reduced.
The invention is further configured to: in the mixture of phenol and tetrachloroethane in the polyamide fiber treating agent, the mass ratio of phenol to tetrachloroethane is 3: 1.
by adopting the technical scheme, the treatment effect of the polyamide fiber treatment agent is good under the condition of the mixture ratio.
The invention is further configured to: the acetate fiber treating agent comprises the following components in percentage by weight:
by adopting the technical scheme, the dioxane and the acetone are good solvents of the acetate fibers, but the acetate fibers generally comprise diacetate fibers and triacetate fibers. Wherein, the diacetate fiber is soluble in acetone, and the triacetate fiber is insoluble in acetone. Since dioxane can dissolve triacetyl cellulose under the conditions of alcohol and acid, it is possible to sufficiently dissolve the triacetyl cellulose and the triacetyl cellulose by dioxane and acetone.
However, dioxane often produces small amounts of both diethanol acetal and peroxide during storage. Wherein the diethanol acetal can influence the purity of dioxane, peroxide has peroxy group which is an unstable structure and is very sensitive to heating, vibration and impact, once part of peroxide is finally left in a solid phase and is dried and crushed, explosion is very easy to occur, and great potential safety hazard can be caused to the whole production process.
The dioxane can remove impurities after being heated in the environment of strong acid and water, and the trifluoroethanol in the polyamide fiber treating agent is alcohol with stronger acidity, so that the diethanol acetal can be decomposed and removed under the action of the trifluoroethanol. And acetaldehyde generated in the process of removing the diethanol acetal has a low boiling point and is gasified and discharged under the heating condition, so that the purity of the trifluoroethanol is improved. That is, when the polyamide fiber treating agent is trifluoroethanol, it can not only remove polyamide fibers, but also purify dioxane in the acetate fiber treating agent in cooperation with the acetate fiber treating agent, thereby improving the treatment effect of the acetate fiber treating agent on acetate fibers.
And when the polyamide fiber treating agent is a mixture of phenol and tetrachloroethane, phenol has strong reducibility, so that phenol can perform redox reaction with peroxide in dioxane, so that the peroxide in the dioxane is removed, and the risk coefficient of the whole process is reduced.
The invention is further configured to: the acetate fiber treating agent is added in the order of, according to the weight parts, firstly adding dioxane and acetone, and then adding maleic acid and methanol.
By adopting the technical scheme, the dioxane and the acetone are added firstly, so that the dioxane and the acetone can be uniformly dispersed firstly, and then the maleic acid and the methanol are added, so that the acetate fiber can be dissolved, and the acetate fiber is converted into a liquid phase from a solid phase.
The invention is further configured to: the polypropylene fiber treating agent comprises the following components in percentage by weight:
by adopting the technical scheme, the polypropylene fiber can swell in DMF, but cannot be converted into a liquid phase. And the added dichloromethane and cyclohexanone are matched to convert the swollen polypropylene fiber into a liquid phase. And the methanol in the acetate fiber treating agent and the ethyl acetate in the polypropylene fiber treating agent cooperate to further improve the solubility of the acetate fiber. When the polyamide fiber treating agent is phenol and tetrachloroethane, the phenol can purify peroxide in dioxane, and the diethanol acetal can be removed under the action of concentrated sulfuric acid, so that the removal effect of the acetate fiber is further improved. Namely, the diethanol acetal in dioxane in the acetate fiber treating agent is decomposed under the action of concentrated sulfuric acid in the polypropylene fiber treating agent; and peroxide in dioxane in the acetate fiber treating agent is removed under the action of phenol in the polyamide fiber treating agent, so that the purity of dioxane in the acetate fiber treating agent is improved, and the possibility of production safety accidents caused by the peroxide is reduced.
The invention is further configured to: firstly adding polyamide fiber treating agent, then adding acetate fiber treating agent and then adding polypropylene fiber treating agent.
By adopting the technical scheme, wherein,
because the content of the polyamide fiber in the cloth wool is the largest, in order to reduce the influence of the polyamide fiber on the acetate fiber treating agent and the polypropylene fiber treating agent, the polyamide fiber treating agent is added firstly to treat the polyamide fiber.
The subsequent addition of acetate fiber treating agent can treat acetate fiber, and the acetate fiber treating agent is matched with polyamide fiber treating agent to purify or eliminate peroxide from acetate fiber.
The polypropylene fiber treating agent added finally can treat the polypropylene fiber and can further improve the treatment effect of the acetate fiber through the synergy of the polypropylene fiber treating agent and the acetate fiber treating agent.
In conclusion, the beneficial technical effects of the invention are as follows:
1. removing the cloth hair in the rectification residue, and recovering the filling powder in the rectification residue;
2. by carrying out secondary rectification on the wastewater, the DMF in the wastewater can be further recovered, and a treating agent in the wastewater can be rectified and recovered;
3. through the cooperation of the polyamide fiber treating agent, the acetate fiber treating agent and the polypropylene fiber treating agent, solid cloth hair in rectification residues can be converted into a liquid phase, so that filling powder and the cloth hair can be separated during subsequent filter pressing separation.
Detailed Description
Example 1
The invention discloses a synthetic leather rectification residue recovery process, which specifically comprises the following process steps:
s1: pumping the rectification residues in the rectification tower into a recovery pot for temporary storage, and pumping the rectification residues temporarily stored in the recovery pot into a reaction kettle when the rectification residues in the recovery pot need to be treated.
S2: pumping clear water into the reaction kettle in the step S1, mixing the clear water with the rectification residues, stirring at the heating temperature of 40 ℃ and the stirring speed of 1000r/min, adding a treating agent into the reaction kettle in the step S1 during stirring, and treating by using the treating agent to obtain a turbid liquid.
Wherein, the treating agent in the step S2 comprises the following components in percentage by weight:
80% of polyamide fiber treating agent;
10% of acetate fiber treating agent;
10% of polypropylene fiber treating agent.
And the addition sequence of the treating agents is as follows: firstly adding polyamide fiber treating agent, then adding acetate fiber treating agent and then adding polypropylene fiber treating agent.
The polyamide fiber treating agent is a mixture of phenol and tetrachloroethane, wherein the weight ratio of phenol: the mass ratio of tetrachloroethane is 3: 1.
the acetate fiber treating agent comprises the following components in percentage by weight:
and the acetate fiber treating agent is added into the reaction kettle according to the following parts by weight: dioxane and acetone were added first, and after stirring for 5 minutes, maleic acid and methanol were added.
The polypropylene fiber treating agent comprises the following components in percentage by weight:
adding a polyamide fiber treating agent, an acetate fiber treating agent and a polypropylene fiber treating agent into a reaction kettle according to the following parts by weight: firstly adding polyamide fiber treating agent, then adding acetate fiber treating agent and then adding polypropylene fiber treating agent.
S3: pumping the mixed solution obtained in the step S2 into a middle tank, and standing, thereby layering the mixed solution.
S4: and (5) pumping the mixed liquid at the bottom of the intermediate tank in the step S3 into a filter press for filter pressing to obtain a filter cake and a filtrate.
S5: and (5) drying the filter cake obtained in the step (S4), crushing the dried filter cake into 600-mesh particles by using a crusher, and obtaining the regenerated filling powder.
S6: the method for recycling the wastewater specifically comprises the following process steps:
step a, pumping the upper-layer wastewater in the middle tank in the step S3 into a wastewater tank, and pumping the filtrate obtained by pressure filtration in the step S4 into the wastewater tank to transfer and control the flow rate of the wastewater;
b, pumping the wastewater in the wastewater tank into a wastewater storage tank to store the wastewater;
and c, pumping the wastewater in the wastewater storage tank into the rectifying tower in the step S2 to recycle the residual DMF and the treating agent in the wastewater.
Examples 2-5 differ from example 1 in that the weight fraction ratio of the ingredients in the treatment agent is as follows:
example 6 differs from example 1 in that the polyamide treating agent in the treating agent is trifluoroethanol.
Examples 7 to 11 differ from example 1 in that the cellulose acetate fiber treatment agent comprises the following components in the following weight percentages:
examples 12-16 differ from example 1 in that the polypropylene fiber treatment agent comprises the following components in the following weight percentages:
comparative example
Comparative example 1 is different from example 1 in that a treating agent is not added in step S2.
Comparative example 2 is different from example 1 in that a polyamide fiber treating agent was not added in step S2.
Comparative example 3 is different from example 1 in that the acetate fiber treating agent is not added in step S2.
Comparative example 4 is different from example 1 in that the polypropylene fiber treating agent is not added in step S2.
The detection method comprises the following steps:
100g of the reclaimed filler powder subjected to the processes of example 1, comparative example 2, comparative example 3 and comparative example 4 was taken, and the reclaimed filler powder was sieved with a 400-mesh sieve. Although the particle size of the crushed filling powder is normally distributed, the crushed filling powder can basically pass through the sieve opening of a 400-mesh sieve, and the crushed filling powder is not easy to crush due to the strong toughness of the polyamide fiber, the acetate fiber and the polypropylene fiber. Even if the cloth wool is crushed, the cloth wool is often crushed into long fibers due to the characteristics of the cloth wool, and therefore the cloth wool cannot pass through the sieve holes of the 400-mesh sieve, and the aim of separating the cloth wool from the filling powder is fulfilled. The mass of the lint left on the screen after separation is as follows:
by comparing example 1 with comparative example 1, it can be seen that the addition of the treating agent can effectively remove the cloth hair in the rectification residue, thereby improving the purity of the obtained regenerated filling powder and improving the utilization value.
By comparing example 1 with comparative example 2, it can be seen that the most contained polyamide fibers are contained in the cloth wool, and since no polyamide fiber treatment agent is added, the polyamide fibers in the regenerated filling powder are not removed, while the acetate fibers and the polypropylene fibers are removed.
From a comparison between example 1 and comparative example 3, it can be seen that the acetate fibers in the regenerated filling powder were not removed because no acetate fiber treatment agent was added.
By comparing example 1, comparative example 2 and comparative example 4, it can be seen that since the polyamide fiber treating agent is not added in comparative example 2, dioxane in the acetate fiber cannot be purified in cooperation with the polyamide fiber treating agent, and thus purity of dioxane is decreased, resulting in a decrease in the treatment effect on triacetate fiber.
In contrast, in comparative example 4, no polypropylene fiber treatment agent was added, the methanol in the acetate fiber could not cooperate with the ethyl acetate in the polypropylene fiber treatment agent to improve the solubility of the acetate fiber, and thus the treatment effect of the corresponding acetate fiber treatment agent on the acetate fiber was also reduced.
The embodiments of the present invention are preferred embodiments of the present invention, and the scope of the present invention is not limited by these embodiments, so: all equivalent changes made according to the structure, shape and principle of the invention are covered by the protection scope of the invention.
Claims (9)
1. A synthetic leather rectification residue recovery process is characterized in that: the method comprises the following process steps:
s1: pumping the rectification residues in the rectification tower into a recovery pot for temporary storage, and pumping the rectification residues temporarily stored in the recovery pot into a reaction kettle when the rectification residues in the recovery pot need to be treated;
s2: pumping clear water into the reaction kettle in the step S1, mixing the clear water with the rectification residues, and adding a treating agent for treatment in the heating and stirring process to obtain a turbid liquid;
s3: pumping the turbid liquid obtained in the step S2 into a middle tank for standing to obtain a supernatant and a lower solid-liquid mixture;
s4: pumping the lower-layer solid-liquid mixture obtained in the step S3 into a filter press for filter pressing to obtain a filter cake and a filtrate;
s5: and (5) drying the filter cake obtained in the step (S4), and crushing the dried filter cake by a crusher to obtain the regenerated filling powder.
2. The synthetic leather rectification residue recovery process according to claim 1, which is characterized in that: step S6 is further performed after step S5 to recycle wastewater, and step S6 specifically includes the following steps:
step a: pumping the supernatant liquid obtained in the step S3 into a wastewater tank, and pumping the filtrate obtained by pressure filtration in the step S4 into the wastewater tank;
step b: pumping the wastewater in the wastewater tank into a wastewater storage tank;
step c: the wastewater in the wastewater storage tank is pumped into the rectifying tower in step S1.
3. The synthetic leather rectification residue recovery process according to claim 2, which is characterized in that: the treating agent in the step S2 comprises the following components in percentage by weight:
60-80% of polyamide fiber treating agent;
10-20% of acetate fiber treating agent;
10-20% of polypropylene fiber treating agent.
4. The synthetic leather rectification residue recovery process according to claim 3, which is characterized in that: the polyamide fiber treating agent is selected from one of trifluoroethanol and a mixed reagent, and the mixed reagent is a mixture of phenol and tetrachloroethane.
5. The synthetic leather rectification residue recovery process according to claim 4, which is characterized in that: in the mixture of phenol and tetrachloroethane in the polyamide fiber treating agent, the mass ratio of phenol to tetrachloroethane is 3: 1.
6. the synthetic leather rectification residue recovery process according to claim 3, which is characterized in that: the acetate fiber treating agent comprises the following components in percentage by weight:
7. the synthetic leather rectification residue recovery process according to claim 6, which is characterized in that: the addition sequence of the acetate fiber treating agent is as follows: adding dioxane and acetone, and adding maleic acid and methanol.
8. The synthetic leather rectification residue recovery process according to claim 3, which is characterized in that: the polypropylene fiber treating agent comprises the following components in percentage by weight:
9. the synthetic leather rectification residue recovery process according to claim 3, which is characterized in that: the order of addition of the treating agents in step S2 is: firstly adding polyamide fiber treating agent, then adding acetate fiber treating agent and then adding polypropylene fiber treating agent.
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| JP2012144441A (en) * | 2011-01-06 | 2012-08-02 | Idemitsu Kosan Co Ltd | Ionic liquid, purification method of the ionic liquid, and treatment method of cellulose-based biomass |
| CN103130670A (en) * | 2013-01-04 | 2013-06-05 | 南平博士达节能科技有限公司 | Synthetic leather dimethyl formamide (DMF) recycling residue processing technology and synthetic leather DMF recycling residue processing system |
| CN104384172A (en) * | 2014-10-25 | 2015-03-04 | 陈列鑫 | Disposal method for rectification residues in production of synthetic leather |
| CN107962061A (en) * | 2017-12-13 | 2018-04-27 | 广灵金隅水泥有限公司 | A kind of essence bottoms class danger wastes pretreatment unit |
| CN207628878U (en) * | 2017-10-26 | 2018-07-20 | 中节能清洁技术发展有限公司 | The safety system of DMF rectification residue desiccation disposal plants |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2012144441A (en) * | 2011-01-06 | 2012-08-02 | Idemitsu Kosan Co Ltd | Ionic liquid, purification method of the ionic liquid, and treatment method of cellulose-based biomass |
| CN103130670A (en) * | 2013-01-04 | 2013-06-05 | 南平博士达节能科技有限公司 | Synthetic leather dimethyl formamide (DMF) recycling residue processing technology and synthetic leather DMF recycling residue processing system |
| CN104384172A (en) * | 2014-10-25 | 2015-03-04 | 陈列鑫 | Disposal method for rectification residues in production of synthetic leather |
| CN207628878U (en) * | 2017-10-26 | 2018-07-20 | 中节能清洁技术发展有限公司 | The safety system of DMF rectification residue desiccation disposal plants |
| CN107962061A (en) * | 2017-12-13 | 2018-04-27 | 广灵金隅水泥有限公司 | A kind of essence bottoms class danger wastes pretreatment unit |
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