CN106589445A - Meta-aramid byproduct treatment method - Google Patents
Meta-aramid byproduct treatment method Download PDFInfo
- Publication number
- CN106589445A CN106589445A CN201610960758.9A CN201610960758A CN106589445A CN 106589445 A CN106589445 A CN 106589445A CN 201610960758 A CN201610960758 A CN 201610960758A CN 106589445 A CN106589445 A CN 106589445A
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- CN
- China
- Prior art keywords
- aramid
- meta
- ammonium chloride
- solvent
- washing
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Classifications
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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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/26—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from polyamines and polycarboxylic acids
- C08G69/32—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from polyamines and polycarboxylic acids from aromatic diamines and aromatic dicarboxylic acids with both amino and carboxylic groups aromatically bound
-
- 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
- C08J11/02—Recovery or working-up of waste materials of solvents, plasticisers or unreacted monomers
-
- 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
- C08J2377/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
- C08J2377/10—Polyamides derived from aromatically bound amino and carboxyl groups of amino carboxylic acids or of polyamines and polycarboxylic acids
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Sustainable Development (AREA)
- Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)
Abstract
The invention relates to a meta-aramid byproduct treatment method. The meta-aramid byproduct treatment method mainly includes the steps of (1), washing meta-aramid low polymers in an ammonium chloride crude product by a solvent 5-13 times of the weight of the ammonium chloride crude product for 8-15 times; (2), adding 1.3-3.8 times the volume of deionized water into washing liquid in the step (1), and filtering by a filtering device with the filter material pore size 13-68 micrometers after the meta-aramid low polymers are solidified so as to obtain a solid which can be used for manufacturing meta-aramid reins; rectifying filtrate so as to obtain an organic solvent which can be used for washing or producing meta-aramid circularly; (3), removing the solvent from the washed solid obtained in the step (1) by steaming at 10-20 kPa and 95-120 DEG C so as to obtain ammonium chloride with the purity above 99%, and ammonium chloride recovery rate is above 98%. The solvent recovered by condensation can be used for washing or producing the meta-aramid circularly. The meta-aramid byproduct treatment method has the advantages of simplicity, high efficiency and rapidity.
Description
Technical field
The present invention relates to a kind of processing method of meta-aramid byproduct, more particularly to recycling meta-aramid pair
The method of each component in product.
Background technology
Meta-aramid is a kind of important high-performance fiber, and it has an excellent heat-resisting quantity, good dimensional stability,
Excellent spinnability, fire line and corrosion resistance.
During using m-phthaloyl chloride and m-phenylene diamine (MPD) production meta-aramid, accessory substance chlorine is neutralized using ammonia
When changing hydrogen, byproduct ammonium chloride is generated.Process is as follows：
Due to removing main component ammonium chloride in the ammonium chloride byproduct（Accounting about 60%）Outward, solvent is also contained（Accounting about 35%）With
Meta-aramid oligomer（Accounting about 5%）Deng material, this prevents the ammonium chloride byproduct to face from being used directly to downstream industry
Reluctant problem, if directly filling, the waste and serious environmental pollution of material can be caused.At present, there is not yet
The method that relevant report is effectively treated to meta-aramid ammonium chloride byproduct.Therefore, the place of meta-aramid byproduct is developed
Reason method is significant to the green production of meta-aramid.
The content of the invention
The technical problem to be solved in the present invention is to provide a kind of simple, rational method for processing meta-aramid byproduct,
The each material after recovery is re-used, reach the purpose of green production.
A kind of processing method of meta-aramid byproduct, comprises the steps of：
（1）Crude product ammonium chloride is added in container, with the solvent of 5-13 times of crude product weight ammonium chloride, is divided 8-15 time 30 minutes every time
Meta-aramid oligomer in washing crude product ammonium chloride, filters after washing；Wherein solvent for use be N,N-dimethylformamide or
DMAC N,N' dimethyl acetamide；
（2）Combining step（1）Cleaning solution after add deionized water, solidify meta-aramid oligomer therein, the deionization
Water is 1.3-3.3 with the volume ratio of cleaning solution:1；
（3）Filtration step（2）The mixture of formation, selected aperture of filter material is 13-68 microns, filter cake is dried, for making
Make aramid fiber resin；Filtrate is carried out after rectifying, cleaning solvent therein is reclaimed；
（4）Combining step（1）The solid for obtaining, pressure be 10-20kPa, temperature be 95-120 DEG C under the conditions of be evaporated off, return
Receive, respectively obtain dry ammonium chloride and solvent product.
Further, the step（3）The mode of filtration can be centrifugal filtration or plate-frame filtering.
The method that the present invention processes meta-aramid byproduct, the spy of superior product quality process after high with treatment effeciency
Point.The ammonium chloride for being reclaimed is white crystal, and more than 99%, the rate of recovery of ammonium chloride is more than 90% for purity；The meta of recovery
Aramid fiber oligomer can be used to produce meta-aramid resin；Institute's recovered solvent is circularly used for washing or producing meta-aramid.
Specific embodiment
Example 1：
（1）The crude product ammonium chloride of 1000Kg is added in the kettle with stirring, is washed slightly with 1250Kg DMFs
After product ammonium chloride 30 minutes, filter, repeat this washing operation, wash 8 times altogether；
（2）Will（1）After the cleaning solution of middle gained merges, 2.3 times of deionized water is added thereto to, solidifies meta-aramid therein
Oligomer, then filtered with flame filter press, aperture of filter material is 35-55 microns, and resulting solid is after drying meta
Aramid fiber oligomer, altogether 348Kg, can be used to manufacture meta-aramid resin；Liquid after filtration be N,N-dimethylformamide with
The mixture of water, Jing after rectifying, DMF is circularly used for washing or manufacturing meta-aramid；
（3）Will（1）After the solid of middle gained merges, pressure be 13-18KPa, temperature be to be evaporated off at 105-115 DEG C, reclaim（1）
The solvent contained in solid after middle washing, obtains 588Kg chloride solids, and the rate of recovery is 98.1%, and the ammonium chloride after recovery is pure
Spend for 99.5%, reach industrial ammonium chloride high-class product standard.
Example 2
（1）The crude product ammonium chloride of 1000kg is added in the kettle with stirring, is washed slightly with 1250kg DMAs
After product ammonium chloride 30 minutes, filter, repeat this washing, wash 15 times altogether；
（2）Will（1）After the cleaning solution of middle gained merges, 2.7 times of deionized water is added thereto to, solidifies meta-aramid therein
Oligomer, then filtered with flame filter press, aperture of filter material is 33-48 microns, and resulting solid is after drying meta
Aramid fiber oligomer, altogether 342kg, can be used to manufacture meta-aramid resin；Liquid after filtration be N,N-dimethylformamide with
The mixture of water, Jing after rectifying, DMF is circularly used for washing or manufacturing meta-aramid；
（3）Will（1）After the solid of middle gained merges, pressure be 13-17kPa, temperature be to be evaporated off at 105-118 DEG C, reclaim（1）
The solvent contained in solid after middle washing, obtains 595kg chloride solids, and the rate of recovery is 99.2%, and the ammonium chloride after recovery is pure
Spend for 99.4%, reach industrial ammonium chloride Grade A standard.
Above example is only that the preferred embodiment of the present invention is described, and not the scope of the present invention is limited
Fixed, on the premise of without departing from design spirit of the present invention, those of ordinary skill in the art make to technical scheme
Various modifications and improvement, all should fall within the protection domain of claims of the present invention determination.
Claims (2)
1. a kind of processing method of meta-aramid byproduct, it is characterised in that comprise the steps of：
（1）Crude product ammonium chloride is added in container, with the solvent of 5-13 times of crude product weight ammonium chloride, is divided 8-15 time 30 minutes every time
Meta-aramid oligomer in washing crude product ammonium chloride, filters after washing；Wherein solvent for use be N,N-dimethylformamide or
DMAC N,N' dimethyl acetamide；
（2）Combining step（1）Cleaning solution after add deionized water, solidify meta-aramid oligomer therein, the deionization
Water is 1.3-3.3 with the volume ratio of cleaning solution:1；
（3）Filtration step（2）The mixture of formation, selected aperture of filter material is 13-68 microns, filter cake is dried, for making
Make aramid fiber resin；Filtrate is carried out after rectifying, cleaning solvent therein is reclaimed；
（4）Combining step（1）The solid for obtaining, pressure be 10-20kPa, temperature be 95-120 DEG C under the conditions of be evaporated off, return
Receive, respectively obtain dry ammonium chloride and solvent product.
2. the processing method of a kind of meta-aramid byproduct according to claim 1, it is characterised in that：The step（3）
The mode of filtration be centrifugal filtration or plate-frame filtering.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610960758.9A CN106589445A (en) | 2016-11-04 | 2016-11-04 | Meta-aramid byproduct treatment method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610960758.9A CN106589445A (en) | 2016-11-04 | 2016-11-04 | Meta-aramid byproduct treatment method |
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| Publication Number | Publication Date |
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| CN106589445A true CN106589445A (en) | 2017-04-26 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201610960758.9A Pending CN106589445A (en) | 2016-11-04 | 2016-11-04 | Meta-aramid byproduct treatment method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107446131A (en) * | 2017-08-25 | 2017-12-08 | 广东彩艳股份有限公司 | A kind of meta-aramid polymerization new technology of energy-conserving and environment-protective |
| CN116023652A (en) * | 2023-01-16 | 2023-04-28 | 清华大学 | Treatment method of meta-aramid polymerization waste liquid |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103113576A (en) * | 2013-01-25 | 2013-05-22 | 杭州九隆芳纶有限公司 | Batch polymerization method of aramid 1313 |
| CN103806121A (en) * | 2013-04-22 | 2014-05-21 | 圣欧芳纶（江苏）股份有限公司 | Method for preparing polyisophthaloyl metaphenylene diamine solution without metal ions |
| CN103980145A (en) * | 2014-05-28 | 2014-08-13 | 深圳市灿森科技有限公司 | Recovery method of waste liquid in production process of salt-free m-aramid fiber |
-
2016
- 2016-11-04 CN CN201610960758.9A patent/CN106589445A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103113576A (en) * | 2013-01-25 | 2013-05-22 | 杭州九隆芳纶有限公司 | Batch polymerization method of aramid 1313 |
| CN103806121A (en) * | 2013-04-22 | 2014-05-21 | 圣欧芳纶（江苏）股份有限公司 | Method for preparing polyisophthaloyl metaphenylene diamine solution without metal ions |
| CN103980145A (en) * | 2014-05-28 | 2014-08-13 | 深圳市灿森科技有限公司 | Recovery method of waste liquid in production process of salt-free m-aramid fiber |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107446131A (en) * | 2017-08-25 | 2017-12-08 | 广东彩艳股份有限公司 | A kind of meta-aramid polymerization new technology of energy-conserving and environment-protective |
| CN116023652A (en) * | 2023-01-16 | 2023-04-28 | 清华大学 | Treatment method of meta-aramid polymerization waste liquid |
| CN116023652B (en) * | 2023-01-16 | 2023-10-27 | 清华大学 | Treatment method of meta-aramid polymerization waste liquid |
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Application publication date: 20170426 |