CN104893147A - Method for safely dechlorinating waste polyvinyl chloride and preparing high-purity ammonia chloride - Google Patents
Method for safely dechlorinating waste polyvinyl chloride and preparing high-purity ammonia chloride Download PDFInfo
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- CN104893147A CN104893147A CN201510278098.1A CN201510278098A CN104893147A CN 104893147 A CN104893147 A CN 104893147A CN 201510278098 A CN201510278098 A CN 201510278098A CN 104893147 A CN104893147 A CN 104893147A
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- polyvinyl chloride
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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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/16—Halides of ammonium
- C01C1/164—Ammonium chloride
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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
- C08J2327/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
- C08J2327/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
- C08J2327/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
- C08J2327/06—Homopolymers or copolymers of vinyl chloride
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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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/141—Feedstock
- Y02P20/143—Feedstock the feedstock being recycled material, e.g. plastics
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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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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Sustainable Development (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Inorganic Chemistry (AREA)
- Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)
Abstract
The invention discloses a method for safely dechlorinating waste polyvinyl chloride and preparing high-purity ammonia chloride. The method comprises the following steps of: 1, performing subcritical ammonia water treatment on the waste polyvinyl chloride; 2, performing solid-liquid separation and oil-water separation on the mixed product; and 3, performing heating evaporative crystallization on the aqueous product. By the method, the waste polyvinyl chloride is subjected to subcritical ammonia water treatment; the waste polyvinyl chloride is dechlorinated efficiently and safely and the high-purity ammonia chloride product is obtained by recycling; and the ammonia water has a good absorption and separation effect on hydrogen chloride generated by decomposing the waste polyvinyl chloride. The method has the advantages that the process equipment is simple; the cost is saved; the treatment process is simple; pollution is avoided; resource utilization is realized while the waste polyvinyl chloride is dechlorinated safely; resource utilization of the waste is realized; environment is protected; and environmental benefit and economical benefit are unified.
Description
Technical field
The invention belongs to field of waste recycle, particularly relate to the safe dechlorination of a kind of waste polyvinyl chloride and prepare the method for high-purity ammonium chloride.
Background technology
Polyvinyl chloride is formed by radical polymerization by vinylchlorid, and be one of five large resins for universal use, its product has good process based prediction model, is widely used in all trades and professions.Along with the growth of polrvinyl chloride product consumption, the quantity of its waste also becomes geometry multiple to increase, and adds its natural degradation time long and long-term existence in the environment, forms white pollution.Containing a large amount of stablizers in polyvinyl chloride product, the additives such as softening agent, lubricant, forming agent, tinting material, impact modifier, wherein many to environment and human hazard, so waste polyvinyl chloride has formed serious threat to the environment that the mankind depend on for existence.
Treatment process at present for waste polyvinyl chloride mainly contains: regeneration, burning and thermo-cracking etc.Regeneration comprises Direct Regeneration and modification regeneration two kinds of modes: Direct Regeneration produces recycled product by granulation add suitable additive in waste polyvinyl chloride after; Modification regeneration is shaping to the modified reprocessing of waste polyvinyl chloride by the method for physics and chemistry.Burning disposal process discharges and is formed outside acid rain in a large amount of hydrogen chloride gas entered environment, also can generate the highly toxic substances such as Dioxins, and also very serious to the corrosion of burning facility.Comparatively speaking, thermo-cracking is a kind for the treatment of process few with environmental pollution of comparatively making rational use of resources, but, thermo-cracking still needs special device to collect the hydrogen chloride gas of generation, simultaneously, due to cannot hydrogenchloride in time in separating reaction system and cause the generation of chlorinatedorganic, therefore, still there is larger environmental risk in thermo-cracking process waste polyvinyl chloride.So, how again can in time by the HCl separation in reactive system while the safe dechlorination of waste polyvinyl chloride, the harmless resource utilization for waste polyvinyl chloride is disposed significant.
For above-mentioned present situation, the present invention, in conjunction with the physics-chem characteristic of waste polyvinyl chloride, adopts subcritical ammoniacal liquor reaction technology for the safe dechlorination of waste polyvinyl chloride and prepares high-purity ammonium chloride simultaneously.In subcritical ammoniacal liquor reaction system, the water molecules being in subcritical water condition is obvious for the promoter action of polyvinyl chloride dechlorination reaction, and the hydrogenchloride generated is very easily by the ammonia absorption in reactive system, thus not only avoid the corrosion of hydrogenchloride to conversion unit, with organic reaction in system, good restraining effect is played further to hydrogenchloride simultaneously, avoid the generation of the toxic intermediates such as chlorinatedorganic.In addition, after the completion of reaction, high-purity ammonium chloride can be obtained by being separated after the water-phase product obtained carries out heating evaporation crystallization, thus realize resource utilization recovery, there is good environmental benefit and economic benefit.
At present, be used for the safe dechlorination of waste polyvinyl chloride for adopting subcritical ammoniacal liquor technology and prepare the method for high-purity ammonium chloride simultaneously, there is not been reported.
Summary of the invention
For solving the problem, the invention provides the safe dechlorination of a kind of waste polyvinyl chloride and preparing the method for high-purity ammonium chloride.The present invention adopts subcritical ammoniacal liquor reaction technology, the method of high-purity ammonium chloride product is prepared while the safe dechlorination of waste polyvinyl chloride, solve the problem of environmental pollution of waste polyvinyl chloride hydrogenchloride in removal process, provide with low cost simultaneously, technique is simple, highly purified ammonium chloride product.
For reaching above-mentioned technique effect, technical scheme of the present invention is:
The safe dechlorination of waste polyvinyl chloride also prepares the method for high-purity ammonium chloride, comprises the steps:
The subcritical ammonia treatment of step one, waste polyvinyl chloride: waste polyvinyl chloride is cut into fragment and is placed in high-temperature high-pressure reaction kettle, then the ammoniacal liquor that concentration is 5 ~ 15% is added, controlling solid-to-liquid ratio is 1:2g/mL – 1:10g/mL, closed high temperature autoclave, it is 200 ~ 300 DEG C in temperature of reaction, pressure is react 15 ~ 45 minutes under the condition of 1 ~ 5MPa, obtains mix products;
The solid-liquid separation of step 2, mix products and oily water separation: mix products is cooled to room temperature, filter after then being taken out by mix products, obtain filtrate; Dichloromethane extraction liquid and water-phase product is formed by the oil-phase product in dichloromethane extraction filtrate, after dichloromethane extraction liquid is dewatered by anhydrous sodium sulphate, by Rotary Evaporators by the methylene dichloride in dichloromethane extraction liquid and separating of oil, obtain not chloride oil; Methylene dichloride after being separated is reclaimed and recycles;
The heating evaporation crystallization of step 3, water-phase product: the crystallization of water-phase product heating evaporation is obtained high-purity ammonium chloride.
Further improvement, in described step one, the concentration of ammoniacal liquor is 10%.
Further improvement, in described step one, solid-to-liquid ratio is 1:5g/mL.
Further improvement, in described step one, pressure is 2.5MPa, and the reaction times is 30 minutes.
Further improvement, in described step one, cuts into the fragment that size is less than 1cm × 1cm by waste polyvinyl chloride.
Advantage of the present invention:
1, by the subcritical ammonia treatment to waste polyvinyl chloride, reclaim while highly effective and safe dechlorination and obtain high-purity ammonium chloride product.
2, ammoniacal liquor plays good absorption extraction effect to the hydrogenchloride that waste polyvinyl chloride decomposes generation.
3, processing unit is simple, cost-saving, does not pollute.
4, changing waste into resources utilizes, and protects environment, realizes the unification of environmental benefit and economic benefit.
Accompanying drawing explanation
Fig. 1 is schematic flow sheet of the present invention.
Embodiment
Embodiment 1
The safe dechlorination of waste polyvinyl chloride as a kind of in Fig. 1 also prepares the method for high-purity ammonium chloride, comprises the steps:
The subcritical ammonia treatment of step one, waste polyvinyl chloride: 5 grams of waste polyvinyl chlorides are cut into the fragment being less than 1cm × 1cm and is placed in high-temperature high-pressure reaction kettle, then the ammoniacal liquor that concentration is 5% is added, control solid-to-liquid ratio is 1:2g/mL, closed high temperature autoclave, it is 200 DEG C in temperature of reaction, pressure is react 15 minutes under the condition of 1MPa, obtains mix products;
The solid-liquid separation of step 2, mix products and oily water separation: mix products is cooled to room temperature, filter after then being taken out by mix products, obtain filtrate; Dichloromethane extraction liquid and water-phase product is formed by the oil-phase product in dichloromethane extraction filtrate, after dichloromethane extraction liquid is dewatered by anhydrous sodium sulphate, by Rotary Evaporators by the methylene dichloride in dichloromethane extraction liquid and separating of oil, obtain not chloride oil; Methylene dichloride after being separated is reclaimed and recycles;
The heating evaporation crystallization of step 3, water-phase product: the crystallization of water-phase product heating evaporation is obtained high-purity ammonium chloride.
By determining the dechlorination effect of subcritical ammonia treatment to waste polyvinyl chloride to the analysis of cl content in initial Determination of Chloride in Polyvinyl Chloride content and reaction residues, its dechlorination efficiency is 65.7%.The purity of ammonium chloride is 99.8%, reaches industrial ammonium chloride premium grads standard.
Embodiment 2
The safe dechlorination of waste polyvinyl chloride as a kind of in Fig. 1 also prepares the method for high-purity ammonium chloride, comprises the steps:
The subcritical ammonia treatment of step one, waste polyvinyl chloride: 5 grams of waste polyvinyl chlorides are cut into the fragment being less than 1cm × 1cm and is placed in high-temperature high-pressure reaction kettle, then the ammoniacal liquor that concentration is 10% is added, control solid-to-liquid ratio is 1:5g/mL, closed high temperature autoclave, it is 250 DEG C in temperature of reaction, pressure is react 15 minutes under the condition of 2.5MPa, obtains mix products;
The solid-liquid separation of step 2, mix products and oily water separation: mix products is cooled to room temperature, filter after then being taken out by mix products, obtain filtrate; Dichloromethane extraction liquid and water-phase product is formed by the oil-phase product in dichloromethane extraction filtrate, after dichloromethane extraction liquid is dewatered by anhydrous sodium sulphate, by Rotary Evaporators by the methylene dichloride in dichloromethane extraction liquid and separating of oil, obtain not chloride oil; Methylene dichloride after being separated is reclaimed and recycles;
The heating evaporation crystallization of step 3, water-phase product: the crystallization of water-phase product heating evaporation is obtained high-purity ammonium chloride.
By determining the dechlorination effect of subcritical ammonia treatment to waste polyvinyl chloride to the analysis of cl content in initial Determination of Chloride in Polyvinyl Chloride content and reaction residues, its dechlorination efficiency is 100%.The purity of ammonium chloride is 99.8%, reaches industrial ammonium chloride premium grads standard.
Embodiment 3
The safe dechlorination of waste polyvinyl chloride as a kind of in Fig. 1 also prepares the method for high-purity ammonium chloride, comprises the steps:
The subcritical ammonia treatment of step one, waste polyvinyl chloride: 5 grams of waste polyvinyl chlorides are cut into the fragment being less than 1cm × 1cm and is placed in high-temperature high-pressure reaction kettle, then the ammoniacal liquor that concentration is 15% is added, control solid-to-liquid ratio is 1:10g/mL, closed high temperature autoclave, it is 300 DEG C in temperature of reaction, pressure is react 45 minutes under the condition of 5MPa, obtains mix products;
The solid-liquid separation of step 2, mix products and oily water separation: mix products is cooled to room temperature, filter after then being taken out by mix products, obtain filtrate; Dichloromethane extraction liquid and water-phase product is formed by the oil-phase product in dichloromethane extraction filtrate, after dichloromethane extraction liquid is dewatered by anhydrous sodium sulphate, by Rotary Evaporators by the methylene dichloride in dichloromethane extraction liquid and separating of oil, obtain not chloride oil; Methylene dichloride after being separated is reclaimed and recycles;
The heating evaporation crystallization of step 3, water-phase product: the crystallization of water-phase product heating evaporation is obtained high-purity ammonium chloride.
By determining the dechlorination effect of subcritical ammonia treatment to waste polyvinyl chloride to the analysis of cl content in initial Determination of Chloride in Polyvinyl Chloride content and reaction residues, its dechlorination efficiency is 100%.The purity of ammonium chloride is 99.8%, reaches industrial ammonium chloride premium grads standard.
By determining the dechlorination effect of subcritical ammonia treatment to waste polyvinyl chloride to the analysis of cl content in initial Determination of Chloride in Polyvinyl Chloride content and reaction residues, its dechlorination efficiency is 100%.The purity of ammonium chloride is 99.8%, reaches industrial ammonium chloride premium grads standard.
The results show the inventive method of above-described embodiment 1-3 has dechlorination effect safely and efficiently for waste polyvinyl chloride, and can also obtain highly purified ammonium chloride product simultaneously.In addition, because the inventive method adds the absorption agent of ammoniacal liquor as hydrogenchloride in the dechlorination reaction of polyvinyl chloride, thus the generation of the intermediate products such as such as chloro toxic organic compound is avoided, whole treating processes safety non-toxic, non-secondary pollution.In treating processes, the concentration of ammoniacal liquor, solid-to-liquid ratio, temperature of reaction, pressure, time are key parameters, on dechlorination effect impact significantly.When ammonia concn is greater than 10%, solid-to-liquid ratio is less than 1:5g/mL, and temperature is greater than 250 DEG C, and pressure is greater than 2.5MPa, and when the reaction times is greater than 30 minutes, the dechlorination effect of waste polyvinyl chloride reaches 100%, and the purity of ammonia chloride of acquisition reaches 99.8%.
The present invention, in conjunction with the physics-chem characteristic of waste polyvinyl chloride, adopts subcritical ammoniacal liquor reaction technology for the safe dechlorination of waste polyvinyl chloride and prepares high-purity ammonium chloride simultaneously.In subcritical ammoniacal liquor reaction system, the water molecules being in subcritical water condition is obvious for the promoter action of polyvinyl chloride dechlorination reaction, and the hydrogenchloride generated is very easily by the ammonia absorption in reactive system, thus not only avoid the corrosion of hydrogenchloride to conversion unit, with organic reaction in system, good restraining effect is played further to hydrogenchloride simultaneously, avoid the generation of the toxic intermediates such as chlorinatedorganic.In addition, after the completion of reaction, high-purity ammonium chloride can be obtained by being separated after the water-phase product obtained carries out heating evaporation crystallization, thus realize resource utilization recovery, there is good environmental benefit and economic benefit.
The explanation of above example just understands core concept of the present invention for helping; Meanwhile, for one of ordinary skill in the art, according to thought of the present invention, all will change in specific embodiments and applications, in sum, this description should not be construed as limitation of the present invention.
Claims (5)
1. the safe dechlorination of waste polyvinyl chloride prepare the method for high-purity ammonium chloride, is characterized in that, comprise the steps:
The subcritical ammonia treatment of step one, waste polyvinyl chloride: waste polyvinyl chloride is cut into fragment and is placed in high-temperature high-pressure reaction kettle, then the ammoniacal liquor that concentration is 5 ~ 15% is added, controlling solid-to-liquid ratio is 1:2g/mL – 1:10g/mL, closed high temperature autoclave, it is 200 ~ 300 DEG C in temperature of reaction, pressure is react 15 ~ 45 minutes under the condition of 1 ~ 5MPa, obtains mix products;
The solid-liquid separation of step 2, mix products and oily water separation: mix products is cooled to room temperature, filter after then being taken out by mix products, obtain filtrate; Dichloromethane extraction liquid and water-phase product is formed by the oil-phase product in dichloromethane extraction filtrate, after dichloromethane extraction liquid is dewatered by anhydrous sodium sulphate, by Rotary Evaporators by the methylene dichloride in dichloromethane extraction liquid and separating of oil, obtain not chloride oil; Methylene dichloride after being separated is reclaimed and recycles;
The heating evaporation crystallization of step 3, water-phase product: the crystallization of water-phase product heating evaporation is obtained high-purity ammonium chloride.
2. the safe dechlorination of waste polyvinyl chloride as claimed in claim 1 prepare the method for high-purity ammonium chloride, it is characterized in that, in described step one, the concentration of ammoniacal liquor is 10%.
3. the safe dechlorination of waste polyvinyl chloride as claimed in claim 1 prepare the method for high-purity ammonium chloride, it is characterized in that, in described step one, solid-to-liquid ratio is 1:5g/mL.
4. the safe dechlorination of waste polyvinyl chloride as claimed in claim 1 prepare the method for high-purity ammonium chloride, it is characterized in that, in described step one, pressure is 2.5MPa, and temperature of reaction is 250 DEG C, and the reaction times is 30 minutes.
5. the safe dechlorination of waste polyvinyl chloride as claimed in claim 1 prepare the method for high-purity ammonium chloride, is characterized in that, in described step one, waste polyvinyl chloride is cut into the fragment that size is less than 1cm × 1cm.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105236446A (en) * | 2015-11-24 | 2016-01-13 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for recycling waste hydrochloric acid |
| CN106831548A (en) * | 2017-03-24 | 2017-06-13 | 福建工程学院 | The processing method and its device of a kind of electronic waste epoxy resin |
| CN111333249A (en) * | 2020-03-16 | 2020-06-26 | 新地环保技术有限公司 | Method for treating waste liquid containing chlorinated organic matter |
| CN111777053A (en) * | 2020-06-27 | 2020-10-16 | 同济大学 | Polyvinyl chloride waste treatment method |
| CN114540070A (en) * | 2022-02-08 | 2022-05-27 | 中国石油大学(华东) | Method and process for dechlorinating coal tar |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105236446A (en) * | 2015-11-24 | 2016-01-13 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for recycling waste hydrochloric acid |
| CN106831548A (en) * | 2017-03-24 | 2017-06-13 | 福建工程学院 | The processing method and its device of a kind of electronic waste epoxy resin |
| CN111333249A (en) * | 2020-03-16 | 2020-06-26 | 新地环保技术有限公司 | Method for treating waste liquid containing chlorinated organic matter |
| CN111777053A (en) * | 2020-06-27 | 2020-10-16 | 同济大学 | Polyvinyl chloride waste treatment method |
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| CN114540070A (en) * | 2022-02-08 | 2022-05-27 | 中国石油大学(华东) | Method and process for dechlorinating coal tar |
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Application publication date: 20150909 |