CN106810672A - A kind of production technology of waste polyester polyurethane foam material - Google Patents
A kind of production technology of waste polyester polyurethane foam material Download PDFInfo
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- CN106810672A CN106810672A CN201510845911.9A CN201510845911A CN106810672A CN 106810672 A CN106810672 A CN 106810672A CN 201510845911 A CN201510845911 A CN 201510845911A CN 106810672 A CN106810672 A CN 106810672A
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- polyurethane foam
- foam material
- waste polyester
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/03—Preparation of carboxylic acid esters by reacting an ester group with a hydroxy group
-
- 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
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/32—Polyhydroxy compounds; Polyamines; Hydroxyamines
-
- 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
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
- C08G18/76—Polyisocyanates or polyisothiocyanates cyclic aromatic
- C08G18/7657—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings
- C08G18/7664—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings containing alkylene polyphenyl groups
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)
Abstract
A kind of production technology of waste polyester polyurethane foam material, it is main to utilize glycolysis alcoholysis method degraded waste polyester fibers, obtain ethylene glycol terephthalate (BHET), after repeatedly washing, crystallization, purification, reacted with-NCO the bases in polyisocyanates (PAPI), prepare polyurethane foam material.The present invention is prepared for polyurethane foam material using waste polyester fibers, both the recovery of waste polyester fibers and polyurethane foam material are organically combined, the process problem of waste polyester fibers can not only be solved, and the polyurethane foam material intensity that obtains is high, light weight, using extensive and with low cost.
Description
Technical field
A kind of method that utilization waste polyester fibers produce polyurethane foam material, after specifically related to one kind obtains ethylene glycol terephthalate using degradation of ethylene glycol waste polyester fibers, with the method that polyisocyanates reaction prepares polyurethane foam material, belong to polyester degraded, macromolecular material foaming technique field.
Background technology
Polyester fiber is widely used as a kind of macromolecular material in industry-by-industry, simultaneously, the quantity of waste polyester is also increasingly increasing, if not carrying out recycling utilization to waste polyester, not only result in the wasting of resources, but also substantial amounts of pollution can be brought to environment, therefore, the recycling of waste polyester becomes the great research topic of current polyester industrial development.In addition, China's building energy consumption is lifted continuously and healthily in recent years, building energy conservation turns into the hot issue of whole society's concern, and hard polyurethane foams are a kind of very outstanding heat preserving and insulating materials, it is mainly used in the industrial uses such as exterior-wall heat insulation, this can increase the usable area of interior of building, and to land price, there is special attraction in more and more expensive city.Therefore polyester is reclaimed and both polyurethane foams organically combines, can not only solve the process problem of waste polyester, and the expanded material intensity for obtaining is high, light weight, and it is with low cost.
The content of the invention
It is an object of the invention to provide a kind of method that utilization waste polyester fibers produce polyurethane foam material, by waste polyester fibers and glycol reaction, reduce molecular weight of polyesters, obtain monomer PET (BHET), after crystallized purification, BHET purity is up to 96%.On this basis, reacted by two-OH on the BHET and-NCO in polyisocyanates (PAPI), polyurethane foam material is prepared by the growth of a series of chain, gas generation and cross-linking reaction etc..
Technical scheme：A kind of method that utilization waste polyester fibers produce polyurethane foam material, using glycolysis alcoholysis process degradation waste polyester fibers, obtains ethylene glycol terephthalate BHET, then obtains polyurethane foam material by BHET foaming, and step is as follows：Count by weight：
(1) degraded of waste polyester fibers：
A, installation reaction unit：Four-hole boiling flask is taken for reaction vessel, wherein three mouthfuls dispose thermometer, reflux condensate device and logical nitrogen device respectively；
B, degradation reaction：Take 200~400 parts of ethylene glycol, 0.2~0.5 part of catalyst acetic acid zinc and add four-hole boiling flask mixing, four-hole boiling flask is put into oil bath pan, intensification is heated to zinc acetate and is completely dissolved；Take the cleaning of 150 parts of waste polyester fibers, dry after add reaction unit, open logical nitrogen device and be passed through nitrogen to exclude the oxygen in flask, be to slowly warm up to 185 DEG C of the boiling point of ethylene glycol, reflux condensate device occurs to be incubated after backflow phenomenon to continue to react 3~6h；Own backflow phenomenon rises and 1~2mL is sampled per half an hour；
C, sample treatment：The gasoline and dimethylbenzene for taking isometric ratio are sufficiently mixed and are configured to solvent；After the sample obtained in step b is cooled into room temperature, configured solvent sample dissolution is added；Stop reaction when during samples taken can be dissolved completely in solvent；
(2) preparation of BHET monomers：Step (1) gained mixed solution is cooled to 130~150 DEG C, is poured into the beaker equipped with distilled water, be heated to 90~100 DEG C, carry out being filtrated to get filtrate during the transparent shape of solution, filtrate is put into 8~10h in ice bath, separates out spicule crystal, refilters；Repeat aforesaid operations 3~4 times, you can obtain BHET monomers；
(3) preparation of polyurethane foam material：Take 100 parts of step (2) gained BHET monomers, foaming agent polyisocyanates PAPI90~110 part, 3~5 parts of water, 3~8 parts of octoate catalyst stannous, 2~5 parts of solubilizer silicone oil is sequentially added in reaction flask, mixing and stirring is to start foamable reaction, foamed after anti-1~3 minute and finished, obtain polyurethane foam material crude product；20~40h curings will be placed under gained polyurethane foam material crude product normal temperature and pressure and obtains product polyurethane foam material.
The performance of polyurethane foam material prepared by above-mentioned steps：Fusing point is 145~155 DEG C, and temperature of initial decomposition is 220~240 DEG C, 650~700KPa of compressive strength, 90~100kgm of density-3。
Advantages of the present invention：The present invention is prepared for polyurethane foam material using waste polyester fibers, both the recovery of waste polyester fibers and polyurethane foam material are organically combined, the process problem of waste polyester fibers can not only be solved, and the polyurethane foam material intensity that obtains is high, light weight, using extensive and with low cost.
Specific embodiment
The invention will be further elaborated by the following examples, the purpose is to be best understood from present disclosure.
Therefore, institute's illustrated example has no effect on protection scope of the present invention.
Embodiment 1
(1) degraded of waste polyester fibers：
A, installation reaction unit：Four-hole boiling flask is taken for reaction vessel, wherein three mouthfuls dispose thermometer, reflux condensate device and logical nitrogen device respectively；
B, degradation reaction：Take 300 parts of ethylene glycol, 0.4 part of catalyst acetic acid zinc and add four-hole boiling flask mixing, four-hole boiling flask is put into oil bath pan, intensification is heated to zinc acetate and is completely dissolved；Take the cleaning of 140 parts of waste polyester fibers, dry after add reaction unit, open logical nitrogen device and be passed through nitrogen to exclude the oxygen in flask, be to slowly warm up to 185 DEG C of the boiling point of ethylene glycol, reflux condensate device occurs to be incubated after backflow phenomenon to continue to react 5h；Own backflow phenomenon rises and 1.5mL is sampled per half an hour；
C, sample treatment：No. 94 gasoline and dimethylbenzene for taking isometric ratio are sufficiently mixed and are configured to solvent；After the sample obtained in step b is cooled into room temperature, configured solvent sample dissolution is added；Stop reaction when during samples taken can be dissolved completely in solvent；
(2) preparation of BHET monomers：Step (1) gained mixed solution is cooled to 140 DEG C, is poured into the beaker equipped with distilled water, be heated to 95 DEG C, carry out being filtrated to get filtrate during the transparent shape of solution, filtrate is put into 9h in ice bath, separates out spicule crystal, refilters；Repeat aforesaid operations 4 times, you can obtain BHET monomers；
(3) preparation of polyurethane foam material：Take 100 parts of step (2) gained BHET monomers, 100 parts of foaming agent polyisocyanates PAPI, 2 parts of water, 3 parts of octoate catalyst stannous, 2 parts of solubilizer silicone oil is sequentially added in reaction flask, mixing and stirring is to start foamable reaction, reaction is foamed after 1.5 minutes and is finished, and obtains polyurethane foam material crude product；24h curings will be placed under gained polyurethane foam material crude product normal temperature and pressure and obtains product polyurethane foam material.
The fusing point of the polyurethane foam material for obtaining is 156 DEG C, and temperature of initial decomposition is 240 DEG C, compressive strength 724KPa, density 99kgm-3。
Embodiment 2
(1) degraded of waste polyester fibers：
A, installation reaction unit：Four-hole boiling flask is taken for reaction vessel, wherein three mouthfuls dispose thermometer, reflux condensate device and logical nitrogen device respectively；
B, degradation reaction：Take 400 parts of ethylene glycol, 0.3 part of catalyst acetic acid zinc and add four-hole boiling flask mixing, four-hole boiling flask is put into oil bath pan, intensification is heated to zinc acetate and is completely dissolved；Take the cleaning of 150 parts of waste polyester fibers, dry after add reaction unit, open logical nitrogen device and be passed through nitrogen to exclude the oxygen in flask, be to slowly warm up to 185 DEG C of the boiling point of ethylene glycol, reflux condensate device occurs to be incubated after backflow phenomenon to continue to react 2h；Own backflow phenomenon rises and 1mL is sampled per half an hour；
C, sample treatment：No. 94 gasoline and dimethylbenzene for taking isometric ratio are sufficiently mixed and are configured to solvent；After the sample obtained in step b is cooled into room temperature, configured solvent sample dissolution is added；Stop reaction when during samples taken can be dissolved completely in solvent；
(2) preparation of BHET monomers：Step (1) gained mixed solution is cooled to 140 DEG C, is poured into the beaker equipped with distilled water, be heated to 95 DEG C, carry out being filtrated to get filtrate during the transparent shape of solution, filtrate is put into 8h in ice bath, separates out spicule crystal, refilters；Repeat aforesaid operations 3 times, you can obtain BHET monomers；
(3) preparation of polyurethane foam material：Take 100 parts of step (2) gained BHET monomers, 90 parts of foaming agent polyisocyanates PAPI, 2 parts of water, 2 parts of octoate catalyst stannous, 1 part of solubilizer silicone oil is sequentially added in reaction flask, mixing and stirring is to start foamable reaction, reaction is foamed after 1 minute and is finished, and obtains polyurethane foam material crude product；36h curings will be placed under gained polyurethane foam material crude product normal temperature and pressure and obtains product polyurethane foam material.
The fusing point of the polyurethane foam material for obtaining is 153 DEG C, and temperature of initial decomposition is 230 DEG C, compressive strength 680KPa, density 95kgm-3。
Claims (1)
1. a kind of production technology of waste polyester polyurethane foam material, it is characterised in that utilize glycolysis alcoholysis process degradation waste polyester fibers, obtains ethylene glycol terephthalate BHET, then obtains polyurethane foam material by BHET foaming, and step is as follows：Count by weight：
(1) degraded of waste polyester fibers：
A, installation reaction unit：Four-hole boiling flask is taken for reaction vessel, wherein three mouthfuls dispose thermometer, reflux condensate device and logical nitrogen device respectively；
B, degradation reaction：Take 200~400 parts of ethylene glycol, 0.2~0.5 part of catalyst acetic acid zinc and add four-hole boiling flask mixing, four-hole boiling flask is put into oil bath pan, intensification is heated to zinc acetate and is completely dissolved；Take the cleaning of 150 parts of waste polyester fibers, dry after add reaction unit, open logical nitrogen device and be passed through nitrogen to exclude the oxygen in flask, be to slowly warm up to 185 DEG C of the boiling point of ethylene glycol, reflux condensate device occurs to be incubated after backflow phenomenon to continue to react 3~6h；Own backflow phenomenon rises and 1~2mL is sampled per half an hour
；
C, sample treatment：The gasoline and dimethylbenzene for taking isometric ratio are sufficiently mixed and are configured to solvent；After the sample obtained in step b is cooled into room temperature, configured solvent sample dissolution is added；Stop reaction when during samples taken can be dissolved completely in solvent；
(2) preparation of BHET monomers：Step (1) gained mixed solution is cooled to 130~150 DEG C, is poured into the beaker equipped with distilled water, be heated to 90~100 DEG C, carry out being filtrated to get filtrate during the transparent shape of solution, filtrate is put into 8~10h in ice bath, separates out spicule crystal, refilters；Repeat aforesaid operations 3~4 times, you can obtain BHET monomers；
(3) preparation of polyurethane foam material：Take 100 parts of step (2) gained BHET monomers, foaming agent polyisocyanates PAPI90~110 part, 3~5 parts of water, 3~8 parts of octoate catalyst stannous, 2~5 parts of solubilizer silicone oil is sequentially added in reaction flask, mixing and stirring is to start foamable reaction, foamed after anti-1~3 minute and finished, obtain polyurethane foam material crude product；20~40h curings will be placed under gained polyurethane foam material crude product normal temperature and pressure and obtains product polyurethane foam material.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510845911.9A CN106810672A (en) | 2015-11-30 | 2015-11-30 | A kind of production technology of waste polyester polyurethane foam material |
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| CN201510845911.9A CN106810672A (en) | 2015-11-30 | 2015-11-30 | A kind of production technology of waste polyester polyurethane foam material |
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| CN106810672A true CN106810672A (en) | 2017-06-09 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107417492A (en) * | 2017-06-28 | 2017-12-01 | 中国科学院山西煤炭化学研究所 | A kind of method of controlled degradation recovery pet material |
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2015
- 2015-11-30 CN CN201510845911.9A patent/CN106810672A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107417492A (en) * | 2017-06-28 | 2017-12-01 | 中国科学院山西煤炭化学研究所 | A kind of method of controlled degradation recovery pet material |
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Application publication date: 20170609 |