CN103159981A - Method for recycling polyhydric alcohol by degrading thermal-insulation polyurethane foam materials for buildings - Google Patents
Method for recycling polyhydric alcohol by degrading thermal-insulation polyurethane foam materials for buildings Download PDFInfo
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- CN103159981A CN103159981A CN2013100949799A CN201310094979A CN103159981A CN 103159981 A CN103159981 A CN 103159981A CN 2013100949799 A CN2013100949799 A CN 2013100949799A CN 201310094979 A CN201310094979 A CN 201310094979A CN 103159981 A CN103159981 A CN 103159981A
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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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Abstract
The invention relates to a method for recycling polyhydric alcohol by taking waste materials of thermal-insulation polyurethane foam materials for buildings and reproducing polyurethane foams. The method comprises the steps of adding proper amounts of antioxidants, alcoholysis agents, alcoholysis assistant agents and catalysts in presence of oxygen (in atmosphere which is not protected by inert gas), and recycling the thermal-insulation foam materials for the buildings. The hydroxyl value, acid value and the like of the polyhydric alcohol recycled by utilizing the method are all accordant with government standards. The recycled polyhydric alcohol can be used for partially replacing polyether polyol to reproduce the polyurethane foams. Compared with previous inventions, the method has the advantages that (1) in the atmosphere which is not protected by the inert gas, the industrial production process is simple, and the cost is saved; (2) the degraded polyhydric alcohols in the method are solid materials on an upper layer and a lower layer, and the separation is simple; and (3) the recycled polyhydric alcohol can be used for directly replacing the polyether polyol with a mass fraction of 20-50% to reproduce the polyurethane foams, and the foam property is good.
Description
Technical field
The invention belongs to chemical technology field, be specifically related to a kind of degradation technique recovery polyxol method of heat insulating polyurethane foam materials for building and the foaming properties that degrading alcohol replaces the part polyether glycol to foam again.
Background technology
After nineteen thirty-seven Germanization scholar Baeyer has been found the chemical reaction of isocyanic ester and reactive hydrogen, just begun chemistry and the applied research of urethane, experienced more than 60 year, formed flourish polyurethane industrial.The urethane development is at full speed, and after the eighties in 19th century, polyurethane material consumption in national economy is increasing, and purposes is more and more wider, and its waste is also more and more.Polyurethane material can not natural degradation, and these waste materials become increasingly conspicuous to the pollution problem of environment.
The recycling of urethane mainly contains 3 kinds of modes, Physical, chemical method, energy law.The existing many reports of Physical and practical technique, the product properties of the PU gained of recovery is relatively poor, is only applicable to low-grade goods; Energy recovery is by waste material being burned to reclaim heat, and this mode can cause secondary pollution, does not substantially re-use.The chemical recovering method method mainly comprises: chemical recovery method mainly contains alcoholysis method, hydrolysis method, alcoholysis method, ammonolysis process, amine-decomposing method, phosphorus solution, acid hydrolyzation, based on alkaline hydrolysis and enzymolysis process etc.Hydrolysis method, monohydroxy-alcohol solution, ammonolysis process are to carry out under High Temperature High Pressure, thereby very high to reaction conditions and equipment requirements, and the composition of degradation production is complicated, and the purification techniques difficulty is very large, so this method is not promoted; The based on alkaline hydrolysis reaction is to carry out under high temperature highly basic condition, and high to equipment requirements, production cost is high, realizes comparatively difficulty of industrialization; The product that the phosphorus edman degradation Edman obtains has more phosphorus, can increase the flame retardant properties of product as filler, and it is higher that the phosphorus degraded product prepares hard-foam polyurethane density as filler, better mechanical property, but also need further research.And the phosphorus degraded product mainly is used as filler, and the product usage quantity is also very limited, has limited applying of phosphorus edman degradation Edman; Acid hydrolyzation and enzymolysis process also do not have application example, also are in initial conceptual phase; Alcoholysis method is the most widely used method of present chemical recovery urethane, and alcoholysis is to be suitable for a kind of chemical process that hard polyurethane foams reclaims most.Its degraded product can be directly as the raw material of producing PU, the physical property of products obtained therefrom and product innovation basic identical.
Adopt alcoholysis method this kind heat insulating polyurethane foam materials for building dead meal pulverized particles of degrading, output is high.The present invention under the condition of aerobic (inert-free gas protection atmosphere in), directly adds the alcoholysis agent, helps alcoholysis agent, catalyzer and antioxidant this kind lagging material dead meal pulverized particles of degrading on the basis of alcoholysis method.With invention CN1180689A before, CN102516593A compares, and this kind method degradation process can be carried out under the condition of aerobic, the product of its degraded: supernatant liquid is polyvalent alcohol, and lower floor is the solid material, and lock out operation is convenient, and technique is simple, saves cost.
Summary of the invention
The present invention adopts a kind of heat insulating polyurethane foam materials dead meal for building of alcoholysis method degraded; under the condition of aerobic (inert-free gas protection atmosphere in), directly add the alcoholysis agent, help alcoholysis agent, catalyzer and antioxidant this kind lagging material dead meal of degrading.Use the degraded of this kind method to obtain: supernatant liquid is polyvalent alcohol, and lower floor is the solid material, and lock out operation is convenient, and technique is simple, and cost is lower.Produce urethane foam but replace polyether glycol to be used for regeneration with the polyvalent alcohol direct part of degrading out, foaming properties is good.
Technical scheme of the present invention is as follows:
The present invention adopt alcoholysis method degraded should in heat insulating polyurethane foam materials dead meal for building (being ground into approximately 2-8mm of particle diameter).It is characterized in that: degrade under the condition of aerobic, greatly simplify technique, simple to operate, save cost.And the supernatant liquid of degraded product is polyvalent alcohol, and lower floor is the solid material.Lock out operation is simple, and isolated polyvalent alcohol can directly replace the part polyether glycol to be used for regeneration product urethane foam.
The present invention is with alcoholysis method this kind heat insulating polyurethane foam materials for building dead meal of degrading, and regeneration produces polyurethane foam, and its method is as follows:
With the alcoholysis agent, help alcoholysis agent, catalyzer, antioxidant to join in reactor, heat temperature raising, until in reactor, fluid temperature reaches 140-170 ℃, successively add dead meal again in reactor, add repeatedly (preferentially adding 3-10 times), polyurethane foam proportion is little, repeatedly adds, and reaction efficiency is high.The add-on of lagging material dead meal, alcoholysis agent, to help the mass ratio of alcoholysis agent, catalyzer, antioxidant be 100:(50 1): (2.5-12): (0.2-0.5): (0.5-2), heated and stirred heats up, temperature of reaction is controlled at 160-210 ℃, reaction 3-8h, filter out unreacted solid impurity, cooling, the liquid that obtains is namely polyvalent alcohol; Its degradation principles reaction formula is as follows:
Reaction formula 1 monoethanolamine degradable polyurethane principle
Reaction formula 2 diethanolamine degraded Urethylane principles
Reaction formula 3 diethanolamine degraded urea groups urethane principles
Described a kind of heat insulating polyurethane foam materials degraded for building, it is characterized in that alcoholysis agent used is: glycol ether, ethylene glycol, propylene glycol, dipropylene glycol, any one or a few combination in neopentyl glycol, Isosorbide-5-Nitrae one butyleneglycol, hexylene glycol, polyether Glycols, low molecular polyether polyvalent alcohol;
Described a kind of heat insulating polyurethane foam materials for building degraded is characterized in that described to help the alcoholysis agent be Monoethanolamine MEA BASF, diethanolamine, trolamine, N, N-dimethyl propanol amine, N, the one or more combination in the N-dimethylethanolamine;
Described a kind of heat insulating polyurethane foam materials degraded for building is characterized in that described catalyzer is any one or a few combination in potassium acetate, zinc acetate, calcium chloride, aluminum chloride, sodium hydroxide, potassium hydroxide;
Described a kind of heat insulating polyurethane foam materials degraded for building, it is characterized in that described antioxidant is any one or a few combination in 2,6 di tert butyl 4 methyl phenol (BHT), butylhydroxy anisole (BHA), Tenox PG (PG), tertiarybutylhydroquinone (TBHQ).
The employing aforesaid method obtains hydroxyl value 450-590mgKOH/g, acid number is the polyvalent alcohol of 0.5 1 2.0mgKOH/g.
The resulting polyvalent alcohol of method that polyvalent alcohol is reclaimed in described a kind of lagging material degraded for building can directly replace massfraction 20-50% polyether glycol regeneration to produce polyurethane foam.The performance of its foam is as follows: density: 30-40kg/m
3, compressive strength: 200-380kPa, thermal conductivity: 22-30mW/ (m ﹒ K).
The method of polyvalent alcohol is reclaimed in a kind of heat insulating polyurethane foam materials dead meal production for building of the present invention; be incubated with the polyurethane foam dead meal as raw material production recovery polyvalent alcohol in producing; solve the waste disposal problem that produces in producing and protected environment; in alcoholysis process; do not need the protection of rare gas element, greatly simplified the degradation technique process.Reclaiming simultaneously polyvalent alcohol can be used for again producing by the brand-new polyvalent alcohol of Substitute For Partial, has reduced production cost, economizes on resources.The alcoholysis agent used of alcoholysis dead meal pulverized particles, help alcoholysis agent, catalyzer, antioxidant not to affect to reclaim polyvalent alcohol and reuse, the polyvalent alcohol of Separation and Recovery is simple to operate, saves cost; The hydroxyl value of the polyvalent alcohol that reclaims is between 0.5 1 2.0mgKOH/g at 450-590mgKOH/g, acid number, meets the requirement of hard bubbling with polyvalent alcohol.Can directly replace the part polyether glycol to be used for regeneration and produce porous plastics, foaming properties is good.
Embodiment
Below by example, the present invention is described in further detail:
Embodiment 1
The heat insulating polyurethane foam materials dead meal production a kind of for building of the present embodiment is reclaimed method and the regeneration of polyvalent alcohol and is produced foaming, comprises the following steps:
1, glycol ether, Monoethanolamine MEA BASF, calcium chloride, BHT are joined in reactor, heat temperature raising, until in reactor, fluid temperature reaches 170 ℃, successively add dead meal again in reactor, adding indegree is 3 times, the mass ratio of the add-on of lagging material dead meal, glycol ether, Monoethanolamine MEA BASF, calcium chloride, BHT is 100:50:12:0.3:2, heated and stirred heats up, temperature of reaction is controlled at 210 ℃, reaction 3h, filter out unreacted solid impurity, cooling, the liquid that obtains is namely polyvalent alcohol;
Adopting aforesaid method to obtain hydroxyl value is that 508mgKOH/g, acid number are the 1.56gKOH/g polyvalent alcohol.
2, substitute 20% polyether glycol with above-mentioned degraded polyvalent alcohol and be used for regeneration product polyurethane foam, its performance is as follows: density 40kg/m
3, compressive strength 380kPa, thermal conductivity 25mW/ (m ﹒ K).
Embodiment 2
The heat insulating polyurethane foam materials dead meal production a kind of for building of the present embodiment is reclaimed method and the regeneration of polyvalent alcohol and is produced foaming, comprises the following steps:
1, dipropylene glycol, trolamine, zinc acetate, BHA are joined in reactor, heat temperature raising, until in reactor, fluid temperature reaches 140 ℃, successively add dead meal again in reactor, adding indegree is 10 times, the mass ratio of lagging material dead meal add-on, dipropylene glycol, trolamine, zinc acetate, BHA is 100:150:10:0.5:0.5, heated and stirred heats up, temperature of reaction is controlled at 175 ℃, reaction 5h, filter out unreacted solid impurity, cooling, the liquid that obtains is namely polyvalent alcohol;
Adopting aforesaid method to obtain hydroxyl value is that 498mgKOH/g, acid number are the 1.29gKOH/g polyvalent alcohol.
2, substitute 50% polyether glycol with above-mentioned degraded polyvalent alcohol and be used for regeneration product polyurethane foam, its performance is as follows: density 30kg/m
3, compressive strength 200kPa, thermal conductivity 30mW/ (m ﹒ K).
Embodiment 3
The heat insulating polyurethane foam materials dead meal production a kind of for building of the present embodiment is reclaimed method and the regeneration of polyvalent alcohol and is produced foaming, comprises the following steps:
1, propylene glycol, Diethylene Glycol, sodium hydroxide, TBHQ are joined in reactor, heat temperature raising, until in reactor, fluid temperature reaches 150 ℃, successively add dead meal again in reactor, adding indegree is 5 times, the mass ratio of the add-on of lagging material dead meal, propylene glycol, Diethylene Glycol, sodium hydroxide, TBHQ is 100:100:2.5:0.2:1, heated and stirred heats up, temperature of reaction is controlled at 160 ℃, reaction 8h, filter out unreacted solid impurity, cooling, the liquid that obtains is namely polyvalent alcohol;
Adopting aforesaid method to obtain hydroxyl value is that 482mgKOH/g, acid number are the 0.98gKOH/g polyvalent alcohol.
2, substitute 35% polyether glycol with above-mentioned degraded polyvalent alcohol and be used for regeneration product polyurethane foam, its performance is as follows: density 33kg/m
3, compressive strength 250kPa, thermal conductivity 27mW/ (m ﹒ K).
Embodiment 4
The heat insulating polyurethane foam materials dead meal production a kind of for building of the present embodiment is reclaimed method and the regeneration of polyvalent alcohol and is produced foaming, comprises the following steps:
1, with ethylene glycol, N, N-dimethyl propanol amine, aluminum chloride, TBHQ join in reactor, heat temperature raising, until in reactor, fluid temperature reaches 170 ℃, successively add dead meal again in reactor, adding indegree is 4 times, the add-on of lagging material dead meal, ethylene glycol, N, the mass ratio of N-dimethyl propanol amine, aluminum chloride, TBHQ is 100:125:8:0.5:2, and heated and stirred heats up, and temperature of reaction is controlled at 180 ℃, reaction 6h, filter out unreacted solid impurity, cooling, the liquid that obtains is namely polyvalent alcohol;
Adopting aforesaid method to obtain hydroxyl value is that 514mgKOH/g, acid number are the 1.12gKOH/g polyvalent alcohol.
2, substitute 25% polyether glycol with above-mentioned degraded polyvalent alcohol and be used for regeneration product polyurethane foam, its performance is as follows: density 38kg/m
3, compressive strength 340kPa, thermal conductivity 22mW/ (m ﹒ K).
Embodiment 5
The heat insulating polyurethane foam materials dead meal production a kind of for building of the present embodiment is reclaimed method and the regeneration of polyvalent alcohol and is produced foaming, comprises the following steps:
1, with 1,4 one butyleneglycols, N, N-dimethylethanolamine, potassium hydroxide, BHT join in reactor, heat temperature raising, until in reactor, fluid temperature reaches 160 ℃, successively add dead meal again in reactor, adding indegree is 6 times, the add-on of lagging material dead meal, 1,4 one butyleneglycols, N, the mass ratio of N-dimethylethanolamine, potassium hydroxide, BHT is 100:100:8:0.3:0.5, and heated and stirred heats up, and temperature of reaction is controlled at 180 ℃, reaction 8h, filter out unreacted solid impurity, cooling, the liquid that obtains is namely polyvalent alcohol;
Adopting aforesaid method to obtain hydroxyl value is that 480mgKOH/g, acid number are the 0.90gKOH/g polyvalent alcohol.
2, substitute 40% polyether glycol with above-mentioned degraded polyvalent alcohol and be used for regeneration product polyurethane foam, its performance is as follows: density 31kg/m
3, compressive strength 220kPa, thermal conductivity 28mW/ (m ﹒ K).
Embodiment 6
The heat insulating polyurethane foam materials dead meal production a kind of for building of the present embodiment is reclaimed method and the regeneration of polyvalent alcohol and is produced foaming, comprises the following steps:
1, hexylene glycol, Monoethanolamine MEA BASF, zinc acetate, BHT are joined in reactor, heat temperature raising, until in reactor, fluid temperature reaches 140 ℃, successively add dead meal again in reactor, adding indegree is 8 times, the mass ratio of the add-on of lagging material dead meal, hexylene glycol, Monoethanolamine MEA BASF, zinc acetate, BHT is 100:125:8:0.2:2, heated and stirred heats up, temperature of reaction is controlled at 185 ℃, reaction 6h, filter out unreacted solid impurity, cooling, the liquid that obtains is namely polyvalent alcohol;
Adopting aforesaid method to obtain hydroxyl value is that 512mgKOH/g, acid number are the 1.23gKOH/g polyvalent alcohol.
2, substitute 30% polyether glycol with above-mentioned degraded polyvalent alcohol and be used for regeneration product polyurethane foam, its performance is as follows: density 37kg/m
3, compressive strength 320kPa, thermal conductivity 23mW/ (m ﹒ K).
Embodiment 7
The heat insulating polyurethane foam materials dead meal production a kind of for building of the present embodiment is reclaimed method and the regeneration of polyvalent alcohol and is produced foaming, comprises the following steps:
1, neopentyl glycol, diethanolamine, potassium hydroxide, PG are joined in reactor, heat temperature raising, until reactor temperature reaches 165 ℃, successively add dead meal again in reactor, adding indegree is 5 times, the mass ratio of the add-on of lagging material dead meal, neopentyl glycol, diethanolamine, potassium hydroxide, TBHQ is 100:150:12:0.2:0.5, heated and stirred heats up, temperature of reaction is controlled at 170 ℃, reaction 8h, filter out unreacted solid impurity, cooling, the liquid that obtains is namely polyvalent alcohol;
Adopting aforesaid method to obtain hydroxyl value is that 501mgKOH/g, acid number are the 0.89gKOH/g polyvalent alcohol.
2, substitute 45% polyether glycol with above-mentioned degraded polyvalent alcohol and be used for regeneration product polyurethane foam, its performance is as follows: density 31kg/m
3, compressive strength 230kPa, thermal conductivity 29mW/ (m ﹒ K).
Compared with the prior art, excellent part of the present invention is:
1, utilizing building heat preservation is that raw material production reclaims polyvalent alcohol with the polyurethane foamed material dead meal; solved the waste disposal problem that produces in the production process; protected environment; reclaiming simultaneously polyvalent alcohol can be used for again producing by the brand-new polyether glycol of Substitute For Partial; reduced production cost, economized on resources.
2, degradation technique process of the present invention can be carried out (namely not needing the protection atmosphere of rare gas element) and greatly simplified processing condition under the condition of aerobic, saves cost.
3, the product of the present invention's degraded: supernatant liquid is polyvalent alcohol, and lower floor is the solid material, and lock out operation is convenient, and technique is simple, saves cost.
4, alcoholysis foam alcoholysis agent used, help alcoholysis agent, catalyzer, antioxidant not to affect to reclaim polyvalent alcohol and reuse, therefore reclaiming polyvalent alcohol does not need through distillation, separates out the step such as filtration, and it is standing not stratified to reclaim polyvalent alcohol, can directly use.
5, the hydroxyl value of the polyvalent alcohol of the present invention's recovery is between 420-560mgKOH/g, and acid number meeting the requirement of hard bubbling with polyvalent alcohol between 0.90-1.76mgKOH/g.The polyvalent alcohol that degraded obtains can directly replace massfraction 20-50% polyether glycol to be used for regeneration product polyurethane foam.The performance of its foam is as follows: density: 30-40kg/m
3, compressive strength: 200-380kPa, thermal conductivity: 22-30mW/ (m ﹒ K).
The present invention is not limited to the technology described in embodiment; its description is illustrative; and nonrestrictive; authority of the present invention is limited by claim; based on the art personnel according to the technology related to the present invention that the present invention can change, the method such as restructuring obtains, all within protection scope of the present invention.
Claims (7)
1. a heat insulating polyurethane foam materials for building is degraded and is reclaimed the method for polyvalent alcohol; It is characterized in that the alcoholysis agent, help alcoholysis agent, catalyzer, oxidation inhibitor to join in reactor, heat temperature raising is until in reactor, fluid temperature reaches 140-170 ℃; Polyurethane foamed material is ground into particle diameter 2-8mm, then time has added several times the polyurethane foam dead meal in the reactor; Heated and stirred heats up, and temperature of reaction is controlled at 160-210 ℃, and reaction 3-8h filters out unreacted solid impurity, and cooling, the liquid that obtains is namely polyvalent alcohol.
2. the method for claim 1, it is characterized in that polyurethane foam dead meal, alcoholysis agent, helping the mass ratio of alcoholysis agent, catalyzer, antioxidant is 100:(50-150): (2.5-12): (0.2-0.5): (0.5-2).
3. the method for claim 1, is characterized in that described antioxidant is any one or a few combination in 2,6 di tert butyl 4 methyl phenol, butylhydroxy anisole, Tenox PG or tertiarybutylhydroquinone.
4. the method for claim 1, is characterized in that described alcoholysis agent is: glycol ether, ethylene glycol, propylene glycol, dipropylene glycol, any one or a few combination in neopentyl glycol, Isosorbide-5-Nitrae one butyleneglycol, hexylene glycol, polyether Glycols or low molecular polyether polyvalent alcohol.
5. the method for claim 1 is characterized in that described to help the alcoholysis agent be Monoethanolamine MEA BASF, diethanolamine, trolamine, N, N-dimethyl propanol amine, N, the one or more combination in the N-dimethylethanolamine.
6. the method for claim 1, is characterized in that described described catalyzer is any one or a few combination in potassium acetate, zinc acetate, calcium chloride, aluminum chloride, sodium hydroxide or potassium hydroxide.
7. lagging material degraded recovery polyvalent alcohol for building directly replaces massfraction 20-50% polyether glycol regeneration to produce polyurethane foam.
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| CN103849135A (en) * | 2014-03-04 | 2014-06-11 | 北华大学 | Preparation method of degradable polyurethane foaming plastic |
| CN104479094A (en) * | 2014-10-19 | 2015-04-01 | 浙江华江科技发展有限公司 | Polyurethane foam produced from regenerated polyether polyol and used for automobile roofs, and preparing method thereof |
| CN104672414A (en) * | 2014-11-27 | 2015-06-03 | 上海鹤城高分子科技有限公司 | Method of preparing polyurethane thermal insulation material by recovering waste polyurethane elastomer |
| CN104788716A (en) * | 2015-04-08 | 2015-07-22 | 景富新材料(唐山)有限公司 | Composite degradation method of PU (polyurethane) solid waste |
| CN105001390A (en) * | 2015-07-29 | 2015-10-28 | 龙江神华节能墙材有限公司 | Method for preparing all-water polyurethane rigid foam |
| CN105330891A (en) * | 2015-10-22 | 2016-02-17 | 烟台正海合泰科技股份有限公司 | Recovery reutilization method for polyurethane foam waste material |
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| CN103849135A (en) * | 2014-03-04 | 2014-06-11 | 北华大学 | Preparation method of degradable polyurethane foaming plastic |
| CN104479094A (en) * | 2014-10-19 | 2015-04-01 | 浙江华江科技发展有限公司 | Polyurethane foam produced from regenerated polyether polyol and used for automobile roofs, and preparing method thereof |
| CN104672414B (en) * | 2014-11-27 | 2017-10-10 | 上海鹤城高分子科技有限公司 | A kind of method that waste polyurethane elastomer recovery prepares polyurethane heat insulation material |
| CN104672414A (en) * | 2014-11-27 | 2015-06-03 | 上海鹤城高分子科技有限公司 | Method of preparing polyurethane thermal insulation material by recovering waste polyurethane elastomer |
| CN104788716A (en) * | 2015-04-08 | 2015-07-22 | 景富新材料(唐山)有限公司 | Composite degradation method of PU (polyurethane) solid waste |
| CN105001390A (en) * | 2015-07-29 | 2015-10-28 | 龙江神华节能墙材有限公司 | Method for preparing all-water polyurethane rigid foam |
| CN105330891A (en) * | 2015-10-22 | 2016-02-17 | 烟台正海合泰科技股份有限公司 | Recovery reutilization method for polyurethane foam waste material |
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Application publication date: 20130619 |