CN110093026A - A kind of recycling technique of polyurethane - Google Patents
A kind of recycling technique of polyurethane Download PDFInfo
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- CN110093026A CN110093026A CN201910373470.5A CN201910373470A CN110093026A CN 110093026 A CN110093026 A CN 110093026A CN 201910373470 A CN201910373470 A CN 201910373470A CN 110093026 A CN110093026 A CN 110093026A
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- 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
- C08G18/40—High-molecular-weight compounds
- C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
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- 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
- C08G18/75—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic
- C08G18/751—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring
- C08G18/752—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group
- C08G18/753—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group
- C08G18/755—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group and at least one isocyanate or isothiocyanate group linked to a secondary carbon atom of the cycloaliphatic ring, e.g. isophorone diisocyanate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L75/00—Compositions of polyureas or polyurethanes; Compositions of derivatives of such polymers
- C08L75/04—Polyurethanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)
Abstract
The invention discloses a kind of recycling technique of polyurethane, include the following steps: that the pretreatment of (1) reclaimed materials, (2) montmorillonite processing, (3) raw material weighs, prepared by (4) premix, the preparation of (5) finished product.The present invention provides a kind of recycling techniques of polyurethane; the utilization rate of substance is improved well; improve the protection to natural environment, the performances such as polyurethane material obtained is wear-resisting, intensity, temperature tolerance, elasticity are obviously improved, great application value and the market competitiveness.
Description
Technical field
The invention belongs to polyurethane utilization technology fields, and in particular to a kind of recycling technique of polyurethane.
Background technique
Polyurethane with its excellent physical property, good processable type, excellent resistant to chemical media and ageing-resistant performance,
Have become one of widest high molecular material of current application field, and its yield and the range of application constantly expand
Among big.But it along with the extension of production-scale expansion and application field, is generated in polyurethane production and use process
A large amount of wastes, including for heat-insulated and Sofa cushion a large amount of polyurethane foams, waste polyurethane sole, waste and old poly- ammonia
Ester leather etc..If only these waste materials are handled by the method for filling and burning, not only land occupation, but also pollution environment,
It is simultaneously also a kind of waste to resource.Therefore, the recycling problem of polyurethane has been that there is an urgent need to solve for polyurethane industrial
One of significant problem certainly carries out recycling and reusing to waste polyurethane, reduces environmental pollution, while reducing the production of new product
Cost has economical and environmentally friendly meaning.
Have in the prior art by waste polyurethane be used for shoes industry manufacture scheme, it is seen that its be used for sole, upper of a shoe, sock,
The production of vamp etc. can effectively reduce manufacturing cost.Application No. is: CN201410677754.0 discloses a kind of using useless
Old polyurethane shoe-sole regenerative polyurethane composite material and its preparation process, re-use waste polyurethane sole,
The utilization rate of material is improved, material obtained has the qualities such as good intensity.But the mechanics product of material made from this mode
Matter is still poor, still needs to further be promoted to the recycling effect of waste polyurethane sole.
Summary of the invention
The purpose of the present invention is being directed to existing problem, a kind of recycling technique of polyurethane is provided.
The present invention is achieved by the following technical solutions:
A kind of recycling technique of polyurethane, includes the following steps:
(1) reclaimed materials pre-processes: by the polyurethane of recycling successively by once washing, oil removing, after secondary washing process, then put into
It is dried 1 ~ 2h in drying box, finally puts it into again and carries out break process in crusher, control broken particle
Partial size be 200 ~ 300 mesh, take out polyurethane reclaimed materials is spare；
(2) montmorillonite is handled: progress high-temperature calcination processing in calcining furnace first is put into montmorillonite, is taken out after 1 ~ 1.5h, then
10 ~ 15min of immersion treatment in acid solution is put it into, is subsequently filtered out and is rinsed with deionized water to neutrality, finally put it into
Laser irradiation treatment is carried out in laser treatment instrument, take out after the completion modified montmorillonoid is spare；
(3) raw material weighs: following raw materials according is weighed by corresponding parts by weight: polyurethane reclaimed materials made from 190 ~ 200 parts of steps (1),
Modified montmorillonoid made from 10 ~ 13 parts of steps (2), 8 ~ 12 parts of compatilizers, 6 ~ 9 parts of isophorone diisocyanate, 4 ~ 7 parts of polyester
Polyalcohol, 3 ~ 6 parts of zinc stearates, 1 ~ 3 part of antioxidant, 3 ~ 5 parts of alkylolamides, 1 ~ 2 part of epoxidized soybean oil, 0.5 ~ 1.5 part it is micro-
Spar wax, 5 ~ 8 parts of dibutyl tin dilaurates, 1 ~ 1.5 part of bismuth neodecanoate, 0.4 ~ 0.7 part of vaseline, 2 ~ 5 parts of calcium carbonate；
(4) prepared by premix: modified montmorillonoid, zinc stearate, antioxidant, alkyl made from the step of step (3) is weighed (2)
Alkylolamides, epoxidized soybean oil, microcrystalline wax, dibutyl tin dilaurate, vaseline, calcium carbonate mix jointly and put into high-speed stirring
Mix in machine and be stirred, taken out after 1 ~ 1.5h premix is spare；
(5) prepared by finished product: the recycling of polyurethane made from the step of premix made from step (4) and step (3) are weighed (1)
Material, compatilizer, isophorone diisocyanate, polyester polyol, bismuth neodecanoate are put into extruder melt jointly and be squeezed
It handles, takes out after naturally cooling to room temperature after the completion out.
Further, it is 40 ~ 45 DEG C clear that primary washing as described in step (1), secondary washing process, which are with temperature,
Water is rinsed processing；The oil removal treatment is to carry out immersion oil removal treatment with commercially available degreaser.
Further, it is 85 ~ 90 DEG C that the temperature in drying box is controlled when drying process as described in step (1).
Further, temperature when high-temperature calcination described in step (2) is handled in control calcining furnace is 750 ~ 800 DEG C；
The acid solution is the hydrochloric acid solution that mass fraction is 0.3 ~ 0.5%.
Further, laser irradiation treatment described in step (2) be specifically control laser treatment instrument in carry out argon from
Sub- laser irradiation treatment, the wavelength for controlling laser is 500 ~ 520nm, the power density of laser is 60 ~ 65W/mm2, laser facula
Diameter is 1.8 ~ 2.0mm, and the scanning speed for controlling laser is 3 ~ 4cm/s, and the mode of scanning is progressive scan.In argon laser
It is when radiation treatment, montmorillonite is evenly laid out on processing table top, the thickness of tiling is controlled no more than 4mm, then controls laser
Radiation treatment is carried out by the way of the progressive scan of S type, completes the modification to montmorillonite；Existing spot diameter is smaller, disadvantage
End is that the time of processing is slightly long, and the amount of processing is little, condition or the more advanced intensity that processing can be improved of technology, increases hot spot
Diameter, with promoted processing efficiency；
Further, antioxidant described in step (3) is antioxidant 1010, any one in irgasfos 168.
Further, the granular size of calcium carbonate described in step (3) is 600 ~ 800 mesh.
Further, when stir process described in step (4) control high-speed mixer in speed of agitator be 2500 ~
2800 revs/min.
Further, the temperature in an area is 155 ~ 160 in control extruder when melting extrusion described in step (5) is handled
DEG C, the temperature in 2nd area be 170 ~ 175 DEG C, the temperature that the temperature in 3rd area is 185 ~ 190 DEG C, the temperature in 4th area is 200 ~ 215 DEG C, head
Degree is 220 ~ 225 DEG C.
It is decreased obviously when polyurethane reclaimed materials recycles because the reasons such as internal structure recombination will cause mechanical quality, other property
The problems such as capable of obviously weakening, there are a certain distance compared with polyurethane new material.This those skilled in the art has been carried out respectively
The enhancing processing operation of kind of various kinds, it is common such as to add reinforcing agent, compatilizer, filler, wherein the addition of filler be it is a kind of not
Wrong processing mode, it is from a wealth of sources on the one hand because filler is cheap, be on the other hand it is easy to use, have good
Treatment effect, as application No. is a kind of multiple using waste polyurethane sole regenerative polyurethane disclosed in CN201410677754.0
The ingredients such as medical stone powder, nano montmorillonite, calcium carbonate have just been used in condensation material and its preparation process, have been made with certain enhancing
With effect, but it does not carry out specially treated to such components, is easy to appear that dispersion is uneven, is easy polymerization when filling and using
The problems such as reunion, although the auxiliary agents such as compatilizer can improve to a certain degree, the effect played is relatively limited, to this this field skill
Art personnel often carry out specific aim processing with coupling agent isoreactivity ingredient, and effect has good promotion, but as people are for material
Expect the continuous improvement of performance requirement, such method also produces technical bottleneck.Therefore the application has carried out further improvement processing,
Special modification is especially carried out to montmorillonite, wherein first carried out calcination processing, its loose internal structure is promoted
Then specific surface area uses acid soak, eliminates magazine ingredient, improve surface-active, finally use ar ion laser illumination
It is handled, by the effect of laser, so that the interlayer spacing of montmorillonite increases, and to being filled with a large amount of argon inside montmorillonite
Ion improves its whole activity, improves dispersion performance, and polyurethane macromolecular is inserted into montmorillonite layer structure
Between, by itself electronegativity group and the montmorillonite modified by argon ion, further strong combination is fixed, it will be apparent that
Whole wear-resisting, intensity, temperature tolerance, elasticity etc. are improved, and then realizes the enhancing processing of reclaimed materials.
The present invention has the advantage that compared with prior art
The present invention provides a kind of recycling techniques of polyurethane, improve the utilization rate of substance well, improve to certainly
The protection of right environment, the performances such as polyurethane material obtained is wear-resisting, intensity, temperature tolerance, elasticity are obviously improved, great popularization
Application value and the market competitiveness.
Specific embodiment
Embodiment 1
A kind of recycling technique of polyurethane, includes the following steps:
(1) reclaimed materials pre-processes: by the polyurethane of recycling successively by once washing, oil removing, after secondary washing process, then put into
It is dried 1h in drying box, finally puts it into again and carries out break process in crusher, control broken particle
Diameter be 200 mesh, take out polyurethane reclaimed materials is spare；
(2) montmorillonite is handled: progress high-temperature calcination processing in calcining furnace first is put into montmorillonite, is taken out after 1h, then by it
It is put into immersion treatment 10min in acid solution, is subsequently filtered out and is rinsed with deionized water to neutrality, finally put it into laser treatment
Laser irradiation treatment is carried out in instrument, take out after the completion modified montmorillonoid is spare；
(3) raw material weighs: weighing following raw materials according: polyurethane reclaimed materials, 10 parts made from 190 parts of steps (1) by corresponding parts by weight
Modified montmorillonoid made from step (2), 8 parts of compatilizers, 6 parts of isophorone diisocyanate, 4 parts of polyester polyol, 3 parts of tristearin
Sour zinc, 1 part of antioxidant, 3 parts of alkylolamides, 1 part of epoxidized soybean oil, 0.5 part of microcrystalline wax, 5 parts of dibutyl tin dilaurates,
1 part of bismuth neodecanoate, 0.4 part of vaseline, 2 parts of calcium carbonate；
(4) prepared by premix: modified montmorillonoid, zinc stearate, antioxidant, alkyl made from the step of step (3) is weighed (2)
Alkylolamides, epoxidized soybean oil, microcrystalline wax, dibutyl tin dilaurate, vaseline, calcium carbonate mix jointly and put into high-speed stirring
Mix in machine and be stirred, taken out after 1h premix is spare；
(5) prepared by finished product: the recycling of polyurethane made from the step of premix made from step (4) and step (3) are weighed (1)
Material, compatilizer, isophorone diisocyanate, polyester polyol, bismuth neodecanoate are put into extruder melt jointly and be squeezed
It handles, takes out after naturally cooling to room temperature after the completion out.
Further, it is as described in step (1) it is primary washing, secondary washing process be with temperature be 40 DEG C clear water into
Row flushing processing；The oil removal treatment is to carry out immersion oil removal treatment with commercially available degreaser.
Further, it is 85 DEG C that the temperature in drying box is controlled when drying process as described in step (1).
Further, temperature when high-temperature calcination described in step (2) is handled in control calcining furnace is 750 DEG C；It is described
Acid solution be mass fraction be 0.3% hydrochloric acid solution.
Further, laser irradiation treatment described in step (2) be specifically control laser treatment instrument in carry out argon from
Sub- laser irradiation treatment, the wavelength for controlling laser is 500nm, the power density of laser is 60W/mm2, laser spot diameter be
1.8 ~ 2.0mm, the scanning speed for controlling laser is 3cm/s, and the mode of scanning is progressive scan.
Further, antioxidant described in step (3) is antioxidant 1010.
Further, the granular size of calcium carbonate described in step (3) is 600 mesh.
Further, when stir process described in step (4) control high-speed mixer in speed of agitator be 2500 turns/
Minute.
Further, melting extrusion described in step (5) handle when control extruder in an area temperature be 155 DEG C,
The temperature in 2nd area is 170 DEG C, the temperature in 3rd area is 185 DEG C, the temperature in 4th area is 200 DEG C, the temperature of head is 220 DEG C.
Embodiment 2
A kind of recycling technique of polyurethane, includes the following steps:
(1) reclaimed materials pre-processes: by the polyurethane of recycling successively by once washing, oil removing, after secondary washing process, then put into
It is dried 1.5h in drying box, finally puts it into again and carries out break process in crusher, control broken particle
Partial size be 250 mesh, take out polyurethane reclaimed materials is spare；
(2) montmorillonite is handled: progress high-temperature calcination processing in calcining furnace first is put into montmorillonite, is taken out after 1.3h, then will
It is put into immersion treatment 12min in acid solution, is subsequently filtered out and is rinsed with deionized water to neutrality, is finally put it at laser
Manage instrument in carry out laser irradiation treatment, take out after the completion modified montmorillonoid is spare；
(3) raw material weighs: weighing following raw materials according: polyurethane reclaimed materials, 12 parts made from 195 parts of steps (1) by corresponding parts by weight
Modified montmorillonoid made from step (2), 10 parts of compatilizers, 8 parts of isophorone diisocyanate, 6 parts of polyester polyol, 5 parts it is hard
Resin acid zinc, 2 parts of antioxidant, 4 parts of alkylolamides, 1.5 parts of epoxidized soybean oils, 1 part of microcrystalline wax, 7 parts of di lauric dibutyls
Tin, 1.3 parts of bismuth neodecanoates, 0.6 part of vaseline, 4 parts of calcium carbonate；
(4) prepared by premix: modified montmorillonoid, zinc stearate, antioxidant, alkyl made from the step of step (3) is weighed (2)
Alkylolamides, epoxidized soybean oil, microcrystalline wax, dibutyl tin dilaurate, vaseline, calcium carbonate mix jointly and put into high-speed stirring
Mix in machine and be stirred, taken out after 1.2h premix is spare；
(5) prepared by finished product: the recycling of polyurethane made from the step of premix made from step (4) and step (3) are weighed (1)
Material, compatilizer, isophorone diisocyanate, polyester polyol, bismuth neodecanoate are put into extruder melt jointly and be squeezed
It handles, takes out after naturally cooling to room temperature after the completion out.
Further, it is as described in step (1) it is primary washing, secondary washing process be with temperature be 43 DEG C clear water into
Row flushing processing；The oil removal treatment is to carry out immersion oil removal treatment with commercially available degreaser.
Further, it is 88 DEG C that the temperature in drying box is controlled when drying process as described in step (1).
Further, temperature when high-temperature calcination described in step (2) is handled in control calcining furnace is 770 DEG C；It is described
Acid solution be mass fraction be 0.4% hydrochloric acid solution.
Further, laser irradiation treatment described in step (2) be specifically control laser treatment instrument in carry out argon from
Sub- laser irradiation treatment, the wavelength for controlling laser is 510nm, the power density of laser is 63W/mm2, laser spot diameter be
1.8 ~ 2.0mm, the scanning speed for controlling laser is 3cm/s, and the mode of scanning is progressive scan.
Further, antioxidant described in step (3) is antioxidant 1010.
Further, the granular size of calcium carbonate described in step (3) is 700 mesh.
Further, when stir process described in step (4) control high-speed mixer in speed of agitator be 2700 turns/
Minute.
Further, melting extrusion described in step (5) handle when control extruder in an area temperature be 158 DEG C,
The temperature in 2nd area is 172 DEG C, the temperature in 3rd area is 189 DEG C, the temperature in 4th area is 213 DEG C, the temperature of head is 224 DEG C.
Embodiment 3
A kind of recycling technique of polyurethane, includes the following steps:
(1) reclaimed materials pre-processes: by the polyurethane of recycling successively by once washing, oil removing, after secondary washing process, then put into
It is dried 2h in drying box, finally puts it into again and carries out break process in crusher, control broken particle
Diameter be 300 mesh, take out polyurethane reclaimed materials is spare；
(2) montmorillonite is handled: progress high-temperature calcination processing in calcining furnace first is put into montmorillonite, is taken out after 1.5h, then will
It is put into immersion treatment 15min in acid solution, is subsequently filtered out and is rinsed with deionized water to neutrality, is finally put it at laser
Manage instrument in carry out laser irradiation treatment, take out after the completion modified montmorillonoid is spare；
(3) raw material weighs: weighing following raw materials according: polyurethane reclaimed materials, 13 parts made from 200 parts of steps (1) by corresponding parts by weight
Modified montmorillonoid made from step (2), 12 parts of compatilizers, 9 parts of isophorone diisocyanate, 7 parts of polyester polyol, 6 parts it is hard
Resin acid zinc, 3 parts of antioxidant, 5 parts of alkylolamides, 2 parts of epoxidized soybean oils, 1.5 parts of microcrystalline waxes, 8 parts of di lauric dibutyls
Tin, 1.5 parts of bismuth neodecanoates, 0.7 part of vaseline, 5 parts of calcium carbonate；
(4) prepared by premix: modified montmorillonoid, zinc stearate, antioxidant, alkyl made from the step of step (3) is weighed (2)
Alkylolamides, epoxidized soybean oil, microcrystalline wax, dibutyl tin dilaurate, vaseline, calcium carbonate mix jointly and put into high-speed stirring
Mix in machine and be stirred, taken out after 1.5h premix is spare；
(5) prepared by finished product: the recycling of polyurethane made from the step of premix made from step (4) and step (3) are weighed (1)
Material, compatilizer, isophorone diisocyanate, polyester polyol, bismuth neodecanoate are put into extruder melt jointly and be squeezed
It handles, takes out after naturally cooling to room temperature after the completion out.
Further, it is as described in step (1) it is primary washing, secondary washing process be with temperature be 45 DEG C clear water into
Row flushing processing；The oil removal treatment is to carry out immersion oil removal treatment with commercially available degreaser.
Further, it is 90 DEG C that the temperature in drying box is controlled when drying process as described in step (1).
Further, temperature when high-temperature calcination described in step (2) is handled in control calcining furnace is 800 DEG C；It is described
Acid solution be mass fraction be 0.5% hydrochloric acid solution.
Further, laser irradiation treatment described in step (2) be specifically control laser treatment instrument in carry out argon from
Sub- laser irradiation treatment, the wavelength for controlling laser is 520nm, the power density of laser is 65W/mm2, laser spot diameter be
1.8 ~ 2.0mm, the scanning speed for controlling laser is 4cm/s, and the mode of scanning is progressive scan.
Further, antioxidant described in step (3) is irgasfos 168.
Further, the granular size of calcium carbonate described in step (3) is 800 mesh.
Further, when stir process described in step (4) control high-speed mixer in speed of agitator be 2800 turns/
Minute.
Further, melting extrusion described in step (5) handle when control extruder in an area temperature be 160 DEG C,
The temperature in 2nd area is 175 DEG C, the temperature in 3rd area is 190 DEG C, the temperature in 4th area is 215 DEG C, the temperature of head is 225 DEG C.
Control experiment example 1
A kind of recycling technique of polyurethane, includes the following steps:
(1) reclaimed materials pre-processes: by the polyurethane of recycling successively by once washing, oil removing, after secondary washing process, then put into
It is dried 1.5h in drying box, finally puts it into again and carries out break process in crusher, control broken particle
Partial size be 250 mesh, take out polyurethane reclaimed materials is spare；
(2) montmorillonite is handled: progress high-temperature calcination processing in calcining furnace first is put into montmorillonite, is taken out after 1.3h, then will
It is put into immersion treatment 12min in acid solution, is subsequently filtered out and is rinsed with deionized water to neutrality, takes out to be modified illiteracy after the completion de-
Soil is spare；
(3) raw material weighs: weighing following raw materials according: polyurethane reclaimed materials, 12 parts made from 195 parts of steps (1) by corresponding parts by weight
Modified montmorillonoid made from step (2), 10 parts of compatilizers, 8 parts of isophorone diisocyanate, 6 parts of polyester polyol, 5 parts it is hard
Resin acid zinc, 2 parts of antioxidant, 4 parts of alkylolamides, 1.5 parts of epoxidized soybean oils, 1 part of microcrystalline wax, 7 parts of di lauric dibutyls
Tin, 1.3 parts of bismuth neodecanoates, 0.6 part of vaseline, 4 parts of calcium carbonate；
(4) prepared by premix: modified montmorillonoid, zinc stearate, antioxidant, alkyl made from the step of step (3) is weighed (2)
Alkylolamides, epoxidized soybean oil, microcrystalline wax, dibutyl tin dilaurate, vaseline, calcium carbonate mix jointly and put into high-speed stirring
Mix in machine and be stirred, taken out after 1.2h premix is spare；
(5) prepared by finished product: the recycling of polyurethane made from the step of premix made from step (4) and step (3) are weighed (1)
Material, compatilizer, isophorone diisocyanate, polyester polyol, bismuth neodecanoate are put into extruder melt jointly and be squeezed
It handles, takes out after naturally cooling to room temperature after the completion out.
This control experiment example 1 compared with Example 2, be omitted actually step (2) montmorillonite processing in laser irradiation
Processing operation, method and step in addition to this is identical, and the effect of laser irradiation treatment operation is verified with this.
Control experiment example 2
A kind of recycling technique of polyurethane, includes the following steps:
(1) reclaimed materials pre-processes: by the polyurethane of recycling successively by once washing, oil removing, after secondary washing process, then put into
It is dried 1.5h in drying box, finally puts it into again and carries out break process in crusher, control broken particle
Partial size be 250 mesh, take out polyurethane reclaimed materials is spare；
(2) raw material weighs: weighing following raw materials according: polyurethane reclaimed materials, 12 parts made from 195 parts of steps (1) by corresponding parts by weight
Commercially available common montmorillonite, 10 parts of compatilizers, 8 parts of isophorone diisocyanate, 6 parts of polyester polyol, 5 parts of zinc stearates, 2
Part antioxidant, 4 parts of alkylolamides, 1.5 parts of epoxidized soybean oils, 1 part of microcrystalline wax, 7 parts of dibutyl tin dilaurates, 1.3 parts
Bismuth neodecanoate, 0.6 part of vaseline, 4 parts of calcium carbonate；
(3) premix prepare: by the weighed commercially available common montmorillonite of step (2), zinc stearate, antioxidant, alkylolamides,
Epoxidized soybean oil, microcrystalline wax, dibutyl tin dilaurate, vaseline, calcium carbonate are mixed jointly and are put into high-speed mixer
Be stirred, taken out after 1.2h premix is spare；
(4) prepared by finished product: the recycling of polyurethane made from the step of premix made from step (3) and step (2) are weighed (1)
Material, compatilizer, isophorone diisocyanate, polyester polyol, bismuth neodecanoate are put into extruder melt jointly and be squeezed
It handles, takes out after naturally cooling to room temperature after the completion out.
This control experiment example 2 is obtained with commercially available common montmorillonite step of replacing (2) actually compared with Example 2
Modified montmorillonoid ingredient, method and step in addition to this is identical, verifies modified montmorillonoid produced by the present invention with this
Add using effect.
Control experiment example 3
Application No. is: disclosed in CN201410677754.0 it is a kind of using waste polyurethane sole regenerative polyurethane composite material and
Its preparation process specifically selects 2 scheme of embodiment therein.
Performance inspection is carried out to material made from above-described embodiment 2, control experiment example 1, control experiment example 2, control experiment example 3
It surveys, specific correlation data is as shown in table 1 below:
Table 1
Present invention process method can be obviously improved the comprehensive performance of polyurethane recycling product material it can be seen from upper table 1,
Its intensity quality is significantly improved, its service life, great economic benefit and the market competitiveness are extended.
Claims (9)
1. a kind of recycling technique of polyurethane, which comprises the steps of:
(1) reclaimed materials pre-processes: by the polyurethane of recycling successively by once washing, oil removing, after secondary washing process, then put into
It is dried 1 ~ 2h in drying box, finally puts it into again and carries out break process in crusher, control broken particle
Partial size be 200 ~ 300 mesh, take out polyurethane reclaimed materials is spare；
(2) montmorillonite is handled: progress high-temperature calcination processing in calcining furnace first is put into montmorillonite, is taken out after 1 ~ 1.5h, then
10 ~ 15min of immersion treatment in acid solution is put it into, is subsequently filtered out and is rinsed with deionized water to neutrality, finally put it into
Laser irradiation treatment is carried out in laser treatment instrument, take out after the completion modified montmorillonoid is spare；
(3) raw material weighs: following raw materials according is weighed by corresponding parts by weight: polyurethane reclaimed materials made from 190 ~ 200 parts of steps (1),
Modified montmorillonoid made from 10 ~ 13 parts of steps (2), 8 ~ 12 parts of compatilizers, 6 ~ 9 parts of isophorone diisocyanate, 4 ~ 7 parts of polyester
Polyalcohol, 3 ~ 6 parts of zinc stearates, 1 ~ 3 part of antioxidant, 3 ~ 5 parts of alkylolamides, 1 ~ 2 part of epoxidized soybean oil, 0.5 ~ 1.5 part it is micro-
Spar wax, 5 ~ 8 parts of dibutyl tin dilaurates, 1 ~ 1.5 part of bismuth neodecanoate, 0.4 ~ 0.7 part of vaseline, 2 ~ 5 parts of calcium carbonate；
(4) prepared by premix: modified montmorillonoid, zinc stearate, antioxidant, alkyl made from the step of step (3) is weighed (2)
Alkylolamides, epoxidized soybean oil, microcrystalline wax, dibutyl tin dilaurate, vaseline, calcium carbonate mix jointly and put into high-speed stirring
Mix in machine and be stirred, taken out after 1 ~ 1.5h premix is spare；
(5) prepared by finished product: the recycling of polyurethane made from the step of premix made from step (4) and step (3) are weighed (1)
Material, compatilizer, isophorone diisocyanate, polyester polyol, bismuth neodecanoate are put into extruder melt jointly and be squeezed
It handles, takes out after naturally cooling to room temperature after the completion out.
2. a kind of recycling technique of polyurethane according to claim 1, which is characterized in that as described in step (1)
Primary washing, secondary washing process are that the clear water for being 40 ~ 45 DEG C with temperature is rinsed processing；The oil removal treatment is to use
Commercially available degreaser carries out immersion oil removal treatment.
3. a kind of recycling technique of polyurethane according to claim 1, which is characterized in that as described in step (1)
It is 85 ~ 90 DEG C that the temperature in drying box is controlled when drying process.
4. a kind of recycling technique of polyurethane according to claim 1, which is characterized in that described in step (2)
Temperature when high-temperature calcination is handled in control calcining furnace is 750 ~ 800 DEG C；The acid solution is that mass fraction is 0.3 ~ 0.5%
Hydrochloric acid solution.
5. a kind of recycling technique of polyurethane according to claim 1, which is characterized in that described in step (2)
Laser irradiation treatment is specifically to control to carry out ar ion laser illumination processing in laser treatment instrument, and the wavelength for controlling laser is
500 ~ 520nm, laser power density be 60 ~ 65W/mm2, laser spot diameter be 1.8 ~ 2.0mm, control laser scanning speed
Degree is 3 ~ 4cm/s, and the mode of scanning is progressive scan.
6. a kind of recycling technique of polyurethane according to claim 1, which is characterized in that described in step (3)
Antioxidant is antioxidant 1010, any one in irgasfos 168.
7. a kind of recycling technique of polyurethane according to claim 1, which is characterized in that described in step (3)
The granular size of calcium carbonate is 600 ~ 800 mesh.
8. a kind of recycling technique of polyurethane according to claim 1, which is characterized in that described in step (4)
It is 2500 ~ 2800 revs/min that the speed of agitator in high-speed mixer is controlled when stir process.
9. a kind of recycling technique of polyurethane according to claim 1, which is characterized in that described in step (5)
The temperature in an area is 155 ~ 160 DEG C in control extruder when melting extrusion is handled, the temperature in 2nd area is 170 ~ 175 DEG C, 3rd area
Temperature is 185 ~ 190 DEG C, the temperature in 4th area is 200 ~ 215 DEG C, the temperature of head is 220 ~ 225 DEG C.
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