CN105017581A - Method for preparing modified waste rigid polyurethane foaming plastic active micro-powder reinforcing rubber material - Google Patents
Method for preparing modified waste rigid polyurethane foaming plastic active micro-powder reinforcing rubber material Download PDFInfo
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- CN105017581A CN105017581A CN201510510432.1A CN201510510432A CN105017581A CN 105017581 A CN105017581 A CN 105017581A CN 201510510432 A CN201510510432 A CN 201510510432A CN 105017581 A CN105017581 A CN 105017581A
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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
Abstract
The invention relates to a method for preparing a modified waste rigid polyurethane foaming plastic (WRPUF) active micro-powder reinforcing rubber material. The method comprises the steps of removing impurities in WRPUF, and conducting coarse crushing at the normal temperature; making the WRPUF to be subjected to solid state mechanical-chemical reaction at the normal temperature, pulverizing the WRPUF into WRPUF active micro-powder; adding a de-crosslinking agent, conducting thermal-mechanical de-crosslinking chemical modification on the surface of the WRPUF active micro-powder, and obtaining the WRPUF active micro-powder with the surface modified; applying the WRPUF active micro-powder with the surface modified to reinforcing rubber, and with the help of other rubber auxiliary agents and through the plastification, mixing and vulcanization processes, obtaining the rubber material which is reinforced by the WRPUF active micro-powder with the surface modified. The method has the advantages that the solid state mechanical-chemical reaction and the thermal-mechanical de-crosslinking chemical modification method are adopted for recycling the WRPUF, advantages of the physical recycling method and advantages of the chemical recycling method are integrated, the process is simple and practicable, the operation is convenient, no secondary pollution is caused, the material can be used as reinforcing filler of rubber materials, the reinforcing effect is good, the recycling rate is high, and the WRPUF recycling high in additional value is achieved.
Description
Technical field
The present invention relates to a kind of preparation method of modified abandoned rigid urethane foam activate micro powder Reinforced Rubber material.
Background technology
Rigid urethane foam (RPUF) has the premium propertiess such as hard toughness, wear resistance, heat insulating ability, solvent resistance and ageing resistance, makes it be widely used in the field such as refrigerating equipment, automobile, train, roof, the hollow brick that hard bubbles, hard polyurethane foam concrete, basin pipe insulation, packaging, office appliance.But along with a large amount of uses of the mankind, the waste of rigid urethane foam is also got more and more, thus extremely serious pollution is caused to the living environment of the mankind.The source of waste hard polyurethane foam plastic (WRPUF) mainly contains two aspects, and one is producing and preparing the waste product and scrap stock that produce in rigid urethane foam goods process; Two is use for many years the aging various rigid urethane foams scrapped afterwards.
Waste hard polyurethane foam plastic belongs to cross-linked polymer, and its recycling difficulty is very large.The mode of traditional process WRPUF is landfill or burning.Urethane is difficult to be degraded by microorganisms, so landfill method can not solve root problem.And a large amount of dense smoke and very pungent smell in burning process, can be produced, severe contamination is produced to atmospheric environment.So a large amount of rigid urethane foams, if correctly effectively do not recycled, is not only the waste of resource, threat that more can be huge to environment structure.
Along with improving constantly of people's environmental consciousness, particularly in today of Sustainable development, realize the Appropriate application of resource, referred important strategic height.Rigid urethane foam is as a kind of important material, and its reasonable recycling will have great economic benefit and social benefit.Therefore world today's problem the most in the urgent need to address has been become to the recovery of WRPUF and process.
The achievement in research that relevant WRPUF recycles is more, and the recovery and treatment method related in correlative theses and patent mainly contains physiochemical mutagens method, chemical recycling, biological degradation absorption method and energy recovery method.For the recycling of WRPUF, from the economic angle of antenatal input, be good with physiochemical mutagens method.But the product properties obtained by reworked material declines, and uses mainly as low-grade articles for use.And chemical recycling, biological degradation absorption method and energy recovery method are due to the restriction by technology or Cost Problems, secondary pollution can be produced in removal process or cost too high, be also difficult to large-scale industrial production at present.Therefore, study that a kind of technique is simple, non-secondary pollution, the with low cost and WRPUF resource utilization method that added value is high realize WRPUF efficient circulation to utilize and the effective way of protection of the environment.
For the environmental pollution that causes of discarded a large amount of rigid urethane foam every year of current China and problem of resource waste; the present invention is from environment protection, energy-saving and cost-reducing and Sustainable development; activation is pulverized in WRPUF solid state mechanochemistry reaction; and chemical modification is carried out to the microparticle surfaces of activation micro mist, use it for the reinforcing filler of elastomeric material.WRPUF adds in rubber and will play strengthening action after pulverizing, and must solve following three key technical problems.
(1) control of WRPUF micro mist size and size distribution
In the molecular structure of PU foam itself and WRPUF, the existence of abscess, causes WRPUF to have certain toughness, simply utilizes mechanical disintegration, be difficult to meet the requirements of particle fineness and uniform size distribution.And certain particle fineness and uniform size distribution are the keys that WRPUF high added value is recycled, therefore select suitable solid state mechanochemistry to pulverize activation method, to design appropriate pulverizing activating process most important to follow-up research.
(2) WRPUF separates the control of crosslinking degree and modification micro mist color
WRPUF micro mist is wanted to play obvious strengthening action to rubber as reinforcing filler, must separate cross-linking modified through chemistry, make with the functional group that can react on its molecular chain, so as when Reinforced Rubber and compatilizer react, improve and the consistency of rubber matrix.The solution crosslinking degree of WRPUF be directly connected to functional group's number on WRPUF molecular chain number, thus control well and separate crosslinking degree and seem particularly important.In addition, the difference that WRPUF separates cross-linking method and technique may cause modification micro mist to darken, and then affects the outward appearance of end article.So select suitable solution cross-linking method and technique, the solution crosslinking degree of control WRPUF and color are the keys ensureing that WRPUF high added value is recycled.
(3) the dispersed and Study on Compatibility of WRPUF activate micro powder in rubber base material
During WRPUF activate micro powder Reinforced Rubber material, can there is the problem that dispersion is uneven, consistency is bad in WRPUF activate micro powder, cause elastomeric material degradation in rubber matrix.Therefore, suitable dispersion agent and compatilizer should be selected and determine its consumption, design suitable complete processing, to promote that WRPUF activate micro powder is dispersed and have good two-phase consistency in rubber matrix, guarantee that the over-all properties of WRPUF activate micro powder Reinforced Rubber material is best.
Summary of the invention
The technical problem to be solved in the present invention is: based on the problems referred to above, the invention provides a kind of preparation method of modified abandoned rigid urethane foam activate micro powder Reinforced Rubber material.
The present invention solves the technical scheme that its technical problem adopts: a kind of preparation method of modified abandoned rigid urethane foam activate micro powder Reinforced Rubber material, comprises the following steps:
(1) removal of impurities coarse crushing: remove metal parts, metal sheet or other plastic component impurity in waste hard polyurethane foam plastic WRPUF, utilize pulverizer that WRPUF is carried out normal temperature coarse crushing;
(2) activation in small, broken bits: solid state mechanochemistry reaction occurs at normal temperatures for the WRPUF solid state mechanochemistry reactor after coarse crushing or mill, pulverizing is 40 ~ 200 object WRPUF activate micro powders, the speed of grinding plate of solid state mechanochemistry reactor is 20 ~ 80rpm, grinding times 1 ~ 25 time, mill roller spacing is 0.1 ~ 2mm, crosses roller 3 ~ 20 times;
(3) surface modification: the solution linking agent adding 5 ~ 50wt% in WRPUF activate micro powder, mechanically mixing is even, utilize solid state mechanochemistry reactor or mill to carry out Re-Li to WRPUF activate micro powder surface and separate cross-linking chemistry modification, temperature of reaction is 120 ~ 250 DEG C, obtain the WRPUF activate micro powder of surface modification, the speed of grinding plate of solid state mechanochemistry reactor is 15 ~ 60rpm, grinding times 1 ~ 15 time, mill roller spacing is 0.2 ~ 2mm, crosses roller 1 ~ 10 time;
(4) reinforced rubber: in mass parts, the each component of sizing material is weighed: rubber 100 parts by following formula, 2 ~ 8 parts, zinc oxide, stearic acid 1 ~ 4 part, surface modification WRPUF activate micro powder 5 ~ 60 parts, compatilizer 1 ~ 9 part, 1 ~ 4 part, anti-aging agent, dispersion agent 1 ~ 10 part, vulcanizing agent 1 ~ 4 part, vulcanization accelerator 0.5 ~ 5 part, other auxiliary agent 0 ~ 100 part, by plasticating, the conventional rubber complete processings such as mixing and sulfuration, obtain the elastomeric material that surface modification WRPUF activate micro powder strengthens, curing temperature is 135 ~ 185 DEG C, curing time is 5 ~ 120min, sulfide stress is 5 ~ 20MPa.
Further, in step (3), solution linking agent is one or more in low mass molecule alcohol, low molecule amine or hydramine, low mass molecule alcohol is ethylene glycol, propylene glycol, butyleneglycol, glycol ether, dipropylene glycol, 1, one or more in 4-butyleneglycol or polyoxyethylene glycol, low molecule amine is the compound containing amido, be specially one or more in diethylenetriamine, triethylene tetramine or tetraethylene pentamine, hydramine is alkanolamine, is specially one or more in monoethanolamine, diethanolamine, trolamine or dimethylethanolamine.
Further, rubber is one or more in natural rubber or synthetic rubber in step (4).
Further, in step (4), compatilizer is the maleic anhydride grafts of rubber or reacts by maleic anhydride monomer and rubber matrix the grafts generated in the rubber reinforcement material course of processing.
Further, in step (4), vulcanizing agent is one or more in sulphur, sulfur donor, superoxide, metal oxide, polyamine or resin.
Further, in step (4), compatilizer if react generation by maleic anhydride in the Reinforced Rubber course of processing, then then should contain superoxide in vulcanizing agent, part superoxide is as the initiator of compatilizer formation reaction.
Further, in step (4), anti-aging agent, dispersion agent, vulcanization accelerator are all commercially available conventional rubber ingredients.
Further, in step (4), other auxiliary agent determines the kind that adds and quantity according to the use properties of Reinforced Rubber material.
The invention has the beneficial effects as follows: adopt solid state mechanochemistry reaction and Re-Li to separate cross-linking chemistry modification method and reclaim WRPUF, this method synthesis advantage of physiochemical mutagens method and chemical recycling, simple for process, easy to operate, non-secondary pollution, and used as the reinforcing filler of elastomeric material, reinforcing effect is good, the rate of recovery is high, achieves the recycling of WRPUF high added value.
Embodiment
The invention will be further described in conjunction with specific embodiments now, and following examples are intended to the present invention instead of limitation of the invention further are described.
Embodiment 1
Waste hard polyurethane foam plastic (WRPUF) carries out coarse crushing with pulverizer after removing metal wherein or plastic fittings, controls rigid urethane foam grain diameter and is less than 3cm.WRPUF after coarse crushing is placed in mill and carries out activation in small, broken bits by normal-temperature solid-phase force-chemical reaction, roll spacing 0.2mm, and cross roller 8 times, obtaining particle diameter is 80 ~ 100 object WRPUF activate micro powders.
The solution linking agent tetraethylene pentamine of 25wt% (relative to WRPUF activate micro powder quality) is added in WRPUF activate micro powder, mechanical stirring is even, and the mill being placed in 150 ~ 155 DEG C carries out solution crosslinking reaction, roll spacing 0.2mm, cross roller 4 times, obtain the WRPUF activate micro powder of surface modification.
Above-mentioned WRPUF activate micro powder is used for strengthening paracril (NBR), rubber preparation technology traditionally obtains WRPUF activate micro powder and strengthens NBR material, its basic recipe is (phr): NBR 100, ZnO 5, stearic acid 2, anti-aging agent 1.5, dispersion agent 1, promotor 1.5, sulphur 2, and grafted monomer MAH, vulcanizing agent DCP and modification WRPUF activate micro powder are variable.The processes such as plasticating traditionally, mixing and sulfuration are shaping, and cure conditions is 165 DEG C × 15MPa × 20min.Strengthen NBR and do not strengthen NBR and contrast, its performance is as shown in table 1.
Table 1
| Sequence number | Modification micro mist | MAH | DCP | Tensile strength/MPa | Elongation at break/% | Shore hardness |
| 1 | 0 | 0 | 0 | 3.85 | 1243 | 56 |
| 2 | 5 | 1 | 1 | 4.17 | 1372 | 57 |
| 3 | 20 | 4 | 1 | 7.78 | 2114 | 59 |
| 4 | 40 | 6 | 1.5 | 8.27 | 2126 | 65 |
| 5 | 50 | 7 | 1.8 | 6.19 | 1895 | 68 |
| 6 | 60 | 9 | 4 | 4.08 | 1038 | 77 |
Embodiment 2
Waste hard polyurethane foam plastic (WRPUF) carries out coarse crushing with pulverizer after removing metal wherein or plastic fittings, controls rigid urethane foam grain diameter and is less than 3cm.WRPUF after coarse crushing is placed in mill and carries out activation in small, broken bits by normal-temperature solid-phase force-chemical reaction, roll spacing 0.1mm, and cross roller 8 times, obtaining particle diameter is 100 ~ 120 object WRPUF activate micro powders.
The solution linking agent glycol ether of 30wt% (relative to WRPUF activate micro powder quality) is added in WRPUF activate micro powder, mechanical stirring is even, and the mill being placed in 165 ~ 170 DEG C carries out solution crosslinking reaction, roll spacing 0.2mm, cross roller 5 times, obtain the WRPUF activate micro powder of surface modification.
Above-mentioned WRPUF activate micro powder is used for strengthening styrene-butadiene rubber(SBR) (SBR), rubber preparation technology traditionally obtains WRPUF activate micro powder and strengthens SBR material, its basic recipe is (phr): SBR 100, ZnO 5, stearic acid 2, anti-aging agent 2, dispersion agent 1, promotor 1.5, sulphur 2, compatilizer (rubber graft, as SEBS-g-MAH) and modification WRPUF activate micro powder are variable.The processes such as plasticating traditionally, mixing and sulfuration are shaping, and cure conditions is 165 DEG C × 15MPa × 25min.Strengthen SBR and do not strengthen SBR and contrast, its performance is as shown in table 2.
Table 2
| Sequence number | Modification micro mist | Compatilizer | Tensile strength/MPa | Elongation at break/% | Shore hardness |
| 1 | 0 | 0 | 2.82 | 873 | 48 |
| 2 | 5 | 1 | 3.07 | 914 | 49 |
| 3 | 20 | 3 | 5.54 | 1036 | 53 |
| 4 | 40 | 6 | 7.15 | 1173 | 59 |
| 5 | 60 | 9 | 6.13 | 952 | 64 |
With above-mentioned according to desirable embodiment of the present invention for enlightenment, by above-mentioned description, relevant staff in the scope not departing from this invention technological thought, can carry out various change and amendment completely.The technical scope of this invention is not limited to the content on specification sheets, must determine its technical scope according to right.
Claims (8)
1. a preparation method for modified abandoned rigid urethane foam activate micro powder Reinforced Rubber material, is characterized in that: comprise the following steps:
(1) removal of impurities coarse crushing: remove metal parts, metal sheet or other plastic component impurity in waste hard polyurethane foam plastic WRPUF, utilize pulverizer that WRPUF is carried out normal temperature coarse crushing;
(2) activation in small, broken bits: solid state mechanochemistry reaction occurs at normal temperatures for the WRPUF solid state mechanochemistry reactor after coarse crushing or mill, pulverizing is 40 ~ 200 object WRPUF activate micro powders, the speed of grinding plate of solid state mechanochemistry reactor is 20 ~ 80rpm, grinding times 1 ~ 25 time, mill roller spacing is 0.1 ~ 2mm, crosses roller 3 ~ 20 times;
(3) surface modification: the solution linking agent adding 5 ~ 50wt% in WRPUF activate micro powder, mechanically mixing is even, utilize solid state mechanochemistry reactor or mill to carry out Re-Li to WRPUF activate micro powder surface and separate cross-linking chemistry modification, temperature of reaction is 120 ~ 250 DEG C, obtain the WRPUF activate micro powder of surface modification, the speed of grinding plate of solid state mechanochemistry reactor is 15 ~ 60rpm, grinding times 1 ~ 15 time; Mill roller spacing is 0.2 ~ 2mm, crosses roller 1 ~ 10 time;
(4) reinforced rubber: in mass parts, the each component of sizing material is weighed: rubber 100 parts, 2 ~ 8 parts, zinc oxide, stearic acid 1 ~ 4 part, surface modification WRPUF activate micro powder 5 ~ 60 parts, compatilizer 1 ~ 9 part, 1 ~ 6 part, anti-aging agent, dispersion agent 1 ~ 10 part, vulcanizing agent 1 ~ 4 part, vulcanization accelerator 0.5 ~ 5 part, other auxiliary agent 0 ~ 100 part by following formula, by plasticating, mixing and sulfuration process, obtain the elastomeric material that surface modification WRPUF activate micro powder strengthens, curing temperature is 135 ~ 185 DEG C, curing time is 5 ~ 120min, and sulfide stress is 5 ~ 20MPa.
2. the preparation method of a kind of modified abandoned rigid urethane foam activate micro powder Reinforced Rubber material according to claim 1, it is characterized in that: separating linking agent in described step (3) is low mass molecule alcohol, one or more in low molecule amine or hydramine, low mass molecule alcohol is ethylene glycol, propylene glycol, butyleneglycol, glycol ether, dipropylene glycol, 1, one or more in 4-butyleneglycol or polyoxyethylene glycol, low molecule amine is the compound containing amido, be specially diethylenetriamine, one or more in triethylene tetramine or tetraethylene pentamine, hydramine is alkanolamine, be specially monoethanolamine, diethanolamine, one or more in trolamine or dimethylethanolamine.
3. the preparation method of a kind of modified abandoned rigid urethane foam activate micro powder Reinforced Rubber material according to claim 1, is characterized in that: rubber is one or more in natural rubber or synthetic rubber in described step (4).
4. the preparation method of a kind of modified abandoned rigid urethane foam activate micro powder Reinforced Rubber material according to claim 1, is characterized in that: in described step (4), compatilizer is the maleic anhydride grafts of rubber or reacts by maleic anhydride monomer and rubber matrix the grafts generated in the rubber reinforcement material course of processing.
5. the preparation method of a kind of modified abandoned rigid urethane foam activate micro powder Reinforced Rubber material according to claim 1, is characterized in that: in described step (4), vulcanizing agent is one or more in sulphur, sulfur donor, superoxide, metal oxide, polyamine or resin.
6. the preparation method of a kind of modified abandoned rigid urethane foam activate micro powder Reinforced Rubber material according to claim 1, it is characterized in that: described step (4) if in compatilizer be in the Reinforced Rubber course of processing, react generation by maleic anhydride, then then should contain superoxide in vulcanizing agent, part superoxide is as the initiator of compatilizer formation reaction.
7. the preparation method of a kind of modified abandoned rigid urethane foam activate micro powder Reinforced Rubber material according to claim 1, is characterized in that: in described step (4), anti-aging agent, dispersion agent, vulcanization accelerator are all commercially available conventional rubber ingredients.
8. the preparation method of a kind of modified abandoned rigid urethane foam activate micro powder Reinforced Rubber material according to claim 1, is characterized in that: in described step (4), other auxiliary agent determines the kind that adds and quantity according to the use properties of Reinforced Rubber material.
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| CN106433004A (en) * | 2016-10-11 | 2017-02-22 | 佛山市飞时达新材料科技有限公司 | SEBS cable material and preparation method thereof |
| CN107383305A (en) * | 2017-08-23 | 2017-11-24 | 北京家美科技有限公司 | Difficult degradation technical polyurethane product waste regenerated Application way and reconstituted product |
| CN107511947A (en) * | 2017-08-15 | 2017-12-26 | 滁州市玉林聚氨酯有限公司 | A kind of recoverying and utilizing method of polyurethane elastomer waste material |
| CN108485007A (en) * | 2018-04-23 | 2018-09-04 | 周荣 | A kind of preparation method of anti-high-pressure type rubber packing material |
| CN108795021A (en) * | 2018-06-28 | 2018-11-13 | 江苏明科精密橡塑科技有限公司 | A method of along fourth or natural rubber and the compound mixing of polyurethane |
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| CN114805972A (en) * | 2022-05-05 | 2022-07-29 | 青岛科技大学 | Method for preparing reclaimed rubber by using polyurethane chemical catalytic degradation product as regeneration auxiliary agent |
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- 2015-08-19 CN CN201510510432.1A patent/CN105017581B/en active Active
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| CN106433004A (en) * | 2016-10-11 | 2017-02-22 | 佛山市飞时达新材料科技有限公司 | SEBS cable material and preparation method thereof |
| CN107511947A (en) * | 2017-08-15 | 2017-12-26 | 滁州市玉林聚氨酯有限公司 | A kind of recoverying and utilizing method of polyurethane elastomer waste material |
| CN107383305A (en) * | 2017-08-23 | 2017-11-24 | 北京家美科技有限公司 | Difficult degradation technical polyurethane product waste regenerated Application way and reconstituted product |
| CN108485007A (en) * | 2018-04-23 | 2018-09-04 | 周荣 | A kind of preparation method of anti-high-pressure type rubber packing material |
| CN108795021A (en) * | 2018-06-28 | 2018-11-13 | 江苏明科精密橡塑科技有限公司 | A method of along fourth or natural rubber and the compound mixing of polyurethane |
| CN110183153A (en) * | 2019-05-20 | 2019-08-30 | 福建师范大学 | A method of inorganic artificial stone is prepared using solid state mechanochemistry reactor |
| CN110684501A (en) * | 2019-09-25 | 2020-01-14 | 郑州骏惠材料技术有限公司 | Polyurethane hard foam powder filled single-component polyurethane sealant and preparation method thereof |
| CN110684501B (en) * | 2019-09-25 | 2022-03-22 | 郑州大学 | Polyurethane hard foam powder filled single-component polyurethane sealant and preparation method thereof |
| CN114805972A (en) * | 2022-05-05 | 2022-07-29 | 青岛科技大学 | Method for preparing reclaimed rubber by using polyurethane chemical catalytic degradation product as regeneration auxiliary agent |
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