CN103450464A - Low-temperature thermo-cementing polyester - Google Patents
Low-temperature thermo-cementing polyester Download PDFInfo
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- CN103450464A CN103450464A CN2013103555638A CN201310355563A CN103450464A CN 103450464 A CN103450464 A CN 103450464A CN 2013103555638 A CN2013103555638 A CN 2013103555638A CN 201310355563 A CN201310355563 A CN 201310355563A CN 103450464 A CN103450464 A CN 103450464A
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Abstract
The invention discloses a low-temperature thermo-cementing polyester relating to the field of a hot melt adhesive. The polyester comprises the following components by weight: 1760-2640kg of waste polyester, 1511-2267kg of ethylene glycol, 185-200kg of m-phthalic acid, 85-105kg of diethylene glycol, 1.10-1.25kg of trimethyl phosphate, 0.96-1.44kg of antimony acetate, 0.35-0.53kg of sodium acetate, 0.68-1.02kg of antioxidant 1010, and 0.64-0.96kg of sodium benzoate. The polyester is strong in adhesive force, good in elasticity of a bonded product, low in production cost, and relatively low in energy consumption and material consumption in the process.
Description
[technical field]
The present invention relates to the hot melt adhesive field, especially relate to a kind of Low Temperature Thermal bonded polyester of utilizing discarded polyester beverage bottle regeneration.
[background technology]
Known, fusing point is only that the Low Temperature Thermal bonded polyester of 100～150 ℃ is called again low-melting point polyester or polyester hot-melt adhesive, and in application, not only over-all properties is better for it, and does not also need solvent during applying glue, is beneficial to very much the protection to environment; Yet, because existing Low Temperature Thermal bonded polyester is many, by terephthalic acid and the production of ethylene glycol route, made, need to use relatively large m-phthalic acid and glycol ether in its preparation technology, therefore its production cost is relatively high, simultaneously, terephthalic acid and ethylene glycol not only can react the generation water byproduct in preparation, and these water also can absorb amount of heat, be the existing production technique for the preparation of the Low Temperature Thermal bonded polyester not only material consumption is higher, but also the power consumption larger;
On the other hand, the packing bottle of the drinks such as a large amount of soda pops, mineral water is to be made by polyester substantially in the market, according to statistics, the polyester beverage bottle weight that the whole world went out of use in 1 year is just up to 1,000 ten thousand tons of left and right, and wherein the discarded polyester beverage bottle weight of China is just occupied 5,000,000 tons more than; Due to discarded polyester bottles, can not spontaneously degrade after entering physical environment, and then can cause serious environmental pollution and the waste of resource, therefore, how effectively these bond propertiess under molten state of recycle are good, have again simultaneously excellent electrical insulating property and heat-resisting, media-resistant and processability preferably the waste polyester bottle just become an extremely important and significant research topic.
[summary of the invention]
In order to overcome the deficiency in background technology, the invention discloses a kind of Low Temperature Thermal bonded polyester, described polyester is prepared from by discarded polyester beverage bottle, and described polyester not only bounding force is strong, the adhesive article good springiness, and the energy consumption in its production cost and technique, material consumption are all relatively low.
For achieving the above object, the present invention adopts following technical scheme:
A kind of Low Temperature Thermal bonded polyester, described polyester consists of in mass ratio following component: 1760～2640 kilograms of useless polyester, 1511～2267 kilograms of ethylene glycol, 185～200 kilograms of m-phthalic acids, 85～105 kilograms of glycol ethers, 1.10～1.25 kilograms of trimethyl phosphite 99s, 0.96～1.44 kilogram of antimony acetate, 0.35～0.53 kilogram of sodium-acetate, 0.68～1.02 kilogram of antioxidant 1010,0.64～0.96 kilogram of Sodium Benzoate.
Described Low Temperature Thermal bonded polyester, described polyester consists of in mass ratio following component: 2200 kilograms of useless polyester, 1889 kilograms of ethylene glycol, 193 kilograms of m-phthalic acids, 95 kilograms of glycol ethers, 1.08 kilograms of trimethyl phosphite 99s, 1.20 kilograms of antimony acetates,, 0.44 kilogram of sodium-acetate, 0.85 kilogram of antioxidant 1010,0.80 kilogram of Sodium Benzoate.
Described Low Temperature Thermal bonded polyester, described polyester is made by following flow process by above-mentioned component:
A, the polyester that will give up are ground into and are not more than the wide fragment of long * 16 ㎝ of 16 ㎝, then wait until the useless polyester chips of water ratio≤0.4% after clean-out system cleaning, clean water rinsing and negative pressure drying;
B, will give up polyester chips, trimethyl phosphite 99 and sodium-acetate feed in the ethylene glycol that reactor temperature is 197 ± 2 ℃ by feeder, and are 100 ± 1 ℃ by the control of reactor top fractionator overhead temperature; After 20～30 minutes, after temperature rise to 220 in the question response still～240 ℃, stir 60～80 minutes, reactor top fractionator overhead temperature is adjusted into to 192 ± 5 ℃, the ethylene glycol in reactor is steamed;
C, when reactor top fractionator overhead temperature is down to 100 ± 1 ℃, reaction generates ethylene glycol terephthalate, now alcoholysis reaction completes;
D, make reactor be warming up to 260～270 ℃, and added m-phthalic acid by feeder in 1～2 hour, in adition process, reactor top fractionator overhead temperature is controlled to 100 ± 1 ℃, make m-phthalic acid and ethylene glycol generate ethylene isophthalate, and receive the generation water after remaining glycol reaction in m-phthalic acid and system simultaneously;
E, add Sodium Benzoate after adding m-phthalic acid, and stir 30～60 minutes, then first make ethylene glycol terephthalate and ethylene isophthalate melt by high-temperature centrifugal pump through thick non-PET materials such as the first coarse filter filtering metal of 250～300 ц, polyvinyl chloride, again through finely ground particle substances such as the most mechanical impuritys of the second coarse filter filtering of 50～100 ц, the broken ends of polyvinyl chloride carbide, finally by fine particle such as the fine filter filtering residue mechanical impurity of crossing 15～30 ц, polyvinyl chloride carbide powders;
F, melt is fed to polycondensation vessel, add glycol ether, antimony acetate and antioxidant 1010, make temperature rise to 240 in polycondensation vessel～260 ℃; Polycondensation vessel and vacuum system slowly were decompressed to 667～700pa in 45～60 minutes, more further decompression is 40 ± 5Pa to vacuum tightness; In 3～4 hours, to control temperature in polycondensation vessel and rise to gradually 282～285 ℃, reaction product is polyethylene terephthalate;
G, under the effect of smelt gear pump, by underwater pelletizer, the melt cast bar is cut into to the Low Temperature Thermal bonded polyester finished product of Ф 3.0～3.3mm * 3～4mm.
Described Low Temperature Thermal bonded polyester, used during the useless polyester alcoholysis of after the ethylene glycol steamed in described flow process B insulation stores, staying other batches.
Owing to adopting technical scheme as above, the present invention has following beneficial effect:
Low Temperature Thermal bonded polyester of the present invention, described polyester is prepared from by discarded polyester beverage bottle, its melt-spinning good spinnability, melt journey in thaw process short, fiber is easy to dryness finalization, can be used for fibrous heat-bondable fibre, footwear material heat bonding adhesive tape, woodenware heat bonding adhesive tape, the bonding adhesive tape of metal fever, non-woven fabrics and Pading cloth heat bonding powder etc., therefore, prepare described polyester and not only can curb environmental pollution accordingly, but also can effectively create economic benefit;
In addition, the consumption of stupid dioctyl phthalate and glycol ether between described polyester not only can effectively reduce in preparation, but also do not have by product to produce, therefore, the energy consumption in its production cost and technique, material consumption are all relatively low; Described Low Temperature Thermal bonded polyester makes the regeneration of waste polyester break away from low-grade Physical Processing, make waste polyester regeneration come into the modified poly ester field, thereby reach the cost that has reduced modified poly ester, the product specification of waste polyester regeneration and the purpose of added value have been improved again, and then make related products have more price advantage, be more conducive to apply.
[embodiment]
Can explain in more detail the present invention by the following examples, disclose purpose of the present invention and be intended to protect all changes and improvements in the scope of the invention, the present invention is not limited to the following examples:
Described Low Temperature Thermal bonded polyester, described polyester consists of in mass ratio following component: 1760～2640 kilograms of useless polyester, 1511～2267 kilograms of ethylene glycol, 185～200 kilograms of m-phthalic acids, 85～105 kilograms of glycol ethers, 1.10～1.25 kilograms of trimethyl phosphite 99s, 0.96～1.44 kilogram of antimony acetate, 0.35～0.53 kilogram of sodium-acetate, 0.68～1.02 kilogram of antioxidant 1010,0.64～0.96 kilogram of Sodium Benzoate;
Described Low Temperature Thermal bonded polyester is made by following flow process by above-mentioned component:
A, the polyester that will give up are ground into and are not more than the wide fragment of long * 16 ㎝ of 16 ㎝, then wait until the useless polyester chips of water ratio≤0.4% after clean-out system cleaning, clean water rinsing and negative pressure drying;
B, will give up polyester chips, trimethyl phosphite 99 and sodium-acetate feed in the ethylene glycol that reactor temperature is 197 ± 2 ℃ by feeder, and are 100 ± 1 ℃ by the control of reactor top fractionator overhead temperature; After 20～30 minutes, after temperature rise to 220 in the question response still～240 ℃, stir 60～80 minutes, reactor top fractionator overhead temperature is adjusted into to 192 ± 5 ℃, the ethylene glycol in reactor is steamed; Now, in the time of the ethylene glycol steamed can being incubated to the useless polyester alcoholysis of after storage, staying other batches, use;
C, when reactor top fractionator overhead temperature is down to 100 ± 1 ℃, reaction generates ethylene glycol terephthalate, now alcoholysis reaction completes;
D, make reactor be warming up to 260～270 ℃, and added m-phthalic acid by feeder in 1～2 hour, in adition process, reactor top fractionator overhead temperature is controlled to 100 ± 1 ℃, make m-phthalic acid and ethylene glycol generate ethylene isophthalate, and receive the generation water after remaining glycol reaction in m-phthalic acid and system simultaneously;
E, add Sodium Benzoate after adding m-phthalic acid, and stir 30～60 minutes, then first make ethylene glycol terephthalate melt and ethylene isophthalate melt by high-temperature centrifugal pump through thick non-PET materials such as the first coarse filter filtering metal of 250～300 ц, polyvinyl chloride, again through finely ground particle substances such as the most mechanical impuritys of the second coarse filter filtering of 50～100 ц, the broken ends of polyvinyl chloride carbide, finally by fine particle such as the fine filter filtering residue mechanical impurity of crossing 15～30 ц, polyvinyl chloride carbide powders;
F, melt is fed to polycondensation vessel, add glycol ether, antimony acetate and antioxidant 1010, make temperature rise to 240 in polycondensation vessel～260 ℃; Polycondensation vessel and vacuum system slowly were decompressed to 667～700pa in 45～60 minutes, more further decompression is 40 ± 5Pa to vacuum tightness; In 3～4 hours, to control temperature in polycondensation vessel and rise to gradually 282～285 ℃, reaction product is polyethylene terephthalate;
G, under the effect of smelt gear pump, by underwater pelletizer, the melt cast bar is cut into to the Low Temperature Thermal bonded polyester finished product of Ф 3.0～3.3mm * 3～4mm.
Should select in conjunction with particular case the numerical value of temperature and time in the consumption of each component and flow process, for example following flow process while preparing described Low Temperature Thermal bonded polyester:
A, 2200 kilograms of useless polyester are ground into and are not more than the wide fragment of long * 16 ㎝ of 16 ㎝, then through clean-out system clean, the useless polyester chips of water ratio≤0.4% by the time after clean water rinsing and negative pressure drying;
B, the polyester chips that will give up, 1.08 kilograms of trimethyl phosphite 99s and 0.44 kilogram of sodium-acetate feed in the ethylene glycol of 1889 kilograms that reactor temperature is 197 ± 2 ℃ by feeder, and are 100 ± 1 ℃ by the control of reactor top fractionator overhead temperature; After 20 minutes, stir 60 minutes after temperature rise to 220 ℃ in the question response still, reactor top fractionator overhead temperature is adjusted into to 192 ± 5 ℃, the ethylene glycol in reactor is steamed; Now, in the time of the ethylene glycol steamed can being incubated to the useless polyester alcoholysis of after storage, staying other batches, use;
C, when reactor top fractionator overhead temperature is down to 100 ± 1 ℃, reaction generates ethylene glycol terephthalate, now alcoholysis reaction completes;
D, make reactor be warming up to 260 ℃, and added 193 kilograms of m-phthalic acids by feeder in 1 hour, in adition process, reactor top fractionator overhead temperature is controlled to 100 ± 1 ℃, make m-phthalic acid and ethylene glycol generate ethylene isophthalate, and receive the generation water after remaining glycol reaction in m-phthalic acid and system simultaneously;
E, add 0.80 kilogram of Sodium Benzoate after adding m-phthalic acid, and stir 30 minutes, then first make ethylene glycol terephthalate melt and ethylene isophthalate melt by high-temperature centrifugal pump through thick non-PET materials such as the first coarse filter filtering metal of 300 ц, polyvinyl chloride, again through finely ground particle substances such as the most mechanical impuritys of the second coarse filter filtering of 100 ц, the broken ends of polyvinyl chloride carbide, finally by fine particle such as the fine filter filtering residue mechanical impurity of crossing 30 ц, polyvinyl chloride carbide powders;
F, melt is fed to polycondensation vessel, add 95 kilograms of glycol ethers, 1.20 kilograms of antimony acetates and 0.85 kilogram of antioxidant 1010, make temperature rise to 240 ℃ in polycondensation vessel; Polycondensation vessel and vacuum system slowly were decompressed to 667pa in 45 minutes, more further decompression is 40 ± 5Pa to vacuum tightness; In 3 hours, to control temperature in polycondensation vessel and rise to gradually 282 ℃, reaction product is polyethylene terephthalate;
G, under the effect of smelt gear pump, by underwater pelletizer, the melt cast bar is cut into to the Low Temperature Thermal bonded polyester finished product of Ф 3.0～3.3mm * 3～4mm.
With terephthalic acid, with the Low Temperature Thermal bonded polyester of ethylene glycol route production, compare, the preparation flow of described Low Temperature Thermal bonded polyester has following advantage:
1) described polyester is to be prepared from by discarded bottle level production of polyester, a part of m-phthalic acid and glycol ether have been added with when producing due to these bottle of level polyester, therefore, this not only is conducive to reduce the fusing point of polyester, but also can in preparation, reduce the consumption of m-phthalic acid and glycol ether, thereby reach the purpose effectively reduced costs;
2) there is water byproduct to produce when terephthalic acid and glycol reaction, and, in described polyester preparation process, ethylene glycol and reacting of useless polyester do not have by product to produce, and ethylene glycol can also cycling and reutilization, therefore, material consumption is lower in the preparation for described polyester;
3) described polyester only has the intensification heat of ethylene glycol in process of production, and does not have terephthalic acid and glycol reaction to generate evaporation of water heat, and therefore energy consumption is lower in the preparation for described polyester.
Part not in the detailed description of the invention is prior art, therefore the present invention is not described in detail.
Claims (5)
1. a Low Temperature Thermal bonded polyester, it is characterized in that: described polyester consists of in mass ratio following component: 1760～2640 kilograms of useless polyester, 1511～2267 kilograms of ethylene glycol, 185～200 kilograms of m-phthalic acids, 85～105 kilograms of glycol ethers, 1.10～1.25 kilograms of trimethyl phosphite 99s, 0.96～1.44 kilogram of antimony acetate, 0.35～0.53 kilogram of sodium-acetate, 0.68～1.02 kilogram of antioxidant 1010,0.64～0.96 kilogram of Sodium Benzoate.
2. Low Temperature Thermal bonded polyester according to claim 1, it is characterized in that: described polyester consists of in mass ratio following component: 2200 kilograms of useless polyester, 1889 kilograms of ethylene glycol, 193 kilograms of m-phthalic acids, 95 kilograms of glycol ethers, 1.08 kilograms of trimethyl phosphite 99s, 1.20 kilograms of antimony acetates,, 0.44 kilogram of sodium-acetate, 0.85 kilogram of antioxidant 1010,0.80 kilogram of Sodium Benzoate.
3. Low Temperature Thermal bonded polyester according to claim 1 and 2, it is characterized in that: described polyester is made by following flow process:
A, the polyester that will give up are ground into and are not more than the wide fragment of long * 16 ㎝ of 16 ㎝, then wait until the useless polyester chips of water ratio≤0.4% after clean-out system cleaning, clean water rinsing and negative pressure drying;
B, will give up polyester chips, trimethyl phosphite 99 and sodium-acetate feed in the ethylene glycol that reactor temperature is 197 ± 2 ℃ by feeder, and are 100 ± 1 ℃ by the control of reactor top fractionator overhead temperature; After 20～30 minutes, after temperature rise to 220 in the question response still～240 ℃, stir 60～80 minutes, reactor top fractionator overhead temperature is adjusted into to 192 ± 5 ℃, the ethylene glycol in reactor is steamed;
C, when reactor top fractionator overhead temperature is down to 100 ± 1 ℃, reaction generates ethylene glycol terephthalate, now alcoholysis reaction completes;
D, make reactor be warming up to 260～270 ℃, and added m-phthalic acid by feeder in 1～2 hour, in adition process, reactor top fractionator overhead temperature is controlled to 100 ± 1 ℃, make m-phthalic acid and ethylene glycol generate ethylene isophthalate, and receive the generation water after remaining glycol reaction in m-phthalic acid and system simultaneously;
E, add Sodium Benzoate after adding m-phthalic acid, and stir 30～60 minutes, then first make ethylene glycol terephthalate and ethylene isophthalate melt by high-temperature centrifugal pump through thick non-PET materials such as the first coarse filter filtering metal of 250～300 ц, polyvinyl chloride, again through finely ground particle substances such as the most mechanical impuritys of the second coarse filter filtering of 50～100 ц, the broken ends of polyvinyl chloride carbide, finally by fine particle such as the fine filter filtering residue mechanical impurity of crossing 15～30 ц, polyvinyl chloride carbide powders;
F, melt is fed to polycondensation vessel, add glycol ether, antimony acetate and antioxidant 1010, make temperature rise to 240 in polycondensation vessel～260 ℃; Polycondensation vessel and vacuum system slowly were decompressed to 667～700pa in 45～60 minutes, more further decompression is 40 ± 5Pa to vacuum tightness; In 3～4 hours, to control temperature in polycondensation vessel and rise to gradually 282～285 ℃, reaction product is polyethylene terephthalate;
G, under the effect of smelt gear pump, by underwater pelletizer, the melt cast bar is cut into to the Low Temperature Thermal bonded polyester finished product of Ф 3.0～3.3mm * 3～4mm.
4. Low Temperature Thermal bonded polyester according to claim 1 and 2, it is characterized in that: described polyester is made by following flow process:
A, the polyester that will give up are ground into and are not more than the wide fragment of long * 16 ㎝ of 16 ㎝, then wait until the useless polyester chips of water ratio≤0.4% after clean-out system cleaning, clean water rinsing and negative pressure drying;
B, will give up polyester chips, trimethyl phosphite 99 and sodium-acetate feed in the ethylene glycol that reactor temperature is 197 ± 2 ℃ by feeder, and are 100 ± 1 ℃ by the control of reactor top fractionator overhead temperature; After 20 minutes, stir 60 minutes after temperature rise to 220 ℃ in the question response still, reactor top fractionator overhead temperature is adjusted into to 192 ± 5 ℃, the ethylene glycol in reactor is steamed;
C, when reactor top fractionator overhead temperature is down to 100 ± 1 ℃, reaction generates ethylene glycol terephthalate, now alcoholysis reaction completes;
D, make reactor be warming up to 260 ℃, and added m-phthalic acid by feeder in 1 hour, in adition process, reactor top fractionator overhead temperature is controlled to 100 ± 1 ℃, make m-phthalic acid and ethylene glycol generate ethylene isophthalate, and receive the generation water after remaining glycol reaction in m-phthalic acid and system simultaneously;
E, add Sodium Benzoate after adding m-phthalic acid, and stir 30 minutes, then first make ethylene glycol terephthalate and ethylene isophthalate melt by high-temperature centrifugal pump through thick non-PET materials such as the first coarse filter filtering metal of 300 ц, polyvinyl chloride, again through finely ground particle substances such as the most mechanical impuritys of the second coarse filter filtering of 100 ц, the broken ends of polyvinyl chloride carbide, finally by fine particle such as the fine filter filtering residue mechanical impurity of crossing 30 ц, polyvinyl chloride carbide powders;
F, melt is fed to polycondensation vessel, add glycol ether, antimony acetate and antioxidant 1010, make temperature rise to 240 ℃ in polycondensation vessel; Polycondensation vessel and vacuum system slowly were decompressed to 667pa in 45 minutes, more further decompression is 40 ± 5Pa to vacuum tightness; In 3 hours, to control temperature in polycondensation vessel and rise to gradually 282 ℃, reaction product is polyethylene terephthalate;
G, under the effect of smelt gear pump, by underwater pelletizer, the melt cast bar is cut into to the Low Temperature Thermal bonded polyester finished product of Ф 3.0～3.3mm * 3～4mm.
5. according to the described Low Temperature Thermal bonded polyester of claim 3 or 4, it is characterized in that: the ethylene glycol steamed in described flow process B is used while being incubated the useless polyester alcoholysis of after storage, staying other batches.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11131043A (en) * | 1997-10-29 | 1999-05-18 | Asahi Chem Ind Co Ltd | Flame resistant polyester-based hot melt adhesive composition |
| CN101126006A (en) * | 2007-06-29 | 2008-02-20 | 上海天洋热熔胶有限公司 | Method for preparing polyester thermosol |
| CN101434821A (en) * | 2007-11-16 | 2009-05-20 | 比亚迪股份有限公司 | Method for preparing hot-melt adhesive from polyester waste material |
| CN101591519A (en) * | 2009-07-02 | 2009-12-02 | 陈国新 | polyether type polyester hot melt adhesive and production technique thereof |
| CN101760163A (en) * | 2010-02-08 | 2010-06-30 | 启东市鑫鑫粘合剂有限公司 | Preparation method of producing polyester hot melt adhesive based on PET waste materials |
-
2013
- 2013-08-15 CN CN2013103555638A patent/CN103450464A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11131043A (en) * | 1997-10-29 | 1999-05-18 | Asahi Chem Ind Co Ltd | Flame resistant polyester-based hot melt adhesive composition |
| CN101126006A (en) * | 2007-06-29 | 2008-02-20 | 上海天洋热熔胶有限公司 | Method for preparing polyester thermosol |
| CN101434821A (en) * | 2007-11-16 | 2009-05-20 | 比亚迪股份有限公司 | Method for preparing hot-melt adhesive from polyester waste material |
| CN101591519A (en) * | 2009-07-02 | 2009-12-02 | 陈国新 | polyether type polyester hot melt adhesive and production technique thereof |
| CN101760163A (en) * | 2010-02-08 | 2010-06-30 | 启东市鑫鑫粘合剂有限公司 | Preparation method of producing polyester hot melt adhesive based on PET waste materials |
Non-Patent Citations (1)
| Title |
|---|
| 张端: ""用涤纶下脚料生产聚酯热熔胶"", 《粘接》 * |
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Application publication date: 20131218 |