CN101024717A - Method and apparatus for containuously producing fire-retardant polyester - Google Patents
Method and apparatus for containuously producing fire-retardant polyester Download PDFInfo
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- CN101024717A CN101024717A CN 200610038511 CN200610038511A CN101024717A CN 101024717 A CN101024717 A CN 101024717A CN 200610038511 CN200610038511 CN 200610038511 CN 200610038511 A CN200610038511 A CN 200610038511A CN 101024717 A CN101024717 A CN 101024717A
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Abstract
The invention discloses a method and device to continuously produce fire resistance property polyester that includes the following steps: polyester melt passing through main pipeline inputting commixing device; taking crashing and decentralizing process to fire resistance property functionality particle with auxiliary agent in jet mill; taking commixing process to gain the fire resistance property polyester. The invention has the advantages of simple method, reasonable device structure, easy to operate, stable species, low cost, etc.
Description
Technical field:
The present invention relates to a kind of production method and equipment of fire-retardant polyester.
Background technology:
It is reported that particularly polyethylene terephthalate, Poly(Trimethylene Terephthalate) and polybutylene terephthalate owing to its machinery, physics, chemical property excellence, thereby are used widely in fiber, film and other layered products.Trevira belongs to the meltbility combustible fibre, expansion along with its Application Areas, in some special use occasion, finishing material or the used aspects such as protective clothing of special industry as aviation, public place of entertainment, family etc., then require it to reach certain fire-retardant requirement, otherwise will improve the insecurity of fire greatly.
In order to make high molecular polymer possess non-flame properties, just need carry out fire-retardantization to it.At present macromolecular material is carried out fire-retardantization two kinds of methods are roughly arranged: a kind of is that copolymerization is flame-retardant modified, is about to fire-retardant monomer with the polymer monomer copolymerization, the 2nd, and add fire retardant and carry out blending and modifying.Blending and modifying is to add the blending fire retardant agent to make fire-retardant slice or add fire retardant and the blending fire retardant fiber is made in the polyester fondant blend when spinning in the polyester slice manufacturing processed.
Blending method is very strict to the requirement of fire retardant, and the resistance toheat of fire retardant must be complementary with the processing condition of processing, and the fusing point that requires fire retardant is greater than the polyester drying temperature, and decomposition temperature is greater than prilling temperature and spinning temperature.The tiny degree of the granularity of fire retardant should conform to and make the steady quality of silk with spinning processing technology.In addition, fire retardant will have preferably with matrix and is dispersiveness and consistency.Phosphorus flame retardant is because of its good stability, Halogen, nontoxic, and flame retardant properties is stable lasting, is that other bromine systems, fire-retardant dose of commixed type are incomparable.
And have two kinds as method for making polyester: a kind of is the polymerization of still formula, and another is successive polymerization.The polymerization of still formula can be produced many kinds polyester product, but cost is than higher and polymkeric substance quality instability.For the stabilization of polymer quality that reduces production costs, More and more factories adopts the manufacture method of successive polymerization.But continuous polymerization method gained polyester kind is more single, has limited the exploitation of polyester variety diversity so greatly.
In order to obtain fire-retardant polyester, people have adopted the polyester blend technology.Existing production in the polyester blend technology, polyester is all delivered to the scene that produces blend with solid form.The production of this polyester generally occurs in apart from far place, blend production scene before described feeding, and process relates to the monomer structure unit is linked into an integrated entity with chemical bond.With solid form polyester being delivered to the blend production scene requires polyester to cool off in production equipment, randomly granulation has reached curing subsequently, and the traditional way that this kind is commonly used brings following shortcoming: cooling, described steps such as curing, granulation, storage, transportation and fusion, with high costs, formality is various.Moreover desired energy consumption must cause the influence to environment.Happy and harmonious formation this polyester at high temperature the additional exposure of blend components in mixing facilities, this can cause degraded and the therefore deterioration of the blend quality of production.This is especially serious for the thermo-sensitivity polyester.At last, the polyester that the blend production scene is used carries out drying and may prove necessary before fusion, if any moisture that transportation and storage period are absorbed all can cause the polyester in the melt to degrade.
Summary of the invention:
The object of the present invention is to provide that a kind of method is simple, easy to operate, the method and apparatus of the measured fire-retardant polyester of continuous production matter.
Technical solution of the present invention is:
A kind of method of continuous production fire-retardant polyester is characterized in that: comprise the following steps:
1. the polyester fondant that aggregates in the polymerization unit is imported the co-blended device by main pipe line;
2. the flame retardant resistance functional particles is added dispersion agent earlier and in air-flow powder pulverizer, pulverize and dispersion treatment, mix in mixing tank with polyester then;
3. the mixture that 2. step obtained adds in the co-blended device of step in 1. blend to be handled, fire-retardant polyester.
The polyester of step in 2. is directly to add the polyester slice in the mixing tank or enter molten state polyester the mixing tank from polymerization unit through arm.
The raw material consumption of polyester, flame retardant resistance functional particles and three kinds of components of auxiliary agent is by weight percentage: polyester 48%～99.4%, flame retardant resistance functional particles 0.2%～50%, dispersion agent 0.1%～5%.Polyester is polyethylene terephthalate, Poly(Trimethylene Terephthalate) or polybutylene terephthalate.Dispersion agent is polyoxyethylene glycol, trimethylolethane, Metallic stearates, polyvinylpyrrolidone or aluminium titanium compound coupling agent.2. in the mixing tank, also being added with oxidation inhibitor in step, is Hinered phenols antioxidant (as oxidation inhibitor IR1010, antioxidant 1076) and phosphite ester kind antioxidant (as oxidation inhibitor TNP, 168), and the consumption of oxidation inhibitor is 0.01～0.5% of a polyester gross weight.
The flame retardant resistance functional particles is a phosphorus flame retardant, is 2-propyloic benzenephosphonic acid, 2-carboxyethyl methylphosphinate phosphoric acid ester or 2-carboxyethyl methylphosphinate phosphoric acid, and its corresponding structural formula is respectively
Preferred 2-propyloic benzenephosphonic acid (Jinan three is the ST of fire-retardant product company limited copolymerization fire retardant too).
The molten state polyester is a poly terephthalic acid alkane diol ester, molten preferred poly terephthalic acid alkane diol ester,, polybutylene terephthalate or poly terephthalic acid 1, ammediol ester, especially preferred polyethylene terephthalate.The temperature of molten state polyester is 220～320 ℃.The mixing tank of flame retardant resistance functional particles and polyester is the screw mixing tank.The mixing tank of co-blended device and flame retardant resistance functional particles and polyester, their mixinglength is 20～60:1 with the ratio that mixes diameter.
A kind of equipment of continuous production fire-retardant polyester is characterized in that: have the little processing units of particle to be connected with mixing tank, mixing tank is connected with the co-blended device, and mixing tank is connected with continuous polymerization device by main pipe line.
Mixing tank is connected with continuous polymerization device by arm.There is unnecessary polyester output tube to be connected with the person in charge.The mixing tank of functional particles and polyester is the screw mixing tank.The mixing tank of co-blended device and functional particles and polyester, their mixinglength is 20～60: 1 with the ratio that mixes diameter.
The inventive method is simple, and device structure is reasonable, and is easy to operate, and fire retardant disperses homogeneous, stable variety, and the polyester quality of production is good, and production cost is low.
Description of drawings:
The invention will be further described below in conjunction with drawings and Examples.
Fig. 1 is the device structure diagrammatic sketch of the embodiment of the invention 1～7.
Fig. 2 is the device structure diagrammatic sketch of the embodiment of the invention 8.
Fig. 3 is the device structure diagrammatic sketch of the embodiment of the invention 9.
Embodiment:
Embodiment 1
With terephthalic acid and ethylene glycol is that raw material carries out esterification under 200～260 ℃ of temperature, then 280～300 ℃ of temperature, be lower than and carry out heavily polycondensation under the 300Pa vacuum, continuous production viscosity reaches 0.655 polyethylene terephthalate and (is abbreviated as: PET) (or Poly(Trimethylene Terephthalate) or polybutylene terephthalate) melt.Polyethylene terephthalate melt in the continuous polymerization device 1 is under 220～300 ℃ (220 ℃, 240 ℃, 280 ℃, 300 ℃ of examples) in temperature, import co-blended devices 3 with 1000Kg/h speed by main pipe line 2, arm 4 is imported screw mixing tank 5 with polyethylene terephthalate simultaneously, and feed rate is 5kg/h; ST fire retardant (functional particles) is that the fire-retardant powder of 2-propyloic benzenephosphonic acid (or 2-carboxyethyl methylphosphinate phosphoric acid ester, 2-carboxyethyl methylphosphinate phosphoric acid) adds dispersion agent polyoxyethylene glycol (or trimethylolethane or Metallic stearates or polyvinylpyrrolidone or aluminium titanium compound coupling agent) earlier and pulverizes and dispersion treatment in flat air-flow powder pulverizer 12, join then in the screw mixing tank 5 and mix, feed rate is 5kg/h.Mixture further enters blend processing in the co-blended device 3, gets fire-retardant polyester.Blending temperature in the co-blended device 3 is 280 ℃.The ST fire retardant is that the fire-retardant powder of 2-propyloic benzenephosphonic acid content in making the flame retardance poly ethylene glycol terephthalate is 0.5%.The consumption of dispersion agent is 0.1～5% of polyester, fire-retardant powder and three kinds of total consumptions of raw material of dispersion agent.Adopt common spinning-drawing machine to carry out conventional spinning then and draft process is made fire-retardant fibre.The fiber limiting oxygen index(LOI) is 29.The screw mixing tank 5 of above-mentioned co-blended device 3 and flame retardant resistance powder and polyester, their mixinglength is 20～60 with the ratio that mixes diameter: 1, wherein diameter is 20～100 centimetres.
The preparation technology of embodiment 2～6 is as embodiment 1.Its test-results is as follows:
| Test No. | PET feed rate (kg/h) | Arm PET feed rate contains | The fire-retardant powder of 2-propyloic benzenephosphonic acid supplies | The fire-retardant powder of 2-propyloic benzenephosphonic acid contains | Limiting oxygen index(LOI) LOI | Breaking tenacity (cN/dtex) |
| Amount (kg/h) | Give amount (kg/h) | Amount (wt%) | ||||
| Embodiment 1 | 1000 | 5 | 5 | 0.5 | 29 | 3.8 |
| Embodiment 2 | 1000 | 12 | 12 | 1.2 | 30 | 3.6 |
| Embodiment 3 | 1000 | 42 | 42 | 4 | 31 | 3.3 |
| Embodiment 4 | 1000 | 87 | 87 | 8 | 32 | 3.1 |
| Embodiment 5 | 1000 | 136 | 136 | 12 | 32 | 3.0 |
| Embodiment 6 | 1000 | 176 | 176 | 15 | 33 | 2.7 |
Embodiment 7
With terephthalic acid and ethylene glycol is that raw material carries out esterification under 200～260 ℃ of temperature, then 280～300 ℃ of temperature, be lower than and carry out heavily polycondensation under the 300Pa vacuum, continuous production viscosity reaches 0.655 polyethylene terephthalate and (is abbreviated as: PET) melt.Polyethylene terephthalate melt in the continuous polymerization device 1 is under 220～300 ℃ (220 ℃, 240 ℃, 280 ℃, 300 ℃ of examples) in temperature, import co-blended devices 3 with 1000kg/h speed by main pipe line 2, arm 4 is imported screw mixing tank 5 with polyethylene terephthalate simultaneously, and feed rate is 5kg/h; The ST fire retardant is that the fire-retardant powder elder generation's adding dispersion agent polyoxyethylene glycol of 2-propyloic benzenephosphonic acid (or trimethylolethane or Metallic stearates or polyvinylpyrrolidone or aluminium titanium compound coupling agent) is pulverized and dispersion treatment in flat air-flow powder pulverizer 12, with join in the screw mixing tank 5 after oxidation inhibitor IR1010 (or antioxidant 1076, oxidation inhibitor TNP, 168) mixes, feed rate is 5kg/h.Mixture further enters blend processing in the co-blended device 3, gets fire-retardant polyester.Blending temperature in the co-blended device 3 is 280 ℃.The ST fire retardant is that the fire-retardant powder of 2-propyloic benzenephosphonic acid content in making the flame retardance poly ethylene glycol terephthalate is 0.5%.Oxidation inhibitor IR1010 consumption is 0.01～0.5% of a polyester gross weight.The consumption of dispersion agent is 0.1～5% of polyester, fire-retardant powder and three kinds of total consumptions of raw material of dispersion agent.Adopt common spinning-drawing machine to carry out conventional spinning then and draft process is made fire-retardant fibre.The fiber limiting oxygen index(LOI) is 29.The screw mixing tank 5 of above-mentioned co-blended device 3 and flame retardant resistance powder and polyester, their mixinglength is 20～60 with the ratio that mixes diameter, and wherein diameter is 20～100 centimetres.
Embodiment 8
With terephthalic acid and ethylene glycol is that raw material carries out esterification under 200～260 ℃ of temperature, then 280～300 ℃ of temperature, be lower than and carry out heavily polycondensation under the 300Pa vacuum, continuous production viscosity reaches 0.655 polyethylene terephthalate and (is abbreviated as: PET) melt.Polyethylene terephthalate melt in the continuous polymerization device 6 is under 220～300 ℃ (220 ℃, 240 ℃, 280 ℃, 300 ℃ of examples) in temperature, import co-blended devices 8 with 1000kg/h speed by main pipe line 7, with polyethylene terephthalate section input screw mixing tank 9, feed rate is 5kg/h simultaneously; The ST fire retardant is that the fire-retardant powder elder generation's adding dispersion agent polyoxyethylene glycol of 2-propyloic benzenephosphonic acid (or trimethylolethane or Metallic stearates or polyvinylpyrrolidone or aluminium titanium compound coupling agent) is pulverized and dispersion treatment in flat air-flow powder pulverizer 13, join then in the screw mixing tank 9, feed rate is 5kg/h.Mixture further enters blend processing in the co-blended device 8, gets fire-retardant polyester.Blending temperature in the co-blended device 8 is 280 ℃.The ST fire retardant is that the fire-retardant powder of 2-propyloic benzenephosphonic acid content in making the flame retardance poly ethylene glycol terephthalate is 0.5%.The consumption of dispersion agent is 0.1～5% of polyester, fire-retardant powder and three kinds of total consumptions of raw material of dispersion agent.Adopt common spinning-drawing machine to carry out conventional spinning then and draft process is made fire-retardant fibre.The fiber limiting oxygen index(LOI) is 29.The screw mixing tank 9 of above-mentioned co-blended device 8 and flame retardant resistance powder and polyester, their mixinglength is 20～60 with the ratio that mixes diameter, and wherein diameter is 20～100 centimetres.
Embodiment 9:
Have unnecessary polyester output tube 10,11 to be connected with the person in charge, all the other are with embodiment 1.The unnecessary polyester that these distribute can be directly used in spinning, film forming processing or make polyester slice.
Embodiment 10:
The total consumption of raw material of polyester, flame retardant resistance powder and three kinds of components of dispersion agent is polyester 48%～99.4% (example 48%, 70%, 99%) by weight, flame retardant resistance functional particles 0.2%～50% (example 50%, 29%, 0.2%), dispersion agent 0.1%～2% (example 2%, 1%, 0.3%).All the other are with embodiment 1.
Comparative example 1
Still formula polymeric viscosity is 0.655 polyethylene terephthalate section and the fire-retardant powder of ST at L/D is 2 forcing machine blend manufacturing master batches of 44, and blending temperature is 280 ℃.The weight part of the fire-retardant powder of ST is 50% in the master batch.Master batch and above-mentioned polyethylene terephthalate section mix manufacturing section particle once more under above-mentioned condition then, and the weight part of the fire-retardant powder of ST is 4% in this section particle.Adopt common spinning-drawing machine to carry out conventional spinning then and draft process is made fiber.The limiting oxygen index(LOI) 26～30 of fiber, breaking tenacity 3.0～3.4 cN/dtex.
Comparative example 2
Still formula polymeric viscosity is 0.655 polyethylene terephthalate section and the fire-retardant powder of ST at L/D is 2 forcing machine blend manufacturing master batches of 44, and blending temperature is 280 ℃.The weight part of the fire-retardant powder of ST is 50% in the master batch.Master batch and above-mentioned polyethylene terephthalate section mix manufacturing section particle once more under above-mentioned condition then, and the weight part of the fire-retardant powder of ST is 18% in this section particle.Adopt common spinning-drawing machine to carry out conventional spinning then and draft process is made fiber.The limiting oxygen index(LOI) 27～31 of fiber, breaking tenacity 2.9～3.2cN/dtex.
Comparative example 3
The viscosity of successive polymerization is 0.655 polyethylene terephthalate section and the fire-retardant powder of ST at L/D is 2 forcing machine blend manufacturing master batches of 44, and blending temperature is 280 ℃.The weight part of the fire-retardant powder of ST is 50% in the master batch.Master batch and above-mentioned polyethylene terephthalate section mix manufacturing section particle once more under above-mentioned condition then, and the weight part of the fire-retardant powder of ST is 4% in this section particle.Adopt common spinning-drawing machine to carry out conventional spinning then and draft process is made fiber.The limiting oxygen index(LOI) 31～32 of fiber, breaking tenacity 3.8cN/dtex.
Comparative example 4
The viscosity of successive polymerization is 0.655 polyethylene terephthalate section and the fire-retardant powder of ST at L/D is 2 forcing machine blend manufacturing master batches of 44, and blending temperature is 280 ℃.The weight part of the fire-retardant powder of ST is 50% in the master batch.Master batch and above-mentioned polyethylene terephthalate section mix manufacturing section particle once more under above-mentioned condition then, and the weight part of the fire-retardant powder of ST is 18% in this section particle.Adopt common spinning-drawing machine to carry out conventional spinning then and draft process is made fiber.The limiting oxygen index(LOI) 32 of fiber, breaking tenacity 3.5cN/dtex.
Testing method
The testing method of limiting oxygen index(LOI) is according to GB5454-1997, and this standard is non-adopting by equivalent international standard ISO4589:1984
The breaking tenacity testing method is according to GB/T3923.2-1998 textile fabric tensile property part 2: the mensuration grab method of ultimate strength.
Claims (9)
1, a kind of method of continuous production fire-retardant polyester is characterized in that: comprise the following steps:
1. the polyester fondant that aggregates in the polymerization unit is imported the co-blended device by main pipe line;
2. the flame retardant resistance functional particles is added dispersion agent earlier and in air-flow powder pulverizer, pulverize and dispersion treatment, mix in mixing tank with polyester then;
3. the mixture that 2. step obtained adds in the co-blended device of step in 1. blend to be handled, fire-retardant polyester.
2, the method for continuous production fire-retardant polyester according to claim 1 is characterized in that: the polyester of step in 2. is directly to add the polyester slice in the mixing tank or enter molten state polyester the mixing tank from polymerization unit through arm.
3, the method for continuous production fire-retardant polyester according to claim 1 and 2, it is characterized in that: the raw material consumption of polyester, flame retardant resistance functional particles and three kinds of components of dispersion agent is by weight percentage: polyester 48%～99.4%, flame retardant resistance functional particles 0.2%～50%, dispersion agent 0.1%～5%; Polyester is polyethylene terephthalate, Poly(Trimethylene Terephthalate) or polybutylene terephthalate; Dispersion agent is polyoxyethylene glycol, trimethylolethane, Metallic stearates, polyvinylpyrrolidone or aluminium titanium compound coupling agent.
4, the method for continuous production fire-retardant polyester according to claim 1 and 2, it is characterized in that: the flame retardant resistance functional particles is a phosphorus flame retardant, be 2-propyloic benzenephosphonic acid, 2-carboxyethyl methylphosphinate phosphoric acid ester or 2-carboxyethyl methylphosphinate phosphoric acid, its corresponding structural formula is respectively
5, a kind of equipment of continuous production fire-retardant polyester is characterized in that: have the little processing units of particle to be connected with mixing tank, mixing tank is connected with the co-blended device, and mixing tank is connected with continuous polymerization device by main pipe line.
6, the equipment of continuous production fire-retardant polyester according to claim 5 is characterized in that: mixing tank is connected with continuous polymerization device by arm.
7, according to the equipment of claim 5 or 6 described continuous production fire-retardant polyesters, it is characterized in that: have unnecessary polyester output tube to be connected with the person in charge.
8, according to the equipment of claim 5 or 6 described continuous production fire-retardant polyesters, it is characterized in that: the mixing tank of functional particles and polyester is the screw mixing tank.
9, according to the equipment of claim 5 or 6 described continuous production fire-retardant polyesters, it is characterized in that: the mixing tank of co-blended device and functional particles and polyester, their mixinglength is 20～60: 1 with the ratio that mixes diameter.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 200610038511 CN101024717A (en) | 2006-02-23 | 2006-02-23 | Method and apparatus for containuously producing fire-retardant polyester |
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| CN 200610038511 CN101024717A (en) | 2006-02-23 | 2006-02-23 | Method and apparatus for containuously producing fire-retardant polyester |
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| CN101024717A true CN101024717A (en) | 2007-08-29 |
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| CN 200610038511 Pending CN101024717A (en) | 2006-02-23 | 2006-02-23 | Method and apparatus for containuously producing fire-retardant polyester |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103132174A (en) * | 2011-11-29 | 2013-06-05 | 东丽纤维研究所（中国）有限公司 | Normal temperature and pressure disperse dyeable modified polyester fiber |
| CN109208099A (en) * | 2018-07-04 | 2019-01-15 | 钟定怡 | Polyester flame-retardant additive process equipment |
-
2006
- 2006-02-23 CN CN 200610038511 patent/CN101024717A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103132174A (en) * | 2011-11-29 | 2013-06-05 | 东丽纤维研究所（中国）有限公司 | Normal temperature and pressure disperse dyeable modified polyester fiber |
| CN109208099A (en) * | 2018-07-04 | 2019-01-15 | 钟定怡 | Polyester flame-retardant additive process equipment |
| CN109208099B (en) * | 2018-07-04 | 2020-12-08 | 四川华顺海天化纤有限责任公司 | Polyester flame retardant additive processing equipment |
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