CN101792526B - Method and device for drying polymer - Google Patents
Method and device for drying polymer Download PDFInfo
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- CN101792526B CN101792526B CN 200910238293 CN200910238293A CN101792526B CN 101792526 B CN101792526 B CN 101792526B CN 200910238293 CN200910238293 CN 200910238293 CN 200910238293 A CN200910238293 A CN 200910238293A CN 101792526 B CN101792526 B CN 101792526B
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Abstract
The invention relates to a method and a device for drying a polymer, which are used for drying removal of an organic solvent contained in the polymer obtained through oxidative coupling. The method and the device use a high-temperature circulating inert gas to dry the polymer sectionally heated by gradient temperatures and uses a low-pressure circulating inert gas to accelerate the dried polymer to enter a storage bin. The method and the device for drying the polymer not only can avoid dust explosions and simultaneously solve the problem of pipeline blockage caused by bridge formation of powder particles of the polymer, but also have the advantages of low production cost, relatively simple process, less equipment investment and easy continuous production.
Description
Technical field
The drying means and the device of the polymer powder that the present invention relates to obtain through oxidative coupling.Relate in particular to and adopt drying machine and incorporate the intravital organic solvent of the dry ppe powder of circulating nitrogen gas, and be pressurized in the rotation lock, make the ppe powder can flow to feed bin smoothly, prevent the method that ppe is built bridge effectively through circulating nitrogen gas.
Background technology
The oxidative coupling method is meant the compound that has reactive hydrogen in the following oxidizing reaction of the effect of oxide catalyst, and dehydrogenation and coupling form the method for polymkeric substance, claim the dehydrogenation polycondensation again.Compounds such as phenols, acetylene class, arylamine class, aromatic hydrocarbons, thio-alcohol all can generate polymkeric substance through oxidative coupling polymerization.Wherein, the most representative oxidative coupling preparation that belongs to ppe.
Ppe gets application widely owing to having good chemistry, physics and chemical property.The polyphenylene oxide resin that is made by the method for ppe through modification has chemical resistant properties, high thermal resistance, HS, shrinking percentage is low and over-all properties such as high workability; It is through melt injection molding or melt extrude product and the parts that method such as the method for forming provides required shape, therefore can be applied to the material of electric, automobile industry and other Industrial materials field products or parts widely.
The working method of ppe is included under the existence of copper compound, amine compound and oxygen-containing gas, the oxidized coupling of at least a unit price phenol in the good solvent of ppe and obtaining.About separating out the method for ppe the ppe solution that obtains from above-mentioned oxidative coupling method, comprise through the poor solvent such as the methyl alcohol that in above-mentioned solution, add ppe and separate out ppe.Ppe is through washing, and after the filtration, the ppe that contains a certain amount of organic solvent will carry out drying treatment.
At present, the method that the drying that is used for ppe production removes organic solvent is a lot, generally includes (1) twin screw vacuum exhaust forcing machine; Be that polymkeric substance is directly entered into forcing machine after filtering, deviate from organic solvent in the time of melt pelletization, like United States Patent(USP) No. 6365710B1; No.5232649; No.3742093, No.4504338, No.5102591 etc. disclose ppe exsiccant method.These methods all are will be with the dry ppe of ppe fusion; The equipment that this method needs is special; The easy oxidation stain of ppe after the fusion, and the melt temperature of ppe is higher, needs high temperature to extrude; Can adopt twin screw vacuum exhaust forcing machine if obtain Noryl, but will wait until that the former powder this method of ppe is unworkable.(2) spraying drying liberation method utilizes the disclosed method that obtains polycarbonate of the public clear 63-1333 of Japanese Patent Laid, but this method apparatus expensive, the gained resin particle is too meticulous, and bulk density is little, for post-treatment is made troubles.
Summary of the invention
In view of the foregoing, the object of the invention is to provide a kind of production cost low, and technology is simple relatively, and facility investment is few, is easy to quantity-produced, the polymer powder drying means and the device that obtain through oxidative coupling.
And the present invention utilizes circulated inert gas dry polymer powder, not only can avoid dust explosion, through giving the pressurization of rotation lock, solves the problem that the polymer powder particle causes the bridge formation blocking pipe simultaneously.
The present invention provides a kind of drying means of polymer powder, is used for the dry contained organic solvent of polymkeric substance that obtains through oxidative coupling of removing, and it is characterized in that, utilizes the high temperature circulation rare gas element that the said polymkeric substance of gradient temperature zone heating is carried out drying.
In the above-mentioned drying of polymers of the present invention, the loop direction of said high temperature circulation rare gas element and said polymer transport in the opposite direction.
In the above-mentioned drying of polymers of the present invention; Said gradient temperature zone heating can be two sections or three sections heating, and more multistage is also accepted, preferred three sections heating; Throughput direction by polymkeric substance is followed successively by; One section is heated 170 ℃-190 ℃, and two sections are heated 110 ℃-130 ℃, and three sections are heated 80 ℃-100 ℃.
In the above-mentioned drying of polymers of the present invention, said rare gas element is preferably nitrogen.Said high temperature inert gas temperature is preferably 150 ℃-200 ℃, most preferably 170 ℃-190 ℃.
In the above-mentioned drying of polymers of the present invention, be preferably 10min-50min time of drying, most preferably be 10min-30min.
In the above-mentioned drying of polymers of the present invention, the contained organic solvent of said polymer powder is to be selected from least a in methyl alcohol, ethanol, propyl carbinol, acetone, toluene, benzene, the YLENE, particular methanol and toluene.
In the above-mentioned drying of polymers of the present invention, said polymkeric substance is preferably ppe.
Wherein, the ppe solid content of said ppe is 40%-90%, and preferred ppe solid content is 50%-70%.
In the above-mentioned drying of polymers of the present invention, this drying means carries out in a drying machine, and said drying machine comprises discharge port, is connected with a rotation lock at said discharge port, on the throughput direction of said rotation lock, is connected with the low pressure recycle rare gas element.
Wherein, said low pressure recycle rare gas element is preferably nitrogen, and its temperature is 40 ℃-100 ℃.
According to above-mentioned drying of polymers of the present invention, it has prevented effectively that through sectional temperature-controlled polymer powder receives thermooxidizing, has reduced energy consumption.Through in the circulation of said high temperature inert gas, the opposite direction that said high temperature inert gas is carried from said polymer powder gets into, and is discharged from after making it carry the intravital organic solvent of said polymer powder secretly; Through overcooling, rare gas element-organic solvent separates again, the rare gas element heating; Supercharging, thus the working cycle of realization high temperature inert gas can more effectively be carried away organic solvent secretly simultaneously; Improved drying efficiency, and owing to be the circulation of rare gas element, so can prevent that said polymkeric substance is oxidized and dust explosion takes place; Improved security and stability, practiced thrift nitrogen consumption, reduced nitrogen discharge capacity to environmental emission.And through utilizing the low pressure recycle rare gas element to quicken to get into feed bin through the exsiccant polymer powder, blocking problem makes polymer powder flow into feed bin smoothly because polymer powder is built bridge thereby solve effectively.
In addition, the present invention also provides a kind of drying installation of polymkeric substance, is used for the dry contained organic solvent of polymkeric substance that obtains through oxidative coupling of removing, and it comprises:
Drying machine, it possesses opening for feed, discharge port, is used for high temperature inert gas round-robin venting port and inlet mouth and zone heating chuck;
The rotation lock is set at said drying machine discharge port place, and is provided with the low pressure recycle rare gas element path that is used for to its pressurization.
In the drying installation of said polymkeric substance of the present invention, said drying machine, the mode that the opposite direction of carrying from said polymer powder with high temperature inert gas gets into is provided with described opening for feed, discharge port and high temperature inert gas circulation with venting port and inlet mouth.
In the drying installation of said polymkeric substance of the present invention, the said zone heating chuck and the Heating temperature of said drying machine can be provided with as required, are preferably three sections; Wherein, One section is heated 170 ℃-190 ℃, and two sections are heated 110 ℃-130 ℃, and three sections are heated 80 ℃-100 ℃.
In the drying installation of above-mentioned polymkeric substance of the present invention, the circulation of said high temperature inert gas and said low pressure recycle rare gas element path can be realized through increasing the known approaches that is provided with as required separately.The circulation of said high temperature inert gas for example realizes through following known approaches: pressurization enters into the drying machine inlet mouth through blower fan by the high temperature inert gas of interchanger heating; In drying machine, carry organic solvent secretly; Come out from the drying machine venting port, separate through entering into knockout drum after the interchanger cooling, rare gas element comes out from the separating tank top; Process interchanger heating cycle once more gets into drying machine, and rare gas element is mended the loss of pipe with suitable replenishment cycles nitrogen.For example realize through following known approaches said low-pressure inert gas circulation path: the low pressure recycle rare gas element gives the rotation lock suitable pressurization; After quickening polymer powder entering feed bin; Come out from material top, cabin again; Isolate solid particulate through gas-solid separator and reclaim, and low-pressure inert gas realizes circulation through blower fan again.Low-pressure inert gas is replenished mouthful rare gas element of suitable replenish loss.In the circulation of said high temperature inert gas, said high temperature inert gas is to get into from the opposite direction that said polymer powder is carried.Wherein, the temperature of said rare gas element is preferably 150 ℃-200 ℃, most preferably 170 ℃-190 ℃.In the said low-pressure inert gas circulation path, the temperature of low pressure recycle rare gas element is preferably 40 ℃-100 ℃, most preferably is 50 ℃-70 ℃.Said rare gas element is preferably nitrogen.
In the drying installation of above-mentioned polymkeric substance of the present invention, not having special restriction for the device of convey materials, can be and the independent puopulsion unit of said drying machine also can be hollow paddle type thruster or the spiral propeller with the drying machine one.Wherein, preferred hollow paddle type thruster.
In the drying installation of above-mentioned polymkeric substance of the present invention, the contained organic solvent of said polymer powder is to be selected from least a in methyl alcohol, ethanol, propyl carbinol, acetone, toluene, benzene, the YLENE, particular methanol and toluene.
In the drying installation of above-mentioned polymer powder of the present invention, said polymkeric substance is preferably ppe.
Wherein, the ppe solid content of said ppe is 40%-90%, and preferred ppe solid content is 50%-70%.
According to the drying installation of above-mentioned polymkeric substance of the present invention, it comes sectional temperature-controlled through the zone heating chuck that said drying machine possessed, thereby has prevented that effectively polymer powder receives thermooxidizing, has reduced energy consumption.Through in drying machine, being provided for the circulation that high temperature inert gas round-robin venting port and inlet mouth carry out high temperature inert gas, and described opening for feed, discharge opening and high temperature inert gas circulation are set with venting port and inlet mouth through the mode that the opposite direction of carrying from said polymer powder with high temperature inert gas gets into, thus the opposite direction entering that said high temperature inert gas is carried from said polymer powder; Be discharged from after making it carry the intravital organic solvent of said polymer powder secretly, again through overcooling, rare gas element-organic solvent separates; The rare gas element heating; Supercharging, thus the working cycle of realization high temperature inert gas can more effectively be carried away organic solvent secretly simultaneously; Improved drying efficiency; And,, security and stability have been improved so can prevent that said polymkeric substance is oxidized and dust explosion takes place owing to be the circulation of rare gas element; Practiced thrift nitrogen consumption, reduced nitrogen discharge capacity to environmental emission.And through the rotation lock is set at said drying machine discharge opening place; Utilize low pressure recycle rare gas element path to pressurize to it; Thereby quicken to get into feed bin through the exsiccant polymer powder, blocking problem makes polymer powder flow into feed bin smoothly because polymer powder is built bridge in solution effectively.In addition, the drying installation of above-mentioned polymer powder of the present invention is because of need not specific installation, and technology is simple relatively, so facility investment is few, is easy to continuous mass production.
Description of drawings
Fig. 1 is the synoptic diagram of drying installation embodiment of the present invention.
Wherein:
1: wormpropeller; 2: drying machine; 3: the rotation lock; 4: feed bin; 5: interchanger; 6: knockout drum; 7: well heater; 8: high temperature circulation nitrogen blower fan; 9: the gas solid separation jar; 10: low pressure recycle nitrogen blower fan;
A: drying machine opening for feed; B: silo discharge port; C: knockout drum liquid exit; D: gas solid separation jar solid outlet; E: drying machine venting port; F: drying machine inlet mouth; G: drying machine discharge port; H1: three sections heating; H2: two sections heating; H3: one section heating; N1: high temperature circulation nitrogen replenishes; N2: low-pressure nitrogen replenishes; M: motor.
Embodiment
Following examples are used to explain the present invention, but are not used for limiting scope of the present invention.
Embodiment 1
As shown in Figure 1, will pass through washing, the solid content that contains after the filtration is 60%; Contain 40% methyl alcohol, the ppe of toluene promotes ppe through wormpropeller 1 and enters into drying machine 2 from drying machine opening for feed A, and wherein the chuck of drying machine is heated to 190 ℃ through 1 section heating H3 in advance; Two sections heating H2 are heated to 130 ℃, and three sections heating H1 are heated to 100 ℃, when ppe is pushed ahead by the hollow paddle type thruster; High temperature circulation nitrogen is heated to 180 ℃ through interchanger 7 simultaneously; 8 pressurizations enter into drying machine F mouth through blower fan again, and circulating nitrogen gas is carried organic solvent methanol secretly in drying machine, and toluene comes out from drying machine venting port E; Separate through entering into knockout drum 6 after interchanger 5 coolings; Nitrogen comes out from the separating tank top, and process interchanger 7 heating cycle once more gets into drying machine, and nitrogen is mended the suitable replenishment cycles nitrogen loss of pipe N1.The liquids recovery of separating from knockout drum.Ppe enters into feed bin 4 from drying machine discharge port G outflow through rotation lock 3 behind the residence time 30min in drying machine; This moment, low pressure recycle nitrogen gave rotation lock 3 suitable pressurization; Quickened ppe and got into feed bin, solved the bridge formation blocking problem, come out from material top, cabin; Low-pressure nitrogen is isolated solid particulate through gas-solid separator 9 and is reclaimed, and low-pressure nitrogen is realized the circulation of low-pressure nitrogen again through blower fan 10.Low-pressure nitrogen replenishes the nitrogen of the suitable replenish loss of mouthful N2.Behind the feed bin sampling analysis, the ppe solid content is 98.2%.
Embodiment 2
As shown in Figure 1, will pass through washing, the solid content that contains after the filtration is 60%; Contain 40% methyl alcohol, the ppe of toluene promotes ppe through wormpropeller 1 and enters into drying machine 2 from drying machine opening for feed A, and wherein the chuck of drying machine is heated to 190 ℃ through 1 section heating H3 in advance; Two sections heating H2 are heated to 130 ℃, and three sections heating H1 are heated to 100 ℃, when ppe is pushed ahead by spiral thruster; High temperature circulation nitrogen is heated to 180 ℃ through interchanger 7 simultaneously; 8 pressurizations enter into drying machine F mouth through blower fan again, and circulating nitrogen gas is carried organic solvent methanol secretly in drying machine, and toluene comes out from drying machine venting port E; Separate through entering into knockout drum 6 after interchanger 5 coolings; Nitrogen comes out from the separating tank top, and process interchanger 7 heating cycle once more gets into drying machine, and nitrogen is mended the loss of the suitable replenishment cycles nitrogen of pipe N1.The liquids recovery of separating from knockout drum.Ppe flows out the back from drying machine discharge port G behind the residence time 30min and enters into feed bin 4 through rotation lock 3 in drying machine; This moment, low pressure recycle nitrogen gave the rotation lock suitable pressurization; Quickened ppe and got into feed bin, solved the bridge formation blocking problem, come out from material top, cabin; Low-pressure nitrogen is isolated solid particulate through gas-solid separator 9 and is reclaimed, and low-pressure nitrogen is realized the circulation of low-pressure nitrogen once more through blower fan 10.Low-pressure nitrogen replenishes the nitrogen of the suitable replenish loss of mouthful N2.Behind the feed bin sampling analysis, the ppe solid content is 97.5%.
Embodiment 3
As shown in Figure 1, will pass through washing, the solid content that contains after the filtration is 70%; Contain 30% methyl alcohol, the ppe of toluene promotes ppe through wormpropeller 1 and enters into drying machine 2 from drying machine opening for feed A, and wherein the chuck of drying machine is heated to 190 ℃ through 1 section heating H3 in advance; Two sections heating H2 are heated to 120 ℃, and three sections heating H1 are heated to 90 ℃, when ppe is pushed ahead by the hollow paddle type thruster; High temperature circulation nitrogen is heated to 170 ℃ through interchanger 7 simultaneously; 8 pressurizations enter into drying machine F mouth through blower fan again, and circulating nitrogen gas is carried organic solvent methanol secretly in drying machine, and toluene comes out from drying machine venting port E; Separate through entering into knockout drum 6 after interchanger 5 coolings; Nitrogen comes out from the separating tank top, and process interchanger 7 heating cycle once more gets into drying machine, and nitrogen is mended the loss of the suitable replenishment cycles nitrogen of pipe N1.The liquids recovery of separating from knockout drum.Ppe flows out the back from drying machine discharge port G behind the residence time 20min and enters into feed bin 4 through rotation lock 3 in drying machine; This moment, low pressure recycle nitrogen gave the rotation lock suitable pressurization; Quickened ppe and got into feed bin, solved the bridge formation blocking problem, come out from material top, cabin; Low-pressure nitrogen is isolated solid particulate through gas-solid separator 9 and is reclaimed, and low-pressure nitrogen is realized the circulation of low-pressure nitrogen once more through blower fan 10.Low-pressure nitrogen replenishes the nitrogen of the suitable replenish loss of mouthful N2.Behind the feed bin sampling analysis, the ppe solid content is 98.9%.
Embodiment 4
As shown in Figure 1, will pass through washing, the solid content that contains after the filtration is 50%; Contain 50% methyl alcohol, the ppe of toluene promotes ppe through wormpropeller 1 and enters into drying machine 2 from drying machine opening for feed A, and wherein the chuck of drying machine is heated to 190 ℃ through 1 section heating H3 in advance; Two sections heating H2 are heated to 130 ℃, and three sections heating H1 are heated to 100 ℃, when ppe is pushed ahead by the hollow paddle type thruster; High temperature circulation nitrogen is heated to 180 ℃ through interchanger 7 simultaneously; 8 pressurizations enter into drying machine F mouth through blower fan again, and circulating nitrogen gas is carried organic solvent methanol secretly in drying machine, and toluene comes out from drying machine venting port E; Separate through entering into knockout drum 6 after interchanger 5 coolings; Nitrogen comes out from the separating tank top, and process interchanger 7 heating cycle once more gets into drying machine, and nitrogen is mended the loss of the suitable replenishment cycles nitrogen of pipe N1.The liquids recovery of separating from knockout drum.Ppe flows out the back from drying machine discharge port G behind the residence time 40min and enters into feed bin 4 through rotation lock 3 in drying machine; This moment, low pressure recycle nitrogen gave the rotation lock suitable pressurization; Quickened ppe and got into feed bin, solved the bridge formation blocking problem, come out from material top, cabin; Low-pressure nitrogen is isolated solid particulate through gas-solid separator 9 and is reclaimed, and low-pressure nitrogen is realized the circulation of low-pressure nitrogen again through blower fan 10.Low-pressure nitrogen replenishes the nitrogen of the suitable replenish loss of mouthful N2.Behind the feed bin sampling analysis, the ppe solid content is 99.0%.
Embodiment 5
As shown in Figure 1, will pass through washing, the solid content that contains after the filtration is 60%; Contain 40% methyl alcohol, the ppe of toluene promotes ppe through wormpropeller 1 and enters into drying machine 2 from drying machine opening for feed A, and wherein the chuck of drying machine is heated to 190 ℃ through 1 section heating H3 in advance; Two sections heating H2 are heated to 130 ℃, and three sections heating H1 are heated to 100 ℃, when ppe is pushed ahead by the hollow paddle type thruster; High temperature circulation nitrogen is heated to 180 ℃ through interchanger 7 simultaneously; 8 pressurizations enter into drying machine F mouth through blower fan again, and circulating nitrogen gas is carried organic solvent methanol secretly in drying machine, and toluene comes out from drying machine venting port E; Separate through entering into knockout drum 6 after interchanger 5 coolings; Nitrogen comes out from the separating tank top, and process interchanger 7 heating cycle once more gets into drying machine, and nitrogen is mended the loss of the suitable replenishment cycles nitrogen of pipe N1.The liquids recovery of separating from knockout drum.Ppe flows out the back from drying machine discharge port G behind the residence time 40min and enters into feed bin 4 through rotation lock 3 in drying machine; This moment, low pressure recycle nitrogen gave the rotation lock suitable pressurization; Quickened ppe and got into feed bin, solved the bridge formation blocking problem, come out from material top, cabin; Low-pressure nitrogen is isolated solid particulate through gas-solid separator 9 and is reclaimed, and low-pressure nitrogen is realized the circulation of low-pressure nitrogen again through blower fan 10.Low-pressure nitrogen replenishes the nitrogen of the suitable replenish loss of mouthful N2.Behind the feed bin sampling analysis, the ppe solid content is 99.3%.
Method of the present invention is applicable to the ppe that multiple preparation method makes, like USP 3 for the not restriction of preparation ppe method; 306,874 and 3,306; Method described in 875, the title complex that uses cuprous compound and amine compound as catalyzer with 2, the oxypolymerization of 6-xylenol; USP 3,257,357 and 3; 257,358 and the disclosed method for preparing ppe such as Japanese Patent JP50-051187A also be suitable for method of the present invention and utilize circulating nitrogen gas to remove the organic solvent in the ppe.
Claims (6)
1. a polymer dry drying method is used for the dry contained organic solvent of polymkeric substance that obtains through oxidative coupling of removing, and it is characterized in that, utilizes the high temperature circulation rare gas element that the said polymkeric substance of gradient temperature zone heating is carried out drying; The loop direction of said high temperature circulation rare gas element and said polymer transport are in the opposite direction;
Said gradient temperature zone heating is three sections heating, is followed successively by 170 ℃-190 ℃ of one section heating, 110 ℃-130 ℃ of two sections heating, 80 ℃-100 ℃ of three sections heating by the throughput direction of polymkeric substance;
Said high temperature inert gas temperature is 150 ℃-200 ℃;
Said polymkeric substance is a ppe.
2. drying of polymers as claimed in claim 1 is characterized in that, said rare gas element is a nitrogen.
3. drying of polymers as claimed in claim 1 is characterized in that, it is 10min-50min that said polymkeric substance is carried out the exsiccant time.
4. the method for claim 1 is characterized in that, this drying means carries out in a drying machine, and said drying machine comprises discharge port, is connected with a rotation lock at said discharge port, on the throughput direction of said rotation lock, is connected with the low pressure recycle rare gas element.
5. method as claimed in claim 4 is characterized in that, said low pressure recycle rare gas element is a nitrogen, and its temperature is 40 ℃-100 ℃.
6. the employed drying installation of each said polymer dry drying method of claim l-5 is used for the dry contained organic solvent of polymkeric substance that obtains through oxidative coupling of removing, and it comprises:
Drying machine, it possesses opening for feed, discharge port, is used for high temperature inert gas round-robin venting port and inlet mouth and zone heating chuck; Said drying machine, the mode that gets into from the opposite direction of said polymer transport with high temperature inert gas is provided with described opening for feed, discharge port and high temperature inert gas circulation with venting port and inlet mouth;
The rotation lock is set at said drying machine discharge port place, and is provided with the low pressure recycle rare gas element path that is used for to its pressurization.
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| CN101921394B (en) * | 2010-08-25 | 2013-05-01 | 中国蓝星（集团）股份有限公司 | Method for simultaneously drying and blocking polyphenyl ether |
| CN102229678A (en) * | 2011-05-17 | 2011-11-02 | 内蒙古阜丰生物科技有限公司 | Drying method applied to xanthan gum production |
| CN105437404B (en) * | 2014-08-13 | 2018-05-22 | 中国石油化工股份有限公司 | Prepare the system and method that superelevation glues nylon 6 slice |
| CN109490163A (en) * | 2018-10-26 | 2019-03-19 | 无锡风正科技有限公司 | A kind of air purifying filter mesh life test loading device |
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| CN1962098A (en) * | 2006-11-29 | 2007-05-16 | 宁波阿勒法管系机械制造有限公司 | Food refuse treatment device |
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| US6365710B1 (en) * | 2001-08-29 | 2002-04-02 | General Electric Company | Method for removing volatile components from solid polymeric materials |
| CN1962098A (en) * | 2006-11-29 | 2007-05-16 | 宁波阿勒法管系机械制造有限公司 | Food refuse treatment device |
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