CN102617820B - Continuous production method of thermoplastic polyurethane elastic body and special system of continuous production method - Google Patents
Continuous production method of thermoplastic polyurethane elastic body and special system of continuous production method Download PDFInfo
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- CN102617820B CN102617820B CN2012101009220A CN201210100922A CN102617820B CN 102617820 B CN102617820 B CN 102617820B CN 2012101009220 A CN2012101009220 A CN 2012101009220A CN 201210100922 A CN201210100922 A CN 201210100922A CN 102617820 B CN102617820 B CN 102617820B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/36—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
- B29C48/395—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders
Abstract
The invention discloses a continuous production method of a thermoplastic polyurethane elastic body TPU and a special system of the continuous production method, which are characterized in that an extruder and a belt reactor gradually react to synthesize the thermoplastic polyurethane elastic body; the extruder is used for finishing early-stage mixing and initial-stage reaction; the belt reactor provides post-stage reaction and crystallization; through a sectioned reaction, the material staying time can be adjusted so as to give sufficient crystallization time to the materials; and the molecular weight of the TPU can be controlled, so as to effectively eliminate a gelatinization phenomenon; and the manufactured TPU granules are uniform and have very good physical and mechanical properties.
Description
Technical field:
The present invention relates to the high molecular polymer preparing technical field, is a kind of continuous production method and dedicated system of Polyurethane Thermoplastic Elastomer specifically.
Background technology:
Polyurethane Thermoplastic Elastomer (TPU) but there is good elasticity body performance and thermoplastic processibility, be widely used in the fields such as trolley part, sealing member, medical instruments, cable, tubing, fire hose, footwear material.As in Shanxi-Prov Inst of Chemical Industry, write " the polyurethane elastomer handbook (and Chemical Industry Press, 2005, describe relevant TPU preparation, performance and application in detail in P398).
Well-known preparation technology is twin screw extruder technique, and this method is that raw material is metered into to polymerization granulation in double-screw reactor.There is following problem in traditional twin screw extruder technique: 1, this expressing technique is fairly simple, mix and react and carry out simultaneously, but the product homogeneity made by this way is poor; 2, the residence time of material in forcing machine limited, be generally less than 1 minute, make to react restive, cause product reaction not exclusively or gel occurs; 3, starting raw material temperature of reaction in reactor is higher, and easily generation is not wished and uncontrollable crosslinked allophanate secondary reaction.
In order to improve constantly the quality of TPU, meet many-sided demand, much TPU manufacturing enterprise all actively is devoted to the improvement of production technique.Bayer company produces TPU by prepolymer process in CN1281474, be mainly first by polyvalent alcohol and isocyanic ester at the tubular reactor reaction prepolymer, later stage reacts with chainextender prepolymer and generates TPU in double-screw reactor, but the later stage chain extending reaction all reacts by Couble screw rod high-temp, cause producing heterogeneity and uncontrollable secondary reaction.Because prepolymer viscosity is large, impact is measured simultaneously, complicated operation, and the cleaning difficulty, cause obtaining satisfied effect.
Germany Bayer AG has announced a kind of Polyurethane Thermoplastic Elastomer multistage continuous production technology in patent CN1289561C.This technology main process is as follows: at first the part polyvalent alcohol is mixed and generated prepolymer by static mixer with isocyanic ester, then after this prepolymer being mixed by static mixer with the residue polyvalent alcohol, through tubular reactor, react, resultant directly joins the ingress of twin screw and is reacted in twin screw with chainextender, and the most all the material extruding pelletization makes finished product TPU.The twin screw technique that this technique is more traditional can prepare the more complicated TPU of composition, but the method operating procedure very complicated is had higher requirement to actual production control aspect.Also can't avoid the generation of pyroreaction and the crosslinking reaction in later stage simultaneously.Yantai Wanhua New Material Technology Co., Ltd attempts to extend the residence time in screw rod by two rank machine in patent CN101020737, but, due to pyroreaction, causes gel more, and the product homogeneity is poor.
Current twin screw technique and prepolymer process are not all controlled the TPU late phase reaction effectively, therefore easily produce the super large molecule, and the product heterogeneity, easily generate insolubles and gel.
Summary of the invention:
The objective of the invention is to overcome the deficiency of above-mentioned prior art, and a kind of continuous production method of Polyurethane Thermoplastic Elastomer is provided.
Another order of the present invention is to provide a kind of dedicated system of Polyurethane Thermoplastic Elastomer continuous production method.
The present invention mainly solves existing twin screw technique and the continuous production Polyurethane Thermoplastic Elastomer of prepolymer process owing to effectively the TPU late phase reaction not being controlled, easily produce the super large molecule, the product heterogeneity, easily generate the problems such as insolubles and gel.
Technical scheme of the present invention is: a kind of continuous production method of Polyurethane Thermoplastic Elastomer, and its special character is to comprise following processing step:
A mixes and initial reaction in earlier stage, and feed composition is measured in proportion, by casting molding machine, is poured into forcing machine the first heating zone, regulates the Heating temperature in forcing machine rotating speed He Ge district, and material is further mixed, and carries out initial reaction;
B late phase reaction and crystallization, the material of initial reaction enters belt reactor by junctor, the heating of belt reactor leading portion, later stage is cooling, control each district's temperature, carry out late phase reaction and crystallization in belt reactor, obtain the flap reacted completely of higher molecular weight;
The c finished product, pulverize flap by pulverizer, obtain finished product TPU particle.
Further, described forcing machine machine section the first Heating Zone Temperature is 90 ℃, and all the other several Heating Zone Temperature are 140-180 ℃.
Further, described belt reactor heating zone temperature is 80-210 ℃, and the cooling section temperature-stable is 70 ℃, and in belt reactor, the residence time is 8-30 minute.
The continuous production method of a kind of Polyurethane Thermoplastic Elastomer of the present invention, because isocyanate material, polyvalent alcohol, the chainextender of production Polyurethane Thermoplastic Elastomer is surface reaction, need to by three fully contact can be reacted completely.Forcing machine machine section is mainly that mixture makes the material initial reaction, and actual material is lower in this elementary reaction degree, and molecular weight does not also reach the numerical value needed.Therefore this section control temperature is mainly in order to meet the needs of mixing of materials initial reaction.According to the reaction characteristics of TPU self, control temperature and will guarantee that material can initiation reaction in the well-mixed while, therefore, the low 90 ℃ of left and right of forcing machine machine section the first Heating Zone Temperature; Because TPU is thermopositive reaction, so the temperature of several heating zone, back reaches 140-180 ℃.Therefore forcing machine provides pyroreaction, enough strong shearing is provided, each component of TPU is mixed and the initial reaction chain, the residence time of material is shorter, be less than 1 minute, the material of complete reaction is not extruded on belt reactor with certain thickness by T-shaped mouthful of mould, complete late phase reaction on the belt reactor with heating function, trickling is thick to the sheet on belt is 1-10mm, in course of conveying, sheet material is heated, heating zone can adopt the thermopair heating, Heating temperature is 80-210 ℃, it is cooling that cooling section can adopt cold wind to carry out, temperature-stable is 70 ℃, the heat-up time of TPU on belt is 5-20 minute, be 3-10 minute cooling time, reaction times is controlled at 8-30 minute, slowly complete late phase reaction and crystallization, then cooled sheet material is pulverized by pulverizer, obtain the TPU pulverized particles.
Realize the dedicated system of Polyurethane Thermoplastic Elastomer continuous production method, its special character is that it comprises storage tank, casting molding machine, forcing machine, belt reactor, pulverizer and wrapping machine, connects by junctor between described forcing machine and belt reactor; Described forcing machine is twin screw extruder or single screw extrusion machine, and screw extrusion press provides mix and initial reaction early stage; Described belt reactor is with the steel band of temperature controlling function or teflin tape, and belt reactor provides late phase reaction and crystallization.
Further, described single screw rod and twin screw extruder all can be used for reaction and extrude, the degree of mixing that starts material because of reaction is great on the reaction result impact, make the material initial reaction and forcing machine machine section mainly plays a part mixture, so the optimal selection of forcing machine machine section is twin screw extruder; Twin screw extruder is any one in type, incorgruous type, engagement type, non-engagement type in the same way; Preferred tight engagement type twin screw extruder in the same way.
Further, described junctor is T-shaped mouthful of mould.
The applicable TPU of continuation method of the present invention and dedicated system can be any type, as polyester type TPU, and polyether-type TPU, the types such as polycarbonate type TPU.
Compared with the prior art the continuous production method of a kind of Polyurethane Thermoplastic Elastomer of the present invention and dedicated system have outstanding substantive features and marked improvement, by the preferred twin screw extruder of forcing machine, mixed and initial reaction, late phase reaction is reacted product and secondary crystallization by the belt reactor with temperature controlling function, material reaction is more abundant, the degree that is separated is high, increased the product crystallization, tensile strength and the Tc of product have been improved, and undertaken by reacting in batches, suppressed super macromolecular generation, product gel and insolubles have effectively been reduced, improve the use range of product, can meet the demands than high product.
The accompanying drawing explanation:
Fig. 1 is connection diagram of the present invention.
Embodiment:
For Comprehension and Implementation better, provide specific embodiment below in conjunction with accompanying drawing and describe the present invention in detail.
The present invention describes by following embodiment and reference examples:
The TPU formula that following reference examples and embodiment adopt:
Ditan 4,4 '-vulcabond (MDI) 32.6%(weight)
Poly-hexanodioic acid Isosorbide-5-Nitrae butyleneglycol-ester (PBA, molar mass 2000g/mol) 58.1%(weight)
BDO (BDO) (molar mass is 90.123g/mol, and functionality is 2) 8.8%(weight)
Catalyzer: stannous octoate 0.011%(weight)
Oxidation inhibitor: Irganox
?1010 0.5%(weight)
Reference examples 1, by the polyester polyol (catalyzer and oxidation inhibitor directly join in polyvalent alcohol) be stored in mechanical storage tank, vulcabond MDI (diphenylmethanediisocyanate) (43 ℃ of storing temps), chainextender BDO (1, the 4-butyleneglycol) (60 ℃ of storing temps), be poured into the forcing machine machine section of forcing machine by rich thunder casting molding machine, the mixing head rotating speed is 3600RPM, controlling forcing machine machine section the first Heating Zone Temperature is 180 ℃, all the other several Heating Zone Temperature are 200 ℃ ± 5 ℃, and screw speed is controlled as 40Hz; Obtain the TPU particle by granulation underwater.
Reference examples 2, by the polyester polyol (catalyzer and oxidation inhibitor directly join in polyvalent alcohol) be stored in mechanical storage tank, vulcabond MDI (diphenylmethanediisocyanate) is pre-mixed by tubular reactor and generates prepolymer, then with chainextender BDO (1, the 4-butyleneglycol) be poured into the forcing machine machine section of forcing machine by rich thunder casting molding machine, the mixing head rotating speed is 3600RPM, controlling forcing machine machine section the first Heating Zone Temperature is 180 ℃, all the other several Heating Zone Temperature are 200 ℃ ± 5 ℃, and screw speed is controlled as 40Hz; Obtain the TPU particle by granulation underwater.
Embodiment 1, referring to Fig. 1, select storage tank 1 according to the raw material storage amount, select rich thunder casting molding machine 2, selection length is that 2320mm, diameter are that 71mm, screw slenderness ratio L/D are 32, the tight in the same way engagement type twin screw extruder 3 that 8 heating zone are arranged, the T-shaped mouthful of mould that the selection wide cut is 1.2 meters is as junctor 7, and selection length is 20 meters steel bands or adopts teflin tape, additional baking oven runner as belt reactor 4; Select conventional pulverizer 5 simultaneously; To between forcing machine 3 and belt reactor 4, by T-shaped mouthful of mould junctor 7, connect; Finally by wrapping machine 6, packed, by aforesaid device, formed dedicated system of the present invention.
Embodiment 2, adopt the system of embodiment 1, by polyester polyol (catalyzer and oxidation inhibitor directly join in polyvalent alcohol), vulcabond MDI (diphenylmethanediisocyanate) and the chainextender BDO (1 be stored in storage tank, the 4-butyleneglycol), be poured into the forcing machine section of forcing machine with rich thunder casting molding machine, the mixing head rotating speed is 3600RPM, controlling forcing machine machine section the first Heating Zone Temperature is 90 ℃, all the other several Heating Zone Temperature are 140 ℃-180 ℃, and screw speed is controlled as 40Hz; By T-shaped mouthful of mould, TPU is cast on belt reactor, cast thickness is 4mm, the sheet material that wide cut is 1.2 meters, front 5 sections heating in the baking oven runner, temperature is 130 degree, back 3 district's wind cooling temperature lowerings, temperature-stable is 70 degree, and in the baking oven runner, the residence time is 20 minutes; Finally sheet material is pulverized, obtained the TPU pulverized particles, packed by wrapping machine.
Embodiment 3, adopt the system of embodiment 1, by polyester polyol (catalyzer and oxidation inhibitor directly join in polyvalent alcohol), vulcabond MDI (diphenylmethanediisocyanate) and the chainextender BDO (1 be stored in storage tank, the 4-butyleneglycol), be poured into the forcing machine section of forcing machine with rich thunder casting molding machine, the mixing head rotating speed is 3600RPM, controlling forcing machine machine section the first Heating Zone Temperature is 90 ℃, all the other several Heating Zone Temperature are 140 ℃-180 ℃, and screw speed is controlled as 40Hz; By T-shaped mouthful of mould, TPU is cast on belt reactor, cast thickness is 1mm, the sheet material that wide cut is 1.2 meters, front 5 sections heating in the baking oven runner, temperature is 80 degree, back 3 district's wind cooling temperature lowerings, temperature-stable is 70 degree, and in the baking oven runner, the residence time is 8 minutes; Finally sheet material is pulverized, obtained the TPU pulverized particles, packed by wrapping machine.
Embodiment 4, adopt the system of embodiment 1, by polyester polyol (catalyzer and oxidation inhibitor directly join in polyvalent alcohol), vulcabond MDI (diphenylmethanediisocyanate) and the chainextender BDO (1 be stored in storage tank, the 4-butyleneglycol), be poured into the forcing machine section of forcing machine with rich thunder casting molding machine, the mixing head rotating speed is 3600RPM, controlling forcing machine machine section the first Heating Zone Temperature is 90 ℃, all the other several Heating Zone Temperature are 140 ℃-180 ℃, and screw speed is controlled as 40Hz; By T-shaped mouthful of mould, TPU is cast on belt reactor, cast thickness is 10mm, the sheet material that wide cut is 1.2 meters, front 5 sections heating in the baking oven runner, temperature is 210 degree, back 3 district's wind cooling temperature lowerings, temperature-stable is 70 degree, and in the baking oven runner, the residence time is 30 minutes; Finally sheet material is pulverized, obtained the TPU pulverized particles, packed by wrapping machine.
The TPU the physical property of product of above-described embodiment and reference examples production is contrasted, the results are shown in Table 1.
Table 1
Above-mentioned, the film gel is judged in the following manner: the TPU granule materials is melted as the 30mm single screw extrusion machine at diameter and pass through T-shaped die extrusion 4.5-6 centimetre wide, the film of 6-10 mm thick is rectangular.
Compression set is tested by ASTMD395 B method, and test bars is that diameter is 13mm, the cylinder of 6mm.70 ℃ of temperature controls, place 22 hours, compress under the condition of 25% ℃ and tested.
As can be seen from the above results, adopt the product of the system production of forcing machine and belt reactor can improve intensity, effectively reduce the product gel, enlarge the product use range.
Claims (5)
1. the continuous production method of a Polyurethane Thermoplastic Elastomer is characterized in that comprising following processing step:
A mixes and initial reaction in earlier stage, and feed composition is measured in proportion by casting molding machine and is poured into forcing machine the first heating zone, regulates the Heating temperature in forcing machine rotating speed He Ge district, and material is further mixed, and carries out initial reaction; Described forcing machine machine section the first Heating Zone Temperature is 90 ℃, and all the other several Heating Zone Temperature are 140-180 ℃, and residence time of material is less than 1 minute;
B late phase reaction and crystallization, the material of initial reaction enters belt reactor by junctor, controls each district's temperature, carries out late phase reaction and crystallization in belt reactor, obtains higher molecular weight; Described belt reactor heating zone temperature is 80-210 ℃, and the cooling section temperature-stable is 70 ℃, and in belt reactor, the residence time is 8-30 minute;
The c finished product, pulverize by pulverizer, obtains finished product TPU particle.
2. realize the dedicated system of the Polyurethane Thermoplastic Elastomer continuous production method of claim 1, it is characterized in that it comprises storage tank (1), casting molding machine (2), forcing machine (3), belt reactor (4), pulverizer (5) and wrapping machine (6), connect by junctor (7) between described forcing machine (3) and belt reactor (4); Described forcing machine (3) is twin screw extruder or single screw extrusion machine; Described belt reactor (4) is steel band or teflin tape with heating function.
3. dedicated system according to claim 2, is characterized in that described twin screw extruder is for any one in type, incorgruous type, engagement type, non-engagement type in the same way.
4. dedicated system according to claim 3, is characterized in that described double-screw extruder screw type is for engagement type in the same way.
5. dedicated system according to claim 2, is characterized in that described junctor is T-shaped mouthful of mould.
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| CN110272528B (en) * | 2018-03-16 | 2021-07-16 | 浙江华峰热塑性聚氨酯有限公司 | Process for preparing thermoplastic polyurethanes |
| CN109160989B (en) * | 2018-08-23 | 2021-04-02 | 周朝功 | Production system and production process of thermoplastic polyurethane |
| CN114426686B (en) * | 2020-10-15 | 2024-02-09 | 中国石油化工股份有限公司 | Forming method of ultra-low viscosity polyvinyl alcohol solid |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE19754885C1 (en) * | 1997-12-10 | 1999-09-16 | Basf Ag | Process for the continuous production of granules from thermoplastic polyurethane elastomers |
| CN101020737A (en) * | 2007-03-01 | 2007-08-22 | 烟台万华新材料科技有限公司 | Continuous production process of thermoplastic polyurethane elastomer |
| CN202543125U (en) * | 2012-04-09 | 2012-11-21 | 烟台美瑞化学材料有限公司 | System for producing TPU (Thermoplastic Polyurethane Elastomer) by continuous method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2007130775A (en) * | 2005-11-08 | 2007-05-31 | Kaneka Corp | Tandem type reactive extruder and reactive extrusion method |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE19754885C1 (en) * | 1997-12-10 | 1999-09-16 | Basf Ag | Process for the continuous production of granules from thermoplastic polyurethane elastomers |
| CN101020737A (en) * | 2007-03-01 | 2007-08-22 | 烟台万华新材料科技有限公司 | Continuous production process of thermoplastic polyurethane elastomer |
| CN202543125U (en) * | 2012-04-09 | 2012-11-21 | 烟台美瑞化学材料有限公司 | System for producing TPU (Thermoplastic Polyurethane Elastomer) by continuous method |
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| Title |
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| JP特开2007-130775A 2007.05.31 |
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