CN112480611B - Low-emission long glass fiber reinforced PCBT material and preparation method thereof - Google Patents
Low-emission long glass fiber reinforced PCBT material and preparation method thereof Download PDFInfo
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- C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
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- C08G63/18—Dicarboxylic acids and dihydroxy compounds the acids or hydroxy compounds containing carbocyclic rings
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- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
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- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
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Abstract
The invention relates to a low-emission long glass fiber reinforced PCBT material and a preparation method thereof. The in-situ polymerized long glass fiber reinforced PCBT material with sufficient fiber impregnation and excellent performance is produced at low temperature.
Description
Technical Field
The invention belongs to the field of PCBT materials and preparation thereof, and particularly relates to a low-emission long glass fiber reinforced PCBT material and a preparation method thereof.
Background
The Cyclic Butylene Terephthalate (CBT) is a cyclic oligomer with polymerization degree of 2-7 prepared by taking Polybutylene terephthalate (PBT) resin as a raw material and adopting a depolymerization cyclization technology, and the cyclic oligomer is heated, melted and flowed like water, and has extremely low viscosity (30mPa.s, 190 ℃). The CBT resin can be polymerized under the action of tin or titanium catalysts at high temperature (generally more than 180 ℃) to obtain linear polybutylene terephthalate (PCBT for short).
Patent CN 103819882A introduces a halogen-free flame-retardant long glass fiber reinforced PBT composite material and a preparation method thereof, PBT is used as a matrix, primary impregnation is realized in a high-temperature impregnation tank 1 with the length of 2-2.5m at the temperature of 300-360 ℃, and 2 times of flame-retardant master batch impregnation is realized in a low-temperature impregnation tank with the length of 1-1.5m at the temperature of 230-250 ℃. Patent CN 104098875A introduces a continuous fiber reinforced CBT prepreg tape, which makes CBT resin and catalyst not react or difficult to react in an extruder, and then utilizes a resin extrusion melt impregnation method to prepare the continuous fiber reinforced CBT prepreg tape, the production speed is only 2-10m/min, the production efficiency is extremely low, and the continuous fiber reinforced CBT prepreg tape is only suitable for a layer-laying hot-press molding process, the number of cut leftover materials is large in the molding process, the resource waste is caused, and the product requirement of complex structure design cannot be met. In addition, the in-situ polymerization process introduced by the invention has low production efficiency, so that the resin and the auxiliary agent are degraded due to too long time of staying in a high-temperature impregnation die head, and more small molecular substances are generated; and a large amount of initiator and unreacted CBT monomer can remain, and excessive initiator can further initiate the degradation of the finished material in the subsequent processing and heating process, so that the final product has poor emission performance (such as TVOC and odor) and material aging performance.
Disclosure of Invention
The invention aims to solve the technical problem of providing a low-emission long glass fiber reinforced PCBT material and a preparation method thereof,
the technical defects of high production temperature and poor glass fiber impregnation of the conventional long glass fiber reinforced PBT material are overcome; the defect of poor emission performance caused by more small molecular substances in the long glass fiber reinforced PBT material or the prepreg PBT material is overcome; the defects that the production capacity of the prepreg tape is low and the prepreg tape cannot be applied to injection molding parts are overcome.
The invention relates to a long glass fiber reinforced PCBT material, which comprises the following components in percentage by weight:
wherein the low emission modifier is a mixture of diatomaceous earth and rare earth stearate.
The CBT resin is cyclic butylene terephthalate with the polymerization degree of 2-7 and the weight-average molecular weight of 400-2000 measured by gel permeation chromatography.
The continuous long glass fiber is roving with twist, the diameter of the monofilament is 11-17um, and the glass fiber component Al 2 O 3 The content is not less than 15 percentThe sodium hypochlorite solution has excellent alkali resistance, and the mass loss is less than 6 percent when the sodium hypochlorite solution is soaked in 0.1mol/L NaOH solution at the temperature of 80 ℃ for 24 hours.
The catalyst is a tin catalyst; the additive is one or more of a flame retardant, an antibacterial agent, an antistatic agent, a heat conduction filler, an antioxidant and a lubricant.
The catalyst is one or more of dihydroxy butyl tin chloride, dibutyl tin dilaurate and chloro monobutyl stannic acid; the antioxidant is one or more of amines, phosphites, semi-hindered phenols and cyclic aromatics; the lubricant is one or more of Meng Dan esters, metal soaps, stearic acid complex esters and amides.
The diatomite has a porous structure, the pore diameter is between 5 and 20nm, and the pore diameter is 400m 2 Specific surface area is more than 200m 2 (ii)/g; the content of the rare earth is 12 to 30 weight percent.
The mass ratio of the diatomite to the stearic acid rare earth is 1:1-5.
The invention relates to a preparation method of a long glass fiber reinforced PCBT material, which comprises the following steps:
(1) Weighing the raw materials according to the proportion, then pre-mixing the CBT-containing resin, the catalyst and the low-emission modifier uniformly, feeding the mixture into a double-screw extruder by a weigher for pre-extrusion reaction, and feeding the pre-reacted mixed solution into a glass fiber impregnation die head; the glass fiber is drawn by the drawing equipment and is dipped by a dipping die head to obtain a material strip;
(2) And (3) passing the material strips through an infrared heat-preservation oven, and then cooling, shaping and cutting into particles with fixed length.
In the step (1), the temperature of the double-screw extruder is set to be 140-180 ℃, and the rotating speed is 200-400r/min.
The temperature of the impregnation die head in the step (1) is set to be 180-210 ℃ when the glass fiber enters the pre-impregnation section and 215-250 ℃ when the resin is completely reacted; the traction speed is 50-90m/min.
And (3) setting the temperature of the infrared heat preservation oven in the step (2) to be 210 ℃.
The dipping die head adopted in the step (1) adopts CN 108099051A dipping equipment, and a corrugated dipping cavity is adopted, when the resin melt distribution runner is communicated with the peak position of the dipping cavity, the vertical height of the cavity at the peak position of the dipping cavity is greater than that at the trough position of the dipping cavity, when the resin melt distribution runner is communicated with the trough position of the dipping cavity, the vertical height of the cavity at the trough position of the dipping cavity is greater than that at the peak position of the dipping cavity, so that the dipping effect of continuous fibers can be balanced, broken fiber hairiness generated during dipping can be taken out of a dipping area, the yarn breakage phenomenon is avoided, cooling, traction and grain cutting treatment are carried out on the dipped continuous fibers, and the production stability and production efficiency are improved.
The long glass fiber reinforced PCBT material disclosed by the invention is applied to injection molding in products with high design freedom, such as products with multiple reinforcing ribs and multiple concave-convex structures.
Advantageous effects
(1) According to the invention, the CBT resin is polymerized in situ, so that efficient production is realized, the production speed can reach 50-90m/min, the glass fiber and the resin can be fully impregnated under the condition of low processing temperature, more resin coats the glass fiber monofilaments, modified particles cannot be split after being granulated, the glass fiber hairiness is less, and the appearance of a finished product is more excellent. The method is suitable for an injection molding process, efficient and continuous production, high in design freedom degree and suitable for products with multiple reinforcing ribs and multiple concave-convex structures;
(2) The long glass fiber reinforced PCBT material prepared by the invention obtains a low-emission material through the compounding action of diatomite porous and stearic acid rare earth, and simultaneously achieves the effect of improving the high-temperature injection molding thermal stability of the material.
(3) The in-situ polymerized long glass fiber reinforced PCBT material with sufficient fiber impregnation and excellent performance is produced at low temperature.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
(1) Source of raw materials
CBT resin 1: CBT 200, american cycles;
CBT resin 2: CBT 100, american cycles;
PBT resin: GX112, characterization of chemical fibers;
long glass fiber 1: ER4301H-2400, chongqing International composite Co., ltd;
continuous glass fiber 2: ER4301R-2400 untwisted yarn, chongqing International composite Co., ltd;
catalyst 1: dihydroxybutyltin chloride, commercially available;
diatomite: the specific surface area of the brand KFD-8 is more than 200m 2 (iv)/g, qingdao san Ding Yuan diatomaceous Earth, inc.;
stearic acid rare earth, jiangxi macro-remote chemical industry; RE (C17H 35 COO) 3, the melting point is 110-115 ℃, and the content of rare earth is 14-25%.
Antioxidant: antioxidant 1010, commercially available;
lubricant: erucamide, commercially available;
calcium stearate: is commercially available
(2) Mechanical property test evaluation method
According to the ISO527-1/2 standard, the long glass fiber reinforced PCBT material is molded into a test sample strip with the thickness of 4mm by using an injection molding machine, and the tensile strength of the sample strip is tested under the test speed condition of 23 ℃ and 5 mm/min; the dry bars were tested according to ISO179/1eA for their impact strength at 23 ℃ in the form of simple beams notched. The bending strength and the bending modulus of the sample strip are measured according to ISO178 at 23 ℃ and a test speed of 2 mm/min.
(2) Aging performance test and evaluation method
The aging properties of the standard specimens are tested according to ISO 188 at a temperature of 150 ℃ for a time of 1000H, and the tensile strength (in MPa) of the specimens is tested.
(3) Emission analysis
The material particles TVOC were tested according to standard PV 3341.
The odor of injection-molded square plates of the material (injection temperature 235 ℃; size 100 x 3 mm) was tested according to the PV 3900 standard;
the professional evaluator gave the odor score and the odor sensation as a self-experience. The evaluation principle is as follows: 1 minute, no odor; 2 points, has smell but does not disturb people; 3 points, has obvious smell but is still not disturbing; 4 points, disturbing smell exists; 5 points, strong disturbing smell exists; 6 points, cannot be tolerated; in this example, five evaluators were used, and the results were averaged.
(4) Quantitative analysis of degree of impregnation of glass fiber
Randomly weighing 500g of particles, placing in a small-sized high-speed mixer, shaking for 15min, selecting particles without glass fiber hairiness and glass fiber hairiness scattered in the shaking mixer, weighing, and marking as M Y 。
Examples 1 to 10
Weighing the raw materials according to the components and the parts by weight in the table 1;
uniformly premixing CBT resin (dried at 80 ℃ for 6 hours) and a catalyst, a low-emission modifier, an antioxidant and a lubricant, feeding the mixture into a double-screw extruder by a metering scale for pre-extrusion reaction (the temperature is set to be 140-180 ℃, and the rotating speed is 200-400 r/min), forcibly feeding the mixed solution of the pre-reacted CBT resin, the catalyst, the low-emission modifier, the antioxidant and the lubricant into an ER4301H-2400 glass fiber impregnation die head (CN 108099051A is adopted), drawing glass fibers by drawing equipment (the drawing speed is 70 m/min) through the impregnation die head to realize the impregnation of a resin auxiliary agent melt on the glass fibers, passing the well-impregnated strips through an infrared heat-preservation oven (the temperature is 210 ℃), and then cooling, shaping and dicing to obtain fixed-length particles; wherein, the temperature of the impregnation die head is set to be a glass fiber entering preimpregnation section and a resin complete reaction section, and the temperature is respectively set to be the preimpregnation sections of 180, 200 and 210 ℃; reaction sections 210, 230, 245 ℃.
Comparative examples 1 to 5
The raw materials were weighed in the proportions shown in Table 2, and the preparation methods were otherwise the same as in the above examples.
Comparative example 6
Weighing the raw materials according to the proportion in the table 2, uniformly mixing the CBT resin (dried at 80 ℃ for 6H) with the catalyst, the low-emission modifier, the antioxidant and the lubricant to obtain a mixture, extruding the mixture by an extruder (designed in a patent CN 101474868A), enabling the extruded substance to meet the glass fiber at staggered double die heads to realize impregnation, leading out the prepreg tape by a cooling roller, and rolling to obtain the prepreg tape, wherein the extrusion process is the same as that of the example 1, and the traction speed is 8m/min.
Cutting and paving the prepreg tape, performing hot press molding on the prepreg tape on a flat vulcanizing machine, taking out the composite material after cold pressing, and then performing hot press molding on the composite material
Testing the related performance, wherein the temperature is 200 ℃ and is kept for 40min under no pressure, then is kept for 30min at 220 ℃ and 2.5MPa, and is kept for 10min at 240 ℃ and 5MPa, and the pressure is 5MPa under the cold pressing condition and the time is 50min.
Raw material components and parts by weight in the examples of Table 1
Table 2 raw material components and parts by weight in the comparative examples:
| the components are% | Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 | Comparative example 5 | Comparative example 6 |
| CBT resin 1 | 47.5 | 47.5 | 47.5 | 47.5 | 47.5 | |
| PBT resin | 47.5 | |||||
| Long glass fibers 1 | 50 | 50 | 50 | 50 | 50 | |
| Continuous glass fiber 2 | 50 | |||||
| Catalyst 1 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 |
| Diatomite | 1.4 | 1 | 0.7 | 0.7 | 0.7 | |
| Stearic acid rare earth | 1.4 | 0.4 | 0.7 | 0.7 | ||
| Calcium stearate | 0.7 | |||||
| Antioxidant agent | 0.3 | 0.3 | 0.3 | 0.3 | 0.3 | 0.3 |
| Lubricant agent | 0.3 | 0.3 | 0.3 | 0.3 | 0.3 | 0.3 |
Table 3 results of performance testing of examples
Table 4 comparative example performance test results
Example 6 compared to comparative example 4, the stearic acid rare earth system material reduced the odor grade of the material by one grade to 3.5 grade, the TVOC resin by about 53%; the retention rate of the 1000H aging strength of the material at 150 ℃ is improved from 76.4% to 89.3%.
Compared with the comparative examples 1 and 2, the diatomite and the stearic acid rare earth are compounded to play a synergistic role in example 6, the TVOC can be obviously reduced, the reduction ratio is about 50%, and the odor of the material is reduced by half to 3.5; in addition, the tensile strength of the material is obviously improved.
Compared with the comparative example 5, the impregnation degree of the glass fiber of the in-situ polymerization material is greatly improved, and the number of split particles is reduced by about 89%; the mechanical property is better improved, the tensile strength is improved by about 16 percent, the flexural modulus is improved by about 21 percent, and the notch impact strength is improved by about 36.3 percent; the emission performance is better solved, the odor is reduced to 3.5 grade from 4.0, and the TVOC value is reduced by about 69 percent.
Example 6 compared to comparative example 6, the material obtained at high production rate was improved in flexural strength and flexural modulus; more significantly, the TVOC was reduced by about 87%, the odor was reduced to a grade 3.5; the retention rate of the tensile strength aging performance of the material is improved from 73% to 89%.
Example 10 compared to comparative example 3, the ratio of diatomaceous earth to rare earth stearate was changed, 2.5:1 to 1: after 2.5, the overall emission performance and aging performance of the material are better improved.
Claims (9)
1. A long glass fiber reinforced PCBT material is characterized by comprising the following components in percentage by weight:
47 to 89.8 percent of CBT resin,
10 to 50 percent of continuous long glass fiber,
0.1 to 1.0 percent of catalyst,
0.5 to 5 percent of low-emission modifier,
0-30% of additive;
wherein the low-emission modifier is a mixture of diatomite and rare earth stearate; wherein the mass ratio of the diatomite to the stearic acid rare earth is 1 to 5; the continuous long glass fiber is twisted roving; the additive is one or more of a flame retardant, an antibacterial agent, an antistatic agent, a heat-conducting filler, an antioxidant and a lubricant;
wherein the sum of the weight percentages of the components is 100 percent.
2. The material of claim 1, wherein the CBT resin is a cyclic butylene terephthalate having a degree of polymerization of 2 to 7 and a weight average molecular weight of 400 to 2000.
3. The material of claim 1, wherein the continuous long glass fiber has a filament diameter of 11-17um and a glass fiber component of Al 2 O 3 The content is not less than 15 percent.
4. The material of claim 1, wherein the catalyst is a tin-based catalyst.
5. The material of claim 1, wherein the catalyst is one or more of dihydroxy butyl tin chloride, dibutyl tin dilaurate, and chloro monobutyl stannoic acid; the antioxidant is one or more of amines, phosphites, semi-hindered phenols and cyclic aromatics; the lubricant is one or more of Meng Dan esters, metal soaps, stearic acid complex esters and amides.
6. The material of claim 1, wherein the diatomaceous earth is porous with a pore size of 5-20nm, 400m 2 Specific surface area is more than 200m 2 (ii)/g; the content of the rare earth in the stearic acid rare earth is 12-30 wt%.
7. A preparation method of a long glass fiber reinforced PCBT material comprises the following steps:
(1) Weighing the raw materials according to the proportion of claim 1, then pre-mixing the CBT-containing resin, the catalyst and the low-emission modifier, feeding the mixture into a double-screw extruder by a weigher for pre-extrusion reaction, and feeding the pre-reacted mixed solution into a glass fiber impregnation die head; the glass fiber is drawn by the drawing equipment and is impregnated by the impregnation die head to obtain a material strip;
(2) And (3) passing the material strips through an infrared heat-preservation oven, and then cooling, shaping and dicing to obtain particles with fixed length.
8. The preparation method according to claim 7, wherein the temperature setting of the impregnation die head in the step (1) is divided into 180-210 ℃ for glass fiber entering the pre-impregnation section and 215-250 ℃ for resin complete reaction section; the traction speed is 50-90m/min.
9. Use of the long glass fiber reinforced PCBT material of claim 1 in injection moulded design products.
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| CN102555234B (en) * | 2012-02-01 | 2014-06-11 | 中材科技风电叶片股份有限公司 | Resin membrane melt impregnation forming method of fiber reinforced PBT composite material |
| CN104098875B (en) * | 2013-04-09 | 2017-10-17 | 上海杰事杰新材料(集团)股份有限公司 | A kind of continuous lod CBT prepreg tapes and its preparation method and application |
| US10442115B2 (en) * | 2016-05-25 | 2019-10-15 | Johns Manville | Manufacturing thermoplastic composites and articles |
| CN107955340B (en) * | 2017-11-02 | 2020-05-29 | 上海日之升科技有限公司 | PBT (polybutylene terephthalate) material for low-emission automobile air conditioner air outlet blade and preparation method thereof |
| CN107915948A (en) * | 2017-12-08 | 2018-04-17 | 广东技塑新材料股份有限公司 | A kind of low smell sterilization reinforced ABS automobile rearview mirror frame material and preparation method |
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