CN114085500A - Polyester composition and preparation method and application thereof - Google Patents
Polyester composition and preparation method and application thereof Download PDFInfo
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- CN114085500A CN114085500A CN202111441064.1A CN202111441064A CN114085500A CN 114085500 A CN114085500 A CN 114085500A CN 202111441064 A CN202111441064 A CN 202111441064A CN 114085500 A CN114085500 A CN 114085500A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
- C08L67/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2312/00—Crosslinking
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Abstract
The invention discloses a polyester composition, which comprises the following components in parts by weight: 80 parts of polyester resin; 1-20 parts of GMA graft polymer; the GMA grafting rate range of the GMA graft polymer is 0.6-1.5wt%, the melt flow rate is 0.1-3g/10min, and the test conditions are 190 ℃ and 2.16 kg. According to the invention, the epoxy group of the GMA graft polymer with a specific melt flow rate and a specific grafting ratio range is reacted with the end group of the polyester resin to generate micro-crosslinking, so that the melt flow stability of the polyester composition is improved, and the appearance defect of jet lines generated in the injection molding process of the polyester composition is improved.
Description
Technical Field
The invention relates to the technical field of high polymer materials, in particular to a polyester composition and a preparation method and application thereof.
Background
The polyester belongs to a semi-crystalline material, and because the polyester contains a crystalline region, the material has good chemical corrosion resistance and excellent processing performance, and is widely applied to industries such as electronic and electrical elements, fans, bathrooms, household appliances and the like. However, since the molecular weight of polycondensates such as polyesters is generally not high, the problem of spray marks at the locations where the wall thickness of injection molds becomes thinner is likely to occur as a result of good processing flowability.
By spray marks is meant marks of the polymer melt which, in the direction of flow of the injection-molded part, appear to bend like a serpentine. Under normal conditions, the polymer melt filling mold stably fills the mold along the inner cavity wall of the mold in a fountain flowing mode, but when the melt passes through a pouring gate at high speed or the melt is suddenly turned to a thin place from the wall thickness, the melt can be sprayed into the cavity in a spraying mode to form a folded material strip, the whole cavity is stably filled with the subsequent melt, and the folded material strip sprayed previously cannot be fused with the subsequent stably filled melt into a whole due to the fact that the folded material strip is firstly collided with the cooled cavity wall to be solidified, so that snake-shaped marks are generated.
The current solution to the spray pattern is 1) product design, which replaces abrupt wall thickness transition with transitional and gradual wall thickness; 2) in the design of the mold, the sprue is prevented from being opened at one end of the wall thickness as much as possible, or a baffle structure is designed to block the injection; 3) the process adopts a slow injection molding process; 4) the material is selected from polymers with high molecular weight and large melt viscosity. However, the above methods have certain limitations. For example, 1) the product design is a structural design which can not avoid the wall thickness mutation due to the actual application requirement; method 2) is limited by the mold structure, sometimes the gate cannot be moved to the proper position; method 3) the process sometimes loses one another and cannot be improved; method 4) is sometimes limited by the fact that the molecular weight or viscosity of the polymer cannot be increased further by the state of the art synthesis.
Disclosure of Invention
The invention aims to provide a polyester composition which is remarkably improved on the defect of jet lines.
Another object of the present invention is to provide a process for the preparation of the above polyester composition and its use.
The invention is realized by the following technical scheme:
the polyester composition comprises the following components in parts by weight:
80 parts of polyester resin;
1-20 parts of GMA graft polymer;
the GMA grafting rate range of the GMA graft polymer is 0.6-1.5wt%, the melt flow rate is 0.1-3g/10min, and the test conditions are 190 ℃ and 2.16 kg.
The method for testing the carboxyl end group of the polyester resin comprises the following steps: 1) weighing about 1g (W) of sample, and dissolving the sample in 30ml of mixed solution of o-cresol and chloroform; 2) after 3 drops of phenolphthalein indicator are dripped, using HCL solution with the concentration of 0.01mol/l for titration, taking the titration end point when the solution is changed from colorless to pink, and recording the dosage V1 of the titration solution; 3) taking a blank sample without adding a sample, and recording the dosage V0 of the titration solution; 4) calculating the content of terminal amino groups, wherein the formula is as follows:
carboxyl content (mmol/kg) = (V1-V0) × N1000/W
Wherein, N: the molar concentration of the titration solution;
w: the sample weight in grams.
The testing method of the grafting ratio range of GMA in the GMA grafted polymer comprises the following steps: 1) and (3) refining GMA graft: dissolving with dimethylbenzene, washing with acetone, and vacuum drying to obtain refined graft; 2) accurately weighing 0.5g of refined graft, adding 80ml of dimethylbenzene, heating and refluxing to fully open an epoxy group on GMA, using a phenolphthalein/methanol solution as an indicator, using 0.05mol/l of NaOH/methanol solution to titrate until the color of the solution is changed from colorless to pink, and recording consumption V; 3) blank titration, weighing 0.5g of non-graft, repeating step 2), recording the consumption volume V of NaOH/methanol solution consumed in the blank test0. The formula for calculating the grafting ratio is as follows:
CGMA%=142.15*(V0-V)*C/1000m*100%
wherein, CGMAThe percentage of GMA grafting percent and C are the concentration of NaOH standard solutionAnd m is the quality of the refined GMA graft.
The melt flow rate was measured according to ISO 1133-1-2011.
Preferably, 11 to 17 parts of GMA graft polymer.
Preferably, the carboxyl end group content of the polyester resin is 30-50mmol/kg, and more preferably, the carboxyl end group content of the polyester resin is 35-45 mmol/kg.
The GMA grafted polymer is at least one of GMA grafted PP, GMA grafted PE, GMA grafted POE and GMA grafted EPDM.
The grafting rate of the GMA graft polymer ranges from 0.8 to 1.2wt%, the melt flow rate is 1 to 2.5g/10min, and the test conditions are 190 ℃ and 2.16 kg.
Further preferably, the GMA grafted polymer is selected from GMA grafted POE.
The polyester resin is selected from at least one of PET, PBT, PTT, PCT, PEN or PBN.
0-2 parts of auxiliary agent is also included according to the parts by weight; the auxiliary agent is at least one selected from an antioxidant, a lubricant and a light stabilizer.
The antioxidant may be: 1,3, 5-trimethyl-2, 4, 6-tris (3, 5-di-tert-butyl-4-hydroxybenzyl) benzene; 2, 5-di-tert-butyl-4-hydroxybenzyldimethylamine; diethyl-3, 5-di-tert-butyl-4-hydroxybenzyl phosphate; stearyl-3, 5-di-tert-butyl-4-hydroxybenzyl phosphate; 3, 5-di-tert-butyl-4-hydroxyphenyl-3, 5-distearyl-thiotriazolylamine; 2, 6-di-tert-butyl-4-hydroxymethylphenol; 2, 4-bis- (n-octylthio) -6- (4-hydroxy-3, 5-di-tert-butyl glyceryl allyl ether) -1,3, 5-triazine; n, N' -hexamethylenebis (3, 5-di-tert-butyl-4-hydroxy-hydrocinnamamide); n, N' -bis- (3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionyl) hexamethylenediamine; octadecyl-3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate; pentaerythrityl-tetrakis [3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ]; triethylene glycol-bis [3- (3, 5-dimethyl-4-hydroxyphenyl) propionate ]; triethylene glycol bis [ beta- (3-tert-butyl-4-hydroxy-5-methylphenyl) propionate ]; 2, 2' -thiodiethyl-bis [3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate, and the like.
The lubricant may be: at least one of a stearate lubricant, a fatty acid lubricant, and a stearate lubricant; the stearate lubricant is at least one selected from calcium stearate, magnesium stearate and zinc stearate; the fatty acid lubricant is at least one selected from fatty acid, fatty acid derivative and fatty acid ester; the stearate lubricant is at least one selected from pentaerythritol stearate.
The light stabilizer is selected from hydroxy benzoate ultraviolet absorbers, benzophenone ultraviolet absorbers, benzotriazole ultraviolet absorbers and HALS ultraviolet absorbers.
Specifically, the ultraviolet absorber of hydroxybenzoate esters can be selected from cetyl 3, 5-diisobutyl-4-hydroxybenzoate, 2, 4-di-tert-butylphenyl 3, 5-di-tert-butyl-4-hydroxybenzoate, and n-cetyl 3, 5-di-tert-butyl-4-hydroxybenzoate;
the benzophenone-type ultraviolet absorbent can be selected from 2, 4-dihydroxy benzophenone; 2-hydroxy-4-alkoxybenzophenone, 1, 3-bis (methoxy-3-hydroxy-4-benzophenone) benzene, 2-hydroxy-4-phenylalkoxybenzophenone, 2-hydroxy-4-n-octoxybenzophenone, 2-hydroxy-4-methylmethacrylate benzophenone.
The benzotriazole-based ultraviolet absorber may be selected from 2- (2 '-hydroxy-5' -methylphenyl) benzotriazole, 2- (2 '-hydroxy-5' -methyl) -benzotriazole, 2- (3 ', 5' -di-tert-butyl-2 '-hydroxy) -benzotriazole, 2- (2' -hydroxy-3 '-isobutyl-5' -tert-butyl) -benzotriazole, 2- (2 '-hydroxy-3', 5 '-bis (1, 1-dimethylphenyl) -benzotriazole, 2- (2' -hydroxy-5 '-tert-octyl) -benzotriazole, 2- (2' -hydroxy-3 '- (1, 1-dimethylphenyl) -5' - [1 ], 1,3, 3-tetramethylbutyl ] -benzotriazole, 2' methylene- (6- (2H-benzotriazole) -4-tert-octyl) phenol, 2- (2H-benzotriazole-2) -4, 6-bis (1-methyl-1-phenylethyl) phenol;
the HALS ultraviolet absorbent can be selected from bis-2, 2,6, 6-tetramethylpiperidinol sebacate, N' - (2,2,6, 6-tetramethyl, 4-aminopiperidine) -isophthalamide, bis-1-octyloxy-2, 2,6, 6-tetramethylpiperidinol sebacate, (1,2,2,6, 6-pentamethylpiperidinol) methacrylate, poly { [6- [ (1,1,3, 3-tetramethylbutyl) amino ] ] -1,3, 5-triazine-2, 4- [ (2,2,6, 6-tetramethyl-piperidyl) imino ] -1, 6-hexamethylene [ (2,2,6, 6-tetramethyl-4-piperidyl) imino ] }.
A process for preparing a polyester composition comprising the steps of: according to the proportion, the components are uniformly mixed and extruded and granulated by a double-screw extruder, the temperature range of the screw is 220-250 ℃, and the rotating speed range is 300-600rpm, so as to obtain the polyester composition.
The application of the polyester composition is used for electronic and electric appliance parts.
The invention has the following beneficial effects:
according to the invention, the epoxy group of the GMA graft polymer with a specific melt flow rate and a specific grafting ratio range is reacted with the end group of the polyester resin to generate micro-crosslinking, so that the melt flow stability of the polyester composition is improved, and the appearance defect of jet lines generated in the injection molding process of the polyester composition is improved.
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FIG. 1: the die is characterized in that (a) is a front view of a die cavity of the die, scale marks are arranged in the front view, the minimum scale mark is 10mm, and (b) is a top view of the die cavity.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
The raw material sources used in the examples and comparative examples are as follows:
PBT-A: the content of terminal carboxyl is 30mmol/kg, the trademark PBT 1100-211M, the manufacturer Changchun chemical industry.
PBT-B: the content of terminal carboxyl is 35mmol/kg, the trademark PBT GX121, the manufacturer characterizes the chemical fiber.
PBT-C: the carboxyl end group content is 45mmol/kg, the trademark PBT L10XM, Jiangsu and Shili of manufacturers.
PBT-D: the carboxyl end group content is 50mmol/kg, the trademark PBT 1100A, the manufacturer Nantong star.
PBT-E: the content of terminal carboxyl is 20mmol/kg, the trademark PBT GX121J, the manufacturer marks the chemical fiber.
PBT-F: the content of terminal carboxyl is 60mmol/kg, the trademark PBT GX112, manufacturer symbol chemical fiber.
PET: the content of terminal carboxyl is 45mmol/kg, the trade mark PET FG600, the Oriental insulating material of Sichuan of manufacturers.
PTT: the carboxyl end group content is 40mmol/kg, the brand Corterra CP509201, manufactured by Shell chemical company in America.
PCT: the carboxyl end group content is 35mmol/kg, the brand number SKYGREEN JN100, manufactured by Korea SK chemical company.
GMA grafted POE-A: the range of grafting rate is 0.6wt%, the melt flow rate is 0.4g/10min, the test condition is 190 ℃, 2.16 kg;
GMA grafted POE-B: W5A, Koiss, grafting Rate Range 0.8wt%, melt flow Rate 1.9g/10min, test conditions 190 ℃, 2.16 kg;
GMA grafted POE-C: SOG-02, easy to handle, the range of grafting rate is 1.2wt%, the melt flow rate is 2.5g/10min, the test conditions are 190 ℃, 2.16 kg;
GMA grafted POE-D: the range of grafting rate is 1.5wt%, the melt flow rate is 3.0g/10min, the test condition is 190 ℃, 2.16 kg;
GMA grafted POE-E: the range of grafting rate is 0.3wt%, the melt flow rate is 1.4g/10min, the test condition is 190 ℃, 2.16 kg;
GMA grafted POE-F: SOG-02, easy to handle, the range of grafting rate is 2.1wt%, the melt flow rate is 2.0g/10min, the test conditions are 190 ℃, 2.16 kg;
GMA grafted POE-G: GPM600A, Ningwave energy light, grafting rate range is 1.1wt%, melt flow rate is 3.2g/10min, test conditions 190 ℃, 2.16 kg;
GMA grafted POE-H: GPM600D, Ningwave energy light, grafting rate range is 0.9wt%, melt flow rate is 4.3g/10min, test conditions 190 ℃, 2.16 kg;
GMA grafted PP: AD-90, a polymer new material company of south sea cypress morning in Foshan city, the grafting ratio range is 1.5wt%, the melt flow rate is 2g/10min, the test condition is 190 ℃, 2.16 kg;
GMA grafted PE: PX3243, linadebarel, grafting rate range is 1wt%, melt flow rate is 3g/10min, test conditions 190 deg.C, 2.16 kg;
GMA grafted EPDM: GPM500CY, Nicotinable light, grafting Rate in the range of 1.2wt%, melt flow rate of 1g/10min, test conditions 190 ℃, 2.16 kg.
Lubricant: TR044W, STRUKTOL Co.
Examples and comparative example preparation of polyester compositions: according to the proportion, the components are uniformly mixed, and are extruded and granulated by a double-screw extruder, the temperature of a region 1-8 of the screw extruder is set to be 220/230/230/240/240/230/230/250 ℃, and the rotating speed is 350rpm, so that the polyester composition is obtained.
The test methods are as follows:
(1) the spray pattern evaluation method comprises the following steps: in order to quantitatively evaluate the injection lines of the material injection molding, a mold as shown in the attached FIG. 1 was designed. A group of samples are compared and evaluated every time, the same injection molding machine is fixedly used, and the same injection molding process parameters (the highest injection molding speed of the machine is 90% and the injection lines are easy to appear at high speed) are fixedly used. The temperature of the die is fixed at 80 ℃, and circulating water is adopted for cooling. And starting a spray pattern evaluation test when the temperature of the mold is stable, recording the scale (exceeding half of the minimum scale, calculating one scale, and omitting less than half of the minimum scale) where the spray phenomenon starts to occur according to the scale value in the mold, performing injection molding on 10 molds for each sample, and taking an average value L. The larger the value of L, the stronger the material is resistant to the occurrence of spray marks. In order to quantitatively evaluate the injection lines of the material injection molding, the mold shown in the attached figure 1 is designed, wherein (a) is a front view of a mold cavity, scale lines are arranged in the front view, and the minimum scale is 10mm, and (b) is a top view of the mold cavity. The longer the spraying distance appears, the smaller the risk of spraying phenomenon of the material under the same injection molding conditions (including injection molding temperature, injection molding speed, temperature of a mold and a mold, and the like), namely the more obvious the spraying pattern is improved. To enable quantitative evaluation, the occurrence of the throw distance was divided into four grades: 1) 0-5cm, the risk of occurrence of jetting phenomena is high; 2) 6-10cm, the risk of occurrence of jetting phenomena is moderate; 3) 11-15cm, the risk of the spray phenomenon is low; 4) 16-20cm, there is little risk of the occurrence of jetting phenomena.
Table 1: EXAMPLES 1-8 polyester composition compositions (parts by weight) and test results
| Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Example 6 | Example 7 | Example 8 | |
| PBT-A | 80 | 80 | 80 | 80 | 80 | |||
| PET | 80 | |||||||
| PTT | 80 | |||||||
| PCT | 80 | |||||||
| GMA grafted POE-A | 13 | 13 | 13 | 13 | 1 | 11 | 17 | 20 |
| Lubricant agent | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 |
| Occurrence of jet distance cm | 15 | 15 | 16 | 15 | 10 | 13 | 16 | 11 |
As seen in examples 1/5-8, the preferred GMA graft polymer content is 11-17 parts.
Table 2: examples 9-8 polyester composition compositions (parts by weight) and test results
| Example 9 | Example 10 | Example 11 | Example 12 | Example 13 | Example 14 | Example 15 | |
| PBT-A | 80 | 80 | 80 | 80 | 80 | 80 | 80 |
| GMA grafted POE-B | 13 | ||||||
| GMA grafted POE-C | 13 | ||||||
| GMA grafted POE-D | 13 | ||||||
| GMA grafted PP | 13 | 15 | |||||
| GMA grafted PE | 13 | ||||||
| GMA grafted EPDM | 13 | ||||||
| Lubricant agent | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 | |
| Occurrence of jet distance cm | 18 | 19 | 13 | 13 | 12 | 14 | 14 |
As can be seen from examples 1/9-11, the preferred range of graft ratio for GMA graft polymers is 0.8-1.2wt%, the melt flow rate is 1-2.5g/10min, and the test conditions are 190 ℃ and 2.16 kg.
As can be seen from examples 1/12-14, the GMA-grafted polymer is preferably GMA-grafted POE.
Table 3: examples 16-21 polyester composition (parts by weight) and test results
| Example 17 | Example 18 | Example 19 | Example 20 | Example 21 | |
| PBT-B | 80 | ||||
| PBT-C | 80 | ||||
| PBT-D | 80 | ||||
| PBT-E | 80 | ||||
| PBT-F | 80 | ||||
| GMA grafted POE-A | 13 | 13 | 13 | 13 | 13 |
| Lubricant agent | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 |
| Occurrence of jet distance cm | 16 | 17 | 15 | 11 | 12 |
From examples 1/17 to 21, it is preferable that the polyester resin has a carboxyl end group content of 30 to 50mmol/kg, and more preferable that the polyester resin has a carboxyl end group content of 35 to 45 mmol/kg.
Table 4: comparative polyester composition (parts by weight) and test results
| Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 | Comparative example 5 | Comparative example 6 | |
| PBT-A | 80 | 80 | 80 | 80 | 80 | 80 |
| GMA grafted POE-E | 13 | 0.5 | 23 | |||
| GMA grafted POE-F | 13 | |||||
| GMA grafted POE-G | 13 | |||||
| GMA grafted POE-H | 13 | |||||
| Lubricant agent | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 |
| Occurrence of jet distance cm | 6 | 5 | 8 | 3 | 1 | 6 |
It is seen from comparative example 1/4 that too high or too low a grafting yield, melt index of the GMA graft polymer does not result in improved spray pattern appearance.
It is clear from examples 5 to 6 that neither too high nor too low a content of GMA graft polymer leads to an improvement in the appearance of spray marks.
Claims (10)
1. The polyester composition is characterized by comprising the following components in parts by weight:
80 parts of polyester resin;
1-20 parts of GMA graft polymer;
the GMA grafting rate range of the GMA graft polymer is 0.6-1.5wt%, the melt flow rate is 0.1-3g/10min, and the test conditions are 190 ℃ and 2.16 kg.
2. The polyester composition of claim 1, wherein the GMA graft polymer is present in an amount of 11 to 17 parts.
3. The polyester composition according to claim 1, wherein the carboxyl end group content of the polyester resin is 30 to 50mmol/kg, preferably 35 to 45 mmol/kg.
4. The polyester composition according to claim 1, wherein the GMA-grafted polymer is at least one selected from the group consisting of GMA-grafted PP, GMA-grafted PE, GMA-grafted POE, GMA-grafted EPDM.
5. The polyester composition according to claim 4, wherein the GMA graft polymer has a graft ratio in the range of 0.8 to 1.2wt%, a melt flow rate of 1 to 2.5g/10min, and a test condition of 190 ℃ and 2.16 kg.
6. The polyester composition of claim 5, wherein said GMA grafted polymer is selected from GMA grafted POE.
7. The polyester composition of claim 1, wherein the polyester resin is at least one selected from the group consisting of PET, PBT, PTT, PCT, PEN, and PBN.
8. The polyester composition according to claim 1, further comprising 0 to 2 parts by weight of an auxiliary; the auxiliary agent is at least one selected from an antioxidant, a lubricant and a light stabilizer.
9. A process for preparing a polyester composition according to any of claims 1 to 8, comprising the steps of: according to the proportion, the components are uniformly mixed and extruded and granulated by a double-screw extruder, the temperature range of the screw is 220-250 ℃, and the rotating speed range is 300-600rpm, so as to obtain the polyester composition.
10. Use of the polyester composition according to any of claims 1 to 8 for electronic and electrical parts.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1986004076A1 (en) * | 1985-01-11 | 1986-07-17 | Copolymer Rubber And Chemical Corporation | Polyesters having improved impact strength |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1986004076A1 (en) * | 1985-01-11 | 1986-07-17 | Copolymer Rubber And Chemical Corporation | Polyesters having improved impact strength |
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