CN109608877B - Reinforced nylon material for injection molding of product with high precision and complex structure and preparation method thereof - Google Patents
Reinforced nylon material for injection molding of product with high precision and complex structure and preparation method thereof Download PDFInfo
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- CN109608877B CN109608877B CN201811364141.6A CN201811364141A CN109608877B CN 109608877 B CN109608877 B CN 109608877B CN 201811364141 A CN201811364141 A CN 201811364141A CN 109608877 B CN109608877 B CN 109608877B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
- C08J5/0405—Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres
- C08J5/043—Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres with glass fibres
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/26—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from polyamines and polycarboxylic acids
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2377/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
- C08J2377/06—Polyamides derived from polyamines and polycarboxylic acids
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2483/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2483/04—Polysiloxanes
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/04—Ingredients characterised by their shape and organic or inorganic ingredients
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- C—CHEMISTRY; METALLURGY
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/004—Additives being defined by their length
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/14—Glass
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Abstract
The invention discloses a reinforced nylon material for injection molding of a product with high precision and a complex structure and a preparation method thereof. The invention firstly synthesizes nylon 1012 with medium-low viscosity long carbon chains as a base material, then adds a proper amount of compound processing aids, adopts glass fiber for reinforcement, and utilizes a screw extrusion mechanism to prepare a reinforced nylon material suitable for injection molding precision products with high structure and complex structure. The reinforced nylon material for injection molding produced by the invention has the following performance indexes: tensile strength >100 MPa; bending strength >100 MPa; notched impact >10KJ/m 2; the difference in the aspect ratio shrinkage rate is less than 0.1; excellent demoulding performance, and can meet the requirements of reinforced nylon materials for injection molding of products with higher dimensional precision requirements and complex structures.
Description
Technical Field
The invention relates to a reinforced nylon material for injection molding of a product with high precision and a complex structure and a preparation method thereof, belonging to the technical field of chemistry and chemical engineering.
Background
Nylon is the most widely used engineering plastic, reinforced nylon is an important member in nylon products, and the modification of reinforced nylon is always the key point of research of relevant modification factories and scientific research institutes. The common reinforced nylon has poor forming performance, can be used for injection molding of products with low dimensional accuracy and simple structure, but cannot be used for injection molding of products with high dimensional accuracy requirement and complex structure, such as plastic structural parts for mobile phones or notebooks, precise plastic gears for automobiles or mechanical equipment and the like. At present, imported reinforced nylon materials are generally adopted for injection molding of products with higher requirements, and the products are long in purchase period and expensive in price. Compared with common reinforced nylon, the nylon material has the mechanical strength of the common reinforced nylon, and also has excellent dimensional stability, demolding performance and appearance performance so as to be suitable for injection molding of products with high dimensional precision requirements and complex structures.
Nylon 1012 resin, chemical name: the polydecamoyl decamethylene diamine is prepared by using dodecanedioic acid and decamethylene diamine as raw materials, neutralizing and then further performing polycondensation. The nylon 1012 resin produced by the common process has wider molecular weight range and melt index range and poor forming stability, and can not meet the injection molding requirements of products with high precision and complex structures.
Disclosure of Invention
The invention aims to provide a reinforced nylon material for injection molding of products with high precision and complex structures and a preparation method thereof.
The technical scheme of the invention is as follows: a high-precision and complex-structure reinforced nylon material for injection molding of products is characterized by being prepared from the following raw materials, by weight, 60-80 parts of medium-low viscosity nylon 1012 resin and 19.5-40.5 parts of glass fiber; in addition, a compound processing aid accounting for 0.5 to 2 percent of the total mass of the two raw materials is added.
The preferable mixture ratio is as follows: 60-70 parts of medium-low viscosity nylon 1012 resin and 29.5-40.5 parts of glass fiber; in addition, a compound processing aid accounting for 1.0-2.0 percent of the total mass of the two raw materials is added.
The total weight part of the medium and low viscosity nylon 1012 resin and the glass fiber is 100 plus or minus 0.5.
The compound processing aid is a lubricating mold release agent, a glass fiber dewing prevention agent TAF (modified ethylene bis fatty acid amide), an antioxidant 1098 and an antioxidant 168 according to a mass ratio of 2: 0.8-1.2: 0.8-1.2: 0.8-1.2 (preferably 2: 1: 1: 1) are compounded and mixed.
The preferred lubricating and releasing agent is Ethylene Bis Stearamide (EBS) or silicone powder, wherein EBS is preferably EBSB50, the silicone powder requires the content of silicone to be more than 70% and the fineness to be more than 1000 meshes, and the silicone powder is preferred.
The glass fiber is a continuous alkali-free glass fiber with the diameter of 12-14 mu m, and the final length of the glass fiber is 0.3-0.5mm after being sheared by a related screw.
The melt index range of the low-viscosity nylon 1012 resin used in the invention is 15.6-19.2g/10min, and the melting range is 186.5-191.8 ℃. The preparation process is that on the basis of the ordinary nylon 1012 preparation process (formed by further polycondensation after the neutralization of dodecanedioic acid and decanediamine which are used as raw materials), 0.1 +/-0.02 percent of dodecanedioic acid (based on the weight of the dry salt of the nylon 1012) and 0.2 +/-0.05 percent of nucleating agent (based on the weight of the dry salt of the nylon 1012) are additionally added.
The preparation process of the reinforced nylon material comprises the following steps:
1) after weighing according to the proportion, uniformly mixing the medium-low viscosity nylon 1012 resin and the compound processing aid in a high-speed mixer;
2) when the temperature of each section of the extruder reaches the set temperature and the screw rod can be rotated by hands, adding the mixed material into the extruder (pre-cleaned) for mixing, and adding glass fiber when the standby head can stably extrude material strips; setting temperature of the extruder: the feeding section is 140-: 15-45 Hz;
3) after the extruder head discharges stably, drawing the extruded material strips, and cooling by water cooling; drying the cooled material strips by a drying machine;
4) and then granulating by a granulator, screening by a vibrating screen, drying and packaging. Drying requirements are as follows: drying at 80-100 deg.C, and controlling water content within 0.1%.
The performance index of the product is as follows: tensile strength>100 MPa; bending strength>100 MPa; impact of notch>10KJ/m2(ii) a Difference in longitudinal and transverse shrinkage<0.1; excellent mold release properties.
The preparation principle and the effect of the nylon 1012 resin of the invention are as follows: according to the invention, a proper amount of dodecanedioic acid is added on the basis of the original formula to react with the terminal amino group to play a role in end capping, so that the degree of polymerization reaction is reduced, the polymerization degree of the material is controlled, the molecular weight is further controlled, the molecular weight of the material is more uniform, and the melt index range is reduced; the addition of the nucleating agent accelerates the crystallization speed of the material, and simultaneously reduces the size of the crystal ball of the material, thereby accelerating the cooling speed of the material, further shortening the molding cycle and melting range of the material, and improving the molding stability of the material.
The invention has the beneficial effects that:
(1) the invention firstly prepares the medium-low viscosity nylon 1012 which has more uniform molecular weight, short melting range, smaller range of melting index and high dimensional precision as a base material, and provides guarantee for the material to have good dimensional stability;
(2) the length of the glass fiber is accurately controlled to be 0.3-0.5mm, and the glass fiber is uniformly distributed in the nylon resin, so that the glass fiber has excellent dimensional stability on the premise of ensuring good mechanical properties;
(3) the invention adds the compound processing aid, further improves the distribution performance of the glass fiber in the nylon on the premise of ensuring the physical and chemical properties of the product, and further improves the molding stability, the dimensional stability and the demolding performance of the material.
Drawings
FIG. 1 is a process scheme of the present invention.
Detailed Description
Example 1: preparation of middle and low viscosity nylon 1012 resin
Preparation of nylon 1012: dissolving 1.0mol of decamethylene diamine and 1.0mol of dodecanedioic acid in ethanol and/or deionized water, stirring and mixing for 50 minutes at 80 ℃ to perform a neutralization reaction; cooling and centrifuging after the reaction is finished to obtain 1012 salts; adding 1012 salt, 0.1% dodecanedioic acid (based on the weight of the 1012 dry salt), 0.2% nucleating agent (such as BRUGGOLENP22) (based on the weight of the 1012 dry salt), deionized water and antioxidant (such as phosphorus-containing antioxidant (based on the weight of the 1012 dry salt) into a polymerization kettle, heating to 230 ℃, polymerizing for 7 hours under the pressure of 1.5MPa (gauge pressure), then reducing the pressure to normal pressure, continuing to preserve the temperature for 60 minutes, sampling and detecting a melt index, starting discharging if the melt index is less than 20g/10min, continuing to maintain the pressure, determining the pressure maintaining time (about 10-20min) according to the specific melt index condition, sampling and detecting until the melt index meets the requirement, and discharging. Drying the obtained low-viscosity nylon 1012 resin at 100 ℃, and storing the resin in a moisture-proof way for later use when the moisture content is less than 0.1 percent.
The specific effects are as follows:
TABLE 1 comparison of the properties and preparation of nylon 1012 resin used in the present invention and ordinary nylon 1012 resin
Note: the data at the two ends in the range of the melting finger refers to the melting finger (the minimum melting finger) when the material is discharged finally and the melting finger (the maximum melting finger) of the material discharged initially.
Example 2:
1) mixing
Sequentially adding 80 kg of low-viscosity nylon 1012 resin and 0.5 kg of compound processing aid (prepared by compounding silicone powder, TAF, antioxidant 1098 and antioxidant 168 according to the mass ratio of 2: 1: 1: 1) into a high-speed mixer, carrying out high-speed mixing for 3min, and discharging for later use;
2) extrusion
Setting temperature of the extruder: a feeding section at 140 ℃, a melting section at 200 ℃ and 220 ℃, a machine head section at 220 ℃, a screw rotating speed: 15 Hz;
after the temperature of each section of the extruder reaches the set temperature, and when the screw rod can be rotated by hands, the mixed material is added into the extruder (cleaned in advance) for mixing, glass fiber is added when the standby head can stably extrude the material strips, and the final content of the glass fiber is controlled to be 19.5-20.5 percent (the content of the glass fiber is determined by measuring the combustion residue) by adjusting the number of strands and the feeding amount of the glass fiber;
3) after the extruder head discharges stably, drawing the extruded material strips, and cooling by water cooling; drying the cooled material strips by a drying machine;
4) then granulating by a granulator, screening and drying by a vibrating screen, and meeting the drying requirement: drying at 80 deg.C, and controlling water content within 0.1%. And then discharging and carrying out moisture-proof packaging, wherein the performance indexes of the product are shown in the following table 2.
Example 3:
70 kg of nylon 1012 resin and 1.0 kg of compound processing aid (prepared by compounding silicone powder, TAF, antioxidant 1098 and antioxidant 168 according to the mass ratio of 2: 1: 1: 1) are sequentially added into a high-speed mixer to be mixed for 5min, and then the mixture is discharged for standby.
Setting temperature of the extruder: feeding section 160 ℃, melting section 220-: 30 Hz.
The final content of the glass fiber is controlled to be 29.5-30.5% by adjusting the number of strands and feeding amount of the glass fiber.
The drying temperature was 90 ℃.
The rest is the same as example 2. The performance index of the product is shown in Table 2 below.
Example 4:
70 kg of nylon 1012 resin and 1.5 kg of compound processing aids (prepared by compounding silicone powder, TAF, antioxidant 1098 and antioxidant 168 according to the mass ratio of 2: 1: 1: 1) are sequentially added into a high-speed mixer to be mixed for 5min, and then the mixture is discharged for standby.
Setting temperature of the extruder: feeding section 160 ℃, melting section 220-: 30 Hz.
The final content of the glass fiber is controlled to be 29.5-30.5% by adjusting the number of strands and feeding amount of the glass fiber.
The drying temperature was 90 ℃.
The rest is the same as example 2. The performance index of the product is shown in Table 2 below.
Example 5:
60 kg of nylon 1012 resin and 2 kg of compound processing aids (prepared by compounding silicone powder, TAF, antioxidant 1098 and antioxidant 168 according to the mass ratio of 2: 1: 1: 1) are sequentially added into a high-speed mixer to be mixed for 8min, and then the materials are discharged for standby.
Setting temperature of the extruder: the feeding section is 180 ℃, the melting section is 230-: 45 Hz.
The final content of the glass fiber is controlled to be 39.5-40.5% by adjusting the number of strands and feeding amount of the glass fiber.
The drying temperature was 100 ℃.
The rest is the same as example 2. The performance index of the product is shown in Table 2 below.
TABLE 2 Properties of the products of examples 2-5
Note: the impact, tensile strength, bending strength, shrinkage rate and combustion residue of the simply supported beam notch are tested according to corresponding national standards, and the difference of the longitudinal and transverse shrinkage rates refers to the ratio of the difference between the maximum shrinkage rate and the minimum shrinkage rate of the material to the maximum shrinkage rate.
As can be seen from Table 2, the products prepared in examples 2-5 all meet the technical requirements, and the product prepared in example 3 has the best comprehensive performance. Therefore, the sample material is manufactured to relevant clients according to the embodiment 3 to perform injection molding on precision plastic products (precision plastic gears used on automobiles), and compared with the injection molding condition of relevant imported materials, the product can be used for injection molding qualified products by adopting the same process of the imported materials, and the use requirements of the clients can be met. The details are shown in Table 3.
TABLE 3 comparison table of injection molding conditions
Claims (8)
1. A high-precision and complex-structure reinforced nylon material for injection molding of products is characterized by being prepared from the following raw materials, by weight, 60-80 parts of medium-low viscosity nylon 1012 resin and 19.5-40.5 parts of glass fiber; in addition, a compound processing aid accounting for 0.5 to 2 percent of the total mass of the two raw materials is added; the melt index range of the medium and low viscosity nylon 1012 resin is 15.6-19.2g/10min, and the melting range is 186.5-191.8 ℃;
the compound processing aid is a lubricating mold release agent, a glass fiber exposure preventing agent TAF, an antioxidant 1098 and an antioxidant 168 according to a mass ratio of 2: 0.8-1.2: 0.8-1.2: 0.8-1.2 mixing;
the low-viscosity nylon 1012 resin is prepared by the following method: during the preparation of nylon 1012, 0.1 plus or minus 0.02 percent of dodecanedioic acid and 0.2 plus or minus 0.05 percent of nucleating agent by weight of dry salt of nylon 1012 are added in the polymerization stage; the polymerization process adopted in the polymerization stage specifically comprises the following steps: adding 1012 salt, dodecanedioic acid, nucleating agent, deionized water and antioxidant into a polymerization kettle, heating to 230 ℃, polymerizing for 7 hours under the pressure of 1.5MPa, then reducing the pressure to normal pressure, continuously preserving the heat for 60min, sampling and detecting a melt index, starting discharging if the melt index is less than 20g/10min, and otherwise, continuously maintaining the pressure until the melt index meets the requirement, and discharging.
2. The reinforced nylon material for injection molding of high-precision and complex-structure products as claimed in claim 1, wherein the lubricating and releasing agent is ethylene bis stearamide or silicone powder.
3. The reinforced nylon material for injection molding of products with high precision and complex structures as claimed in claim 2, wherein the silicone powder requires that the silicone content is more than 70% and the fineness is more than 1000 meshes.
4. The reinforced nylon material for injection molding of high-precision and complex-structure products of claim 1, wherein the glass fiber is a continuous alkali-free glass fiber with a diameter of 12-14 μm, and is sheared to a final length of 0.3-0.5 mm.
5. The reinforced nylon material for injection molding of high-precision and complex-structure products as claimed in any one of claims 1 to 4, which is prepared from the following raw materials, by weight, 60 to 70 parts of medium-low viscosity nylon 1012 resin, 29.5 to 40.5 parts of glass fiber; in addition, a compound processing aid accounting for 1.0-2.0 percent of the total mass of the two raw materials is added.
6. The preparation method of the reinforced nylon material for injection molding of the product with high precision and complex structure as claimed in any one of claims 1 to 4, which is characterized by comprising the following steps:
1) uniformly mixing the medium-low viscosity nylon 1012 resin and the compound processing aid in a high-speed mixer;
2) when the temperature of each section of the extruder reaches a set temperature and the screw rod can be rotated by hands, adding the mixed material into the extruder for mixing, and adding glass fiber when the standby head can stably extrude material strips;
3) after the extruder head discharges stably, drawing the extruded material strips, and cooling by water cooling; drying the cooled material strips by a drying machine;
4) and then granulating by a granulator, screening by a vibrating screen, drying and packaging.
7. The method according to claim 6, wherein the step 2) sets the temperature of the extruder: the feeding section is 140-: 15-45 Hz.
8. The method according to claim 6, wherein the step 4) drying requires: drying at 80-100 deg.C, and controlling water content within 0.1%.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1837286A (en) * | 2005-03-24 | 2006-09-27 | 上海赛璐化工股份有限公司 | Process for preparing high-strength wearable polyamide 1012 |
| CN102702730A (en) * | 2012-06-12 | 2012-10-03 | 中国科学院化学研究所 | Fiber/long-carbon-chain nylon in-situ composite material and preparation method |
| JP2015017248A (en) * | 2013-06-13 | 2015-01-29 | 旭化成ケミカルズ株式会社 | Glass fiber-reinforced polyamide resin composition, and molding |
| CN104497567A (en) * | 2014-12-05 | 2015-04-08 | 中国科学院化学研究所 | Long-carbon-chain nylon/calcium silicate whisker composite material as well as preparation method and application thereof |
| CN108410167A (en) * | 2018-04-09 | 2018-08-17 | 贵州省材料产业技术研究院 | Low dielectric nylon material of a kind of fiberglass reinforced and preparation method thereof |
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- 2018-11-16 CN CN201811364141.6A patent/CN109608877B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1837286A (en) * | 2005-03-24 | 2006-09-27 | 上海赛璐化工股份有限公司 | Process for preparing high-strength wearable polyamide 1012 |
| CN102702730A (en) * | 2012-06-12 | 2012-10-03 | 中国科学院化学研究所 | Fiber/long-carbon-chain nylon in-situ composite material and preparation method |
| JP2015017248A (en) * | 2013-06-13 | 2015-01-29 | 旭化成ケミカルズ株式会社 | Glass fiber-reinforced polyamide resin composition, and molding |
| CN104497567A (en) * | 2014-12-05 | 2015-04-08 | 中国科学院化学研究所 | Long-carbon-chain nylon/calcium silicate whisker composite material as well as preparation method and application thereof |
| CN108410167A (en) * | 2018-04-09 | 2018-08-17 | 贵州省材料产业技术研究院 | Low dielectric nylon material of a kind of fiberglass reinforced and preparation method thereof |
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Denomination of invention: The invention relates to a reinforced nylon material for injection molding of products with high precision and complex structure and a preparation method thereof Effective date of registration: 20211025 Granted publication date: 20210205 Pledgee: SHANDONG XINSHENG INDUSTRIAL DEVELOPMENT LLC Pledgor: SHANDONG DONGCHEN NEW TECHNOLOGY CO.,LTD. Registration number: Y2021980011243 |