CN111454557A - Preparation process of flame-retardant unsaturated polyester resin - Google Patents
Preparation process of flame-retardant unsaturated polyester resin Download PDFInfo
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- CN111454557A CN111454557A CN202010418762.9A CN202010418762A CN111454557A CN 111454557 A CN111454557 A CN 111454557A CN 202010418762 A CN202010418762 A CN 202010418762A CN 111454557 A CN111454557 A CN 111454557A
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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
- C08J5/10—Reinforcing macromolecular compounds with loose or coherent fibrous material characterised by the additives used in the polymer mixture
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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
- 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
- C08J5/18—Manufacture of films or sheets
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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
- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2367/06—Unsaturated polyesters
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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
- 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
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
- C08K2003/321—Phosphates
- C08K2003/322—Ammonium phosphate
- C08K2003/323—Ammonium polyphosphate
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
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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
Abstract
The invention discloses a preparation process of unsaturated polyester resin with excellent flame retardance. The process adopts unsaturated polyester resin as a base material, calcium carbonate as a filler, styrene as a cross-linking agent and a diluent, polyphosphate as a flame retardant plasticizer, aluminum hydroxide, aluminum hypophosphite, APP and the like which are compounded into a flame retardant according to a certain proportion, and a plurality of anti-shrinkage agents and glass fibers are added. Stirring with a stirrer to mix them uniformly, and finally molding in a tablet press to obtain the glass fiber reinforced plastic. The synthesized glass fiber reinforced plastic has excellent flame retardance, has no difference in bending resistance and impact resistance compared with glass fiber reinforced plastic without a flame retardant, and solves the problem of poor flame retardance of replacing traditional materials in the building and ship industries.
Description
Technical Field
The invention belongs to the field of chemical material preparation, in particular relates to a preparation process of flame-retardant unsaturated polyester resin, and particularly relates to the proportion of each component of a flame retardant.
Background
Glass Fiber Reinforced Plastics (FRP), also known as GFRP, are glass fiber reinforced plastics, generally referred to as fiberglass reinforced resins, most of which are unsaturated polyester resins, epoxy resins and phenolic resin matrices. Reinforced plastics using glass fibers or products thereof as reinforcing materials, also known as glass fiber reinforced plastics or glass fiber reinforced plastics, are essentially different from tempered glass. Because of the different kinds of resins used in the production of glass fiber reinforced plastics, there are polyester glass fiber reinforced plastics, epoxy glass fiber reinforced plastics and phenolic glass fiber reinforced plastics. Light weight, hardness, non-conductivity, stable performance, high mechanical strength, less recovery and corrosion resistance. Can replace steel to produce machine parts, automobile shells, ship shells and the like in the manufacturing industry.
In the last fifty years, the development of the glass fiber reinforced plastic material is very rapid. The glass fiber reinforced plastic has the advantages of light weight, high strength, good designability, corrosion resistance, excellent thermal performance and excellent manufacturability, and is widely applied in various fields at present. The glass fiber reinforced plastic has many excellent characteristics, such as acid and alkali corrosion resistance and the like. At present, the pipeline product made of the glass fiber reinforced plastics can be used in various industries such as petroleum processing and the like. The glass fiber reinforced plastic product can replace the traditional metal material, not only has longer service time, but also has less cost. The glass fiber reinforced plastic pipeline can well avoid the loss caused by the corrosion of the pipeline. At present, the glass fiber reinforced plastic pipeline is widely applied to petrochemical industry, seawater desalination, sewage treatment projects and urban water supply systems.
Through years of development, the glass fiber reinforced plastic composite material industry in China has made great progress in many aspects. It has reached a high level in terms of production technology, product type, production scale, etc., and the yield has also reached a high level. It is second in the world, and the development of matrix resins for the preparation of glass fiber reinforced plastics is also very rapid. However, the matrix resins of china are far less well developed in terms of technical-level product quality, particularly in the development and application of new technologies and new products, and further research is required.
At present, the glass fiber reinforced plastics are mainly used for producing land transportation tools, and the total output accounts for about ten percent of China. The method is mainly used for automobiles and trains. Glass fiber reinforced plastic can be used as an automobile part and can be used for producing an automobile integral body, such as the integral body of the famous automobile schofland in the United states, and is made of glass molded by mechanical thermoplastic plastics. The glass fiber reinforced plastic composite SMC (sheet molding compound) has the advantages of light weight (209 percent lighter than a common automobile body), low oil consumption (8 to 10 percent lower than the common automobile body) and much higher salt corrosion resistance than a metal material. The glass fiber reinforced plastic products are also widely applied to passenger cars, such as car facies, floors, armrest window frames, seats and the like which are all made of SMC materials, and the glass fiber reinforced plastic products have the advantages of light weight, corrosion resistance, good heat preservation, elegant appearance and convenience in cleaning. The glass fiber reinforced plastics also have great application in the aspects of rail transit, high-speed rail and other interior decoration. In recent years, glass fiber reinforced plastics have become a substitute for conventional materials in the construction and marine industries. The method has the advantages of light weight, high strength, corrosion resistance, good thermal property, good designability and excellent manufacturability, and has very wide prospect.
However, most of the matrix resins of the glass fiber reinforced plastics are organic polymers, all of which are flammable and easy to burn under certain conditions, and the polymer burning is a complex and violent thermal oxidation process and is often accompanied with the generation of flames, dense smoke and toxic gases.
General glass fiber reinforced plastics are usually subjected to flame retardant modification by adopting an additive method and a reactive method, the price of a reactive flame retardant system is high, the popularization and the application of the reactive flame retardant system are limited, and products of about nine percent in the world are modified by an additive flame retardant.
Because of the limited technical level in China, the additive modification is adopted in large quantity at present. In general, the additive type flame-retardant glass fiber reinforced plastic can meet the fire-proof requirement of common buildings when the oxygen index reaches 27.
The smoke and toxicity of the glass fiber reinforced plastic during combustion are more and more valued, and the soundness and the perfection of the fireproof safety performance of the glass fiber reinforced plastic are imperative. Therefore, the novel additive type flame-retardant glass fiber reinforced plastic is rapidly and vigorously developed by combining the national conditions to form large-scale production, and the method has great significance for adapting to the future material development trend in the glass fiber reinforced plastic industry, enhancing the market competitiveness of the glass fiber reinforced plastic and expanding the application field of the glass fiber reinforced plastic.
Disclosure of Invention
The preparation process of the flame-retardant unsaturated polyester resin is characterized by comprising the following steps of:
the invention takes unsaturated polyester resin as a matrix material, calcium carbonate as a filler, styrene as a cross-linking agent and a diluent, polyphosphate as a flame retardant plasticizer, tert-butyl perbenzoate as an initiator, aluminum hydroxide, aluminum hypophosphite, APP and the like as flame retardants, and a plurality of anti-shrinkage agents and glass fibers are added. Stirring with a stirrer to mix them uniformly, and finally molding in a tablet press to obtain the glass fiber reinforced plastic. A contrast sample is prepared according to the scheme, and the structural performance of the glass fiber reinforced plastic is characterized by the bending strength tester, the impact strength tester, the oxygen index tester and the tensile strength tester, so that the flame retardant capability is greatly improved.
Detailed Description
Example 1
(1) 100g of unsaturated polyester resin and 42g of anti-shrinking agent are weighed by an electronic balance, and then 85.2g of calcium carbonate, 3.6g of zinc stearate, 14.2g of styrene, 1.7g of tert-butyl perbenzoate and 5.7g of mA-25C are weighed.
(2) Weighing the materials in the step 1, putting the materials into a container, adding 21.3g of APP, 1.42g of aluminum hypophosphite and 1.42g of aluminum hydroxide, wherein the ratio is 15: 1: 1, mixing the materials, turning on an electric stirrer, adjusting a rotating speed knob to a proper position, and stirring the materials to uniformly mix the materials.
(3) And uniformly spreading glass fibers on the stirred material, uniformly mixing, putting into an oven, and curing for 5 hours at the temperature of 45 ℃. A mold with the thickness of 4mm is selected, and the material is poured into the mold and placed between an upper plate and a lower plate of a flat vulcanizing machine. After high-temperature high-pressure solidification for 15min, the mold is replaced by a lower pressing plate, and the pressing plate is lifted to be cooled for 2 min.
(4) Waiting for a cooling process. And (5) taking out the tablet after the whole tabletting process is finished. The plate was carefully removed with a steel knife and demolded for finishing.
Example 2
(1) 200g of unsaturated polyester resin and 84g of anti-shrinking agent are weighed by an electronic balance, and 170.4g of calcium carbonate, 7.2g of zinc stearate, 28.4g of styrene, 3.4g of tert-butyl perbenzoate and 11.4g of mA-25C are weighed.
(2) Weighing the materials in the step 1, putting the materials into a container, adding 28.4g of APP and 5.68g of aluminum hydroxide, wherein the ratio is 4: 1, mixing the materials, turning on an electric stirrer, adjusting a rotating speed knob to a proper position, and stirring the materials to uniformly mix the materials.
(3) And uniformly spreading glass fibers on the stirred material, uniformly mixing, putting into an oven, and curing for 5 hours at the temperature of 45 ℃. A mold with the thickness of 4mm is selected, and the material is poured into the mold and placed between an upper plate and a lower plate of a flat vulcanizing machine. After high-temperature high-pressure solidification for 15min, the mold is replaced by a lower pressing plate, and the pressing plate is lifted to be cooled for 2 min.
(4) Waiting for a cooling process. And (5) taking out the tablet after the whole tabletting process is finished. The plate was carefully removed with a steel knife and demolded for finishing.
Example 3
(1) 100g of unsaturated polyester resin and 42g of anti-shrinking agent are weighed by an electronic balance, and then 85.2g of calcium carbonate, 3.6g of zinc stearate, 14.2g of styrene, 1.7g of tert-butyl perbenzoate and 5.7g of mA-25C are weighed.
(2) Weighing the materials in the step 1, putting the materials into a container, adding 5.68g of APP and 28.4g of aluminum hypophosphite, wherein the ratio is 1: 4, mixing, turning on the electric stirrer, adjusting the rotating speed knob to a proper position, and stirring to uniformly mix.
(3) And uniformly spreading glass fibers on the stirred material, uniformly mixing, putting into an oven, and curing for 5 hours at the temperature of 45 ℃. A mold with the thickness of 4mm is selected, and the material is poured into the mold and placed between an upper plate and a lower plate of a flat vulcanizing machine. After high-temperature high-pressure solidification for 15min, the mold is replaced by a lower pressing plate, and the pressing plate is lifted to be cooled for 2 min.
(4) Waiting for a cooling process. And (5) taking out the tablet after the whole tabletting process is finished. The plate was carefully removed with a steel knife and demolded for finishing.
Example 4
(1) 100g of unsaturated polyester resin and 42g of anti-shrinking agent are weighed by an electronic balance, and then 85.2g of calcium carbonate, 3.6g of zinc stearate, 14.2g of styrene, 1.7g of tert-butyl perbenzoate and 5.7g of mA-25C are weighed.
(2) Weighing the materials in the step 1, putting the materials into a container, adding 35.5g of APP, 0.71g of aluminum hypophosphite and 2.84g of aluminum hydroxide, and mixing the materials in a ratio of 50: 1: 4, mixing, turning on the electric stirrer, adjusting the rotating speed knob to a proper position, and stirring to uniformly mix.
(3) And uniformly spreading glass fibers on the stirred material, uniformly mixing, putting into an oven, and curing for 5 hours at the temperature of 45 ℃. A mold with the thickness of 4mm is selected, and the material is poured into the mold and placed between an upper plate and a lower plate of a flat vulcanizing machine. After high-temperature high-pressure solidification for 15min, the mold is replaced by a lower pressing plate, and the pressing plate is lifted to be cooled for 2 min.
(4) Waiting for a cooling process. And (5) taking out the tablet after the whole tabletting process is finished. The plate was carefully removed with a steel knife and demolded for finishing.
Example 5
(1) 100g of unsaturated polyester resin and 42g of anti-shrinking agent are weighed by an electronic balance, and then 85.2g of calcium carbonate, 3.6g of zinc stearate, 14.2g of styrene, 1.7g of tert-butyl perbenzoate and 5.7g of mA-25C are weighed.
(2) Weighing the materials in the step 1, putting the materials into a container, adding 5.68g of APP and 28.4g of aluminum hydroxide according to the proportion of 1: 4, mixing, turning on the electric stirrer, adjusting the rotating speed knob to a proper position, and stirring to uniformly mix.
(3) And uniformly spreading glass fibers on the stirred material, uniformly mixing, putting into an oven, and curing for 5 hours at the temperature of 45 ℃. A mold with the thickness of 4mm is selected, and the material is poured into the mold and placed between an upper plate and a lower plate of a flat vulcanizing machine. After high-temperature high-pressure solidification for 15min, the mold is replaced by a lower pressing plate, and the pressing plate is lifted to be cooled for 2 min.
(4) Waiting for a cooling process. And (5) taking out the tablet after the whole tabletting process is finished. The plate was carefully removed with a steel knife and demolded for finishing.
Oxygen index of each example
Sample name | Blank test | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 |
Oxygen index | 21% | 26.7% | 25.9% | 25.6% | 30.9% | 25.4% |
Through an oxygen index test, in the added flame retardant, the higher the APP content ratio is, and when the ratio of aluminum hydroxide to aluminum hypophosphite is similar, the more the flame retardant performance is improved.
Comparative example
Comparative example 1
(1) 100g of unsaturated polyester resin and 42g of anti-shrinking agent are weighed by an electronic balance, and then 85.2g of calcium carbonate, 3.6g of zinc stearate, 14.2g of styrene, 1.7g of tert-butyl perbenzoate and 5.7g of mA-25C are weighed.
(2) Weighing the materials in the step 1, putting the materials into a container, adding 14.2g of APP, mixing the materials, turning on an electric stirrer, adjusting a rotating speed knob to a proper position, and stirring the materials to uniformly mix the materials.
(3) And uniformly spreading glass fibers on the stirred material, uniformly mixing, putting into an oven, and curing for 5 hours at the temperature of 45 ℃. A mold with the thickness of 4mm is selected, and the material is poured into the mold and placed between an upper plate and a lower plate of a flat vulcanizing machine. After high-temperature high-pressure solidification for 15min, the mold is replaced by a lower pressing plate, and the pressing plate is lifted to be cooled for 2 min.
(4) Waiting for a cooling process. And (5) taking out the tablet after the whole tabletting process is finished. The plate was carefully removed with a steel knife and demolded for finishing.
Comparative example 2
(1) 100g of unsaturated polyester resin and 42g of anti-shrinking agent are weighed by an electronic balance, and then 85.2g of calcium carbonate, 3.6g of zinc stearate, 14.2g of styrene, 1.7g of tert-butyl perbenzoate and 5.7g of mA-25C are weighed.
(2) Weighing the materials in the step 1, putting the materials into a container, adding 14.2g of aluminum hydroxide, mixing the materials, turning on an electric stirrer, adjusting a rotating speed knob to a proper position, and stirring the materials to uniformly mix the materials.
(3) And uniformly spreading glass fibers on the stirred material, uniformly mixing, putting into an oven, and curing for 5 hours at the temperature of 45 ℃. A mold with the thickness of 4mm is selected, and the material is poured into the mold and placed between an upper plate and a lower plate of a flat vulcanizing machine. After high-temperature high-pressure solidification for 15min, the mold is replaced by a lower pressing plate, and the pressing plate is lifted to be cooled for 2 min.
(4) Waiting for a cooling process. And (5) taking out the tablet after the whole tabletting process is finished. The plate was carefully removed with a steel knife and demolded for finishing.
Comparative example 3
(1) 100g of unsaturated polyester resin and 42g of anti-shrinking agent are weighed by an electronic balance, and then 85.2g of calcium carbonate, 3.6g of zinc stearate, 14.2g of styrene, 1.7g of tert-butyl perbenzoate and 5.7g of mA-25C are weighed.
(2) Weighing the materials in the step 1, putting the materials into a container, adding 14.2g of aluminum hypophosphite, mixing the materials, turning on an electric stirrer, adjusting a rotating speed knob to a proper position, and stirring the materials to uniformly mix the materials.
(3) And uniformly spreading glass fibers on the stirred material, uniformly mixing, putting into an oven, and curing for 5 hours at the temperature of 45 ℃. A mold with the thickness of 4mm is selected, and the material is poured into the mold and placed between an upper plate and a lower plate of a flat vulcanizing machine. After high-temperature high-pressure solidification for 15min, the mold is replaced by a lower pressing plate, and the pressing plate is lifted to be cooled for 2 min.
(4) Waiting for a cooling process. And (5) taking out the tablet after the whole tabletting process is finished. The plate was carefully removed with a steel knife and demolded for finishing.
Comparative example 4
(1) 100g of unsaturated polyester resin and 42g of anti-shrinking agent are weighed by an electronic balance, and then 85.2g of calcium carbonate, 3.6g of zinc stearate, 14.2g of styrene, 1.7g of tert-butyl perbenzoate and 5.7g of mA-25C are weighed.
(2) Weighing the materials in the step 1, putting the materials into a container, adding 28.4g of APP, mixing the materials, turning on an electric stirrer, adjusting a rotating speed knob to a proper position, and stirring the materials to uniformly mix the materials.
(3) And uniformly spreading glass fibers on the stirred material, uniformly mixing, putting into an oven, and curing for 5 hours at the temperature of 45 ℃. A mold with the thickness of 4mm is selected, and the material is poured into the mold and placed between an upper plate and a lower plate of a flat vulcanizing machine. After high-temperature high-pressure solidification for 15min, the mold is replaced by a lower pressing plate, and the pressing plate is lifted to be cooled for 2 min.
(4) Waiting for a cooling process. And (5) taking out the tablet after the whole tabletting process is finished. The plate was carefully removed with a steel knife and demolded for finishing.
Comparative example 5
(1) 100g of unsaturated polyester resin and 42g of anti-shrinking agent are weighed by an electronic balance, and then 85.2g of calcium carbonate, 3.6g of zinc stearate, 14.2g of styrene, 1.7g of tert-butyl perbenzoate and 5.7g of mA-25C are weighed.
(2) Weighing the materials in the step 1, putting the materials into a container, adding 28.4g of aluminum hydroxide, mixing the materials, turning on an electric stirrer, adjusting a rotating speed knob to a proper position, and stirring the materials to uniformly mix the materials.
(3) And uniformly spreading glass fibers on the stirred material, uniformly mixing, putting into an oven, and curing for 5 hours at the temperature of 45 ℃. A mold with the thickness of 4mm is selected, and the material is poured into the mold and placed between an upper plate and a lower plate of a flat vulcanizing machine. After high-temperature high-pressure solidification for 15min, the mold is replaced by a lower pressing plate, and the pressing plate is lifted to be cooled for 2 min.
(4) Waiting for a cooling process. And (5) taking out the tablet after the whole tabletting process is finished. The plate was carefully removed with a steel knife and demolded for finishing.
Comparative example 6
(1) 100g of unsaturated polyester resin and 42g of anti-shrinking agent are weighed by an electronic balance, and then 85.2g of calcium carbonate, 3.6g of zinc stearate, 14.2g of styrene, 1.7g of tert-butyl perbenzoate and 5.7g of mA-25C are weighed.
(2) Weighing the materials in the step 1, putting the materials into a container, adding 28.4g of aluminum hypophosphite, mixing the materials, turning on an electric stirrer, adjusting a rotating speed knob to a proper position, and stirring the materials to uniformly mix the materials.
(3) And uniformly spreading glass fibers on the stirred material, uniformly mixing, putting into an oven, and curing for 5 hours at the temperature of 45 ℃. A mold with the thickness of 4mm is selected, and the material is poured into the mold and placed between an upper plate and a lower plate of a flat vulcanizing machine. After high-temperature high-pressure solidification for 15min, the mold is replaced by a lower pressing plate, and the pressing plate is lifted to be cooled for 2 min.
(4) Waiting for a cooling process. And (5) taking out the tablet after the whole tabletting process is finished. The plate was carefully removed with a steel knife and demolded for finishing.
Comparative oxygen index
Sample name | Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 | Comparative example 5 | Comparative example 6 |
Oxygen index | 23.8% | 23.3% | 23.1% | 24.7% | 23.5% | 23.0% |
Mechanical properties of each example and comparative example
Sample name | Impact strength/kJ/m2 | Flexural Strength/MPa |
Example 1 | 10.78 | 56.99 |
Example 2 | 10.56 | 57.13 |
Example 3 | 8.42 | 48.02 |
Example 4 | 11.02 | 57.26 |
Example 5 | 12.14 | 46.35 |
Comparative example 1 | 11.26 | 59.01 |
Comparative example 2 | 12.26 | 46.03 |
Comparative example 3 | 12.24 | 48.03 |
Comparative example 4 | 8.24 | 55.98 |
Comparative example 5 | 9.86 | 39.26 |
Comparative example 6 | 8.42 | 47.45 |
(1) Through the oxygen index test, APP is found to have the most obvious improvement on the flame retardant performance of the glass fiber reinforced plastic, and aluminum hydroxide is used as the second thing, and aluminum hypophosphite is used as the weakest thing. But with the increase of the amount of APP, aluminum hypophosphite and aluminum hydroxide, the impact strength of the glass fiber reinforced plastic is reduced. It is possible that the crosslinking density of the glass fiber reinforced plastic is decreased due to the increase of the flame retardant, resulting in the decrease of the impact strength and the bending strength.
(2) According to the invention, by compounding and proportioning the three flame retardants, when APP10-30g, aluminum hypophosphite 10-25g and aluminum hydroxide 10-25g are contained in the composite flame retardant, a sample with obviously improved flame retardant property and unaffected mechanical properties can be obtained.
Claims (7)
1. The preparation process of the flame-retardant unsaturated polyester resin is characterized by comprising the following steps of:
(1) under the conditions of normal temperature and normal pressure, a certain amount of unsaturated polyester resin is weighed by an electronic balance, and then a proper amount of raw materials such as calcium carbonate, a flame retardant, an auxiliary agent and the like are weighed according to a formula; mixing the weighed unsaturated polyester resin with calcium carbonate and various auxiliaries, adding the flame retardant in the parts shown in the formula, and stirring the mixture by using an electric stirrer to uniformly mix the mixture; initially curing for 4-8 hours;
(2) putting the material into a mold, and carrying out compression molding to obtain the glass fiber reinforced plastic added with the flame retardant;
10-30g of flame retardant APP, 10-25g of aluminum hypophosphite and 10-25g of aluminum hydroxide, wherein the flame retardant APP is added in the step (1).
2. The process according to claim 1), wherein the unsaturated polyester resin used in step 1) is 80-400g, the calcium carbonate is 80-400g, and the auxiliary agent is a cross-linking agent, a lubricant, an initiator, mA-25C, or the like.
3. The process for preparing the flame-retardant unsaturated polyester resin according to claim 2, wherein the initiator is tert-butyl perbenzoate in an amount of 1 to 6 g; the amount of mA-25C is 4-20 g.
4. The process according to claim 1, wherein the unsaturated polyester resin is MPS-520, the anti-shrinkage agent is MPS-954C, the lubricant is zinc stearate, and the crosslinking agent is styrene.
5. The process according to claim 1, wherein the initial curing temperature is 40 to 60 degrees; the curing temperature is 130 ℃ and 190 ℃, and the curing time is 10-60 minutes.
6. The process according to claim 1, wherein the amount of the glass fiber is 4 to 30 g.
7. The process according to claim 6, wherein the anti-shrinking agent is 2.5 to 100g, the amount of zinc stearate is 3 to 30g, and the amount of styrene is 10 to 100 g.
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Cited By (1)
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CN112852134A (en) * | 2021-01-18 | 2021-05-28 | 南京经略复合材料有限公司 | Additive flame-retardant unsaturated polyester resin and preparation method thereof |
Citations (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS52117979A (en) * | 1976-03-30 | 1977-10-03 | Hitachi Chem Co Ltd | Flame-retardant unsaturated polyester resin molded articles |
US20030083420A1 (en) * | 2001-10-23 | 2003-05-01 | Koito Manufacturing Co., Ltd. | Unsaturated polyester resin composition, cured unsaturated polyester resin and lamp reflecting mirror base |
CN102504123A (en) * | 2011-11-08 | 2012-06-20 | 桂林电器科学研究院 | Self-lubricating wear-resisting unsaturated polyester molding compound and preparation method thereof |
CN103059533A (en) * | 2013-01-16 | 2013-04-24 | 合肥杰事杰新材料股份有限公司 | Expanding flame-retardant glass fiber reinforced unsaturated polyester composite material and preparation method thereof |
JP2013087133A (en) * | 2011-10-13 | 2013-05-13 | Showa Denko Kk | Thermosetting resin composition, sheet molding compound and molded article |
CN103102635A (en) * | 2013-02-20 | 2013-05-15 | 合肥杰事杰新材料股份有限公司 | High efficiency halogen-free flame retardant unsaturated polyester molding material and preparation method thereof |
CN103524975A (en) * | 2013-10-28 | 2014-01-22 | 北京福润德复合材料有限责任公司 | Halogen-free flame-retardant highly-heat-resistant unsaturated polyester glass fiber composite material |
US20180223058A1 (en) * | 2015-08-11 | 2018-08-09 | Showa Denko K.K. | Resin composition, cured product thereof, and friction stir welding method |
CN109722058A (en) * | 2017-10-31 | 2019-05-07 | 江苏创曦复合材料科技有限公司 | A kind of glass reinforced plastic pultrusion flame-retarded resin and preparation method thereof |
WO2020080412A1 (en) * | 2018-10-19 | 2020-04-23 | ジャパンコンポジット株式会社 | Unsaturated polyester resin composition, molding material, molded article and battery pack case for electric vehicles |
-
2020
- 2020-05-18 CN CN202010418762.9A patent/CN111454557A/en active Pending
Patent Citations (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS52117979A (en) * | 1976-03-30 | 1977-10-03 | Hitachi Chem Co Ltd | Flame-retardant unsaturated polyester resin molded articles |
US20030083420A1 (en) * | 2001-10-23 | 2003-05-01 | Koito Manufacturing Co., Ltd. | Unsaturated polyester resin composition, cured unsaturated polyester resin and lamp reflecting mirror base |
JP2013087133A (en) * | 2011-10-13 | 2013-05-13 | Showa Denko Kk | Thermosetting resin composition, sheet molding compound and molded article |
CN102504123A (en) * | 2011-11-08 | 2012-06-20 | 桂林电器科学研究院 | Self-lubricating wear-resisting unsaturated polyester molding compound and preparation method thereof |
CN103059533A (en) * | 2013-01-16 | 2013-04-24 | 合肥杰事杰新材料股份有限公司 | Expanding flame-retardant glass fiber reinforced unsaturated polyester composite material and preparation method thereof |
CN103102635A (en) * | 2013-02-20 | 2013-05-15 | 合肥杰事杰新材料股份有限公司 | High efficiency halogen-free flame retardant unsaturated polyester molding material and preparation method thereof |
CN103524975A (en) * | 2013-10-28 | 2014-01-22 | 北京福润德复合材料有限责任公司 | Halogen-free flame-retardant highly-heat-resistant unsaturated polyester glass fiber composite material |
US20180223058A1 (en) * | 2015-08-11 | 2018-08-09 | Showa Denko K.K. | Resin composition, cured product thereof, and friction stir welding method |
CN109722058A (en) * | 2017-10-31 | 2019-05-07 | 江苏创曦复合材料科技有限公司 | A kind of glass reinforced plastic pultrusion flame-retarded resin and preparation method thereof |
WO2020080412A1 (en) * | 2018-10-19 | 2020-04-23 | ジャパンコンポジット株式会社 | Unsaturated polyester resin composition, molding material, molded article and battery pack case for electric vehicles |
Non-Patent Citations (1)
Title |
---|
林勇强: "基于气相—凝聚相结合的含磷阻燃不饱和聚酯树脂研究", 《中国优秀博硕士学位论文全文数据库(博士) 工程科技Ⅰ辑》 * |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112852134A (en) * | 2021-01-18 | 2021-05-28 | 南京经略复合材料有限公司 | Additive flame-retardant unsaturated polyester resin and preparation method thereof |
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