CN114410008B - Non-halogen flame-retardant polypropylene pipe and preparation method thereof - Google Patents
Non-halogen flame-retardant polypropylene pipe and preparation method thereof Download PDFInfo
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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
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/10—Homopolymers or copolymers of propene
- C08L23/12—Polypropene
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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
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08L2201/00—Properties
- C08L2201/22—Halogen free composition
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/18—Applications used for pipes
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Abstract
The invention discloses a non-halogen flame-retardant polypropylene pipe, which comprises the following components in percentage by mass: 18-22% of polypropylene; 8-12% of maleic anhydride grafted polypropylene; 61-67% of non-halogen flame retardant; 3-9% of ZnMgAl-LDHs compound. The invention also discloses a preparation method of the non-halogen flame-retardant polypropylene pipe. According to the invention, the ZnMgAl-LDHs compound is used as a filling material, the non-halogen flame retardant (M) is added as a flame retardant and mixed with the maleic anhydride grafted polypropylene (PP-g-MA), and the mixed material is used as a composite flame retardant, so that the flame retardant with good performance can be obtained, the use of the halogen flame retardant is reduced, and the environment is protected. In addition, the polypropylene is subjected to maleic anhydride grafting treatment, so that the combination property is improved, and combustion is prevented more easily. In addition, the process has the advantages of convenient raw material selection, low price and production cost reduction.
Description
Technical Field
The invention belongs to the field of PPR flame retardance, and particularly relates to a non-halogen flame-retardant polypropylene pipe and a preparation method thereof. In the practical use process, the pipe is difficult to burn due to open flame and easy to self-extinguish, and toxic substances are not generated in the combustion process.
Background
Polypropylene is a colorless, odorless and nontoxic solid material, and is a thermoplastic synthetic resin with excellent performance, so that the polypropylene can be used for brightening in the fields of machinery, construction, agriculture and forestry and food packaging. And because of its excellent plasticity, polypropylene material is used in building, water pipe and structural support. However, polypropylene is very easy to burn under the condition of high temperature or fire, belongs to inflammable materials, and further makes the fire more difficult to control, which is a potential safety hazard.
When the polymer flame-retardant material is researched, the halogen-containing flame retardant is added in most of early flame-retardant methods, so that the flame-retardant effect is better and the consumption is lower. However, along with the environment-friendly and green industrialization concept, the modification research of the materials is more studied, so that good material performance is ensured, and the human body is not damaged, and the environment is not damaged. Halogen type flame retardants are easy to generate toxic and corrosive gases under the condition of combustion or high temperature, and cause secondary environmental pollution, which is contrary to the current development concept. In this case, non-halogen flame retardants are increasingly being used.
In the field of pipe production, a non-halogen flame retardant pipe is developed, so that good material performance is guaranteed, no harm is caused to human bodies, the pipe is difficult to burn when encountering open fire and easy to self-extinguish in the actual use process, toxic substances are not generated in the combustion process, and the pipe has important practical significance.
Disclosure of Invention
Aiming at the problems, the invention provides a non-halogen flame-retardant polypropylene pipe and a preparation method thereof, which solve the technical problems that the use of the traditional halogen flame retardant material is easy to generate toxic and corrosive gas, and causes harm to human body and environment, and the like.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
a non-halogen flame retardant polypropylene pipe, comprising the following components: the flame retardant comprises the following components in percentage by mass:
as a further technical scheme, the non-halogen flame retardant is an aluminophosphate flame retardant.
The invention also provides a preparation method of the non-halogen flame-retardant polypropylene pipe, which comprises the following steps:
(1) Preparing ZnMgAl-LDHs compound;
(2) Adding polypropylene granules, maleic anhydride grafted polypropylene, a non-halogen flame retardant and a ZnMgAl-LDHs compound into a mixer according to a proportion for mixing;
(3) And (3) adding the premix obtained in the step (2) into an extruder, controlling the temperature of each section of the extruder, and carrying out melt plasticization and extrusion molding.
As a further technical scheme, the preparation process of the ZnMgAl-LDHs compound in the step (1) comprises the following steps: zinc salt, magnesium salt and aluminum salt are mixed according to a mole ratio of 1:3:2 dissolving the precipitate into deionized water, starting a magnetic stirring water bath kettle, stirring uniformly, regulating the pH value to be 10.3-10.7, standing after the reaction is finished, centrifuging, washing the obtained precipitate with deionized water, placing the precipitate in an oven for drying, and grinding the obtained powder after the drying is finished to obtain the ZnMgAl-LDHs compound.
As a further technical scheme, the mixing process parameters of the mixer in the step (2) are as follows: the rotation speed is 60-80rpm, the mixing temperature is 170-185 ℃, and the mixing time is 5-10 minutes.
As a further technical scheme, in the step (3), the extruder is uniformly divided into 6 heating sections, and the temperature of each section of the extruder barrel is as follows: the 1-section heating temperature is 200+/-5 ℃, the 2-section heating temperature is 205+/-5 ℃, the 3-section heating temperature is 210+/-5 ℃, the 4-section heating temperature is 215+/-5 ℃, the 5-section heating temperature is 220+/-5 ℃, and the 6-section heating temperature is 225+/-5 ℃.
As a further technical scheme, the extruder is one of a single screw extruder, a double screw extruder or a planetary screw extruder.
The flame retardant mechanism of the invention is that the flame retardant is combined with the polymer material at high temperature to form a compact and smooth carbon layer, and the basic elements of combustion are broken to a certain extent, thereby preventing further combustion of organic matters.
Compared with the prior art, the invention has the following beneficial effects:
(1) According to the technical scheme, the ZnMgAl-LDHs compound is used as a filling material, the non-halogen flame retardant (M) is added as a flame retardant and is mixed with the maleic anhydride grafted polypropylene (PP-g-MA), so that the flame retardant with good performance can be obtained, the use of the halogen flame retardant is reduced, and harmful substances which are harmful to the environment and human health due to the generation of hydrogen halide are avoided when the material encounters high temperature or fire.
(2) The polypropylene is subjected to maleic anhydride grafting treatment, so that the dispersibility of the flame retardant material in the material is better, and the distribution is more uniform, because most of the flame retardants are polar, and when the flame retardant is combined with nonpolar polypropylene, the distribution is very easy to be uneven. Not only seriously affects the flame retardant effect, but also greatly affects the mechanical properties of the material. When the flame retardant acts, the flame retardant can be combined with polypropylene to form a carbon layer, so that the surface is smoother and smoother, and combustion is prevented more easily.
(3) The invention has the advantages of convenient selection of raw materials, low price and production cost reduction.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely, and it is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Preparation example 1
The preparation method of the non-halogen flame-retardant polypropylene pipe comprises the following steps:
(1) Preparing ZnMgAl-LDHs compound; dissolving 0.1mol of zinc salt, 0.3mol of magnesium salt and 0.2mol of aluminum salt into 250ml of deionized water, starting a magnetic stirring water bath, stirring uniformly, adjusting the pH value to 10.3, standing after the reaction is finished, performing centrifugal treatment, washing the obtained precipitate with deionized water, placing in an oven for drying, and grinding the obtained powder after the drying is finished to obtain the ZnMgAl-LDHs compound.
(2) Polypropylene granules, maleic anhydride grafted polypropylene and a non-halogen flame retardant (aluminum phosphate flame retardant such as aluminum hypophosphite is adopted in the embodiment), and ZnMgAl-LDHs compound are added into a mixer according to the proportion for mixing; the rotation speed is 70rpm, the mixing temperature is 180 ℃, and the mixing time is 8 minutes;
(3) And (3) adding the premix obtained in the step (2) into a double-screw extruder, controlling the temperature of each section of the extruder, and carrying out melt plasticization and extrusion molding. The extruder is evenly divided into 6 heating sections, and the temperature of each section of the extruder barrel is as follows: the 1-stage heating temperature is 200 ℃, the 2-stage heating temperature is 205 ℃, the 3-stage heating temperature is 210 ℃, the 4-stage heating temperature is 215 ℃, the 5-stage heating temperature is 220 ℃, and the 6-stage heating temperature is 225 ℃.
Preparation example 2
In this example, the pH was adjusted to 10.5 in the step (1), the mixing parameter in the step (2) was 60rpm, the mixing temperature was 185℃and the mixing time was 10 minutes; in the step (3), a planetary screw extruder was used, and the same as in preparation example 1 was used.
Preparation example 3
In this example, the pH was adjusted to 10.7 in step (1), the mixing parameters in step (2) were 80rpm, the mixing temperature was 170℃and the mixing time was 6 minutes; otherwise, the same as in preparation example 1 was conducted.
Proportioning examples
Mixing maleic anhydride grafted polypropylene (PP-g-MA), a non-halogen flame retardant (M) and ZnMgAl-LDHs compounds according to different proportions, wherein the proportions are shown in table 1; the polypropylene (PP), the maleic anhydride grafted polypropylene (PP-g-MA), the non-halogen flame retardant (M) and the ZnMgAl-LDHs compound are mixed according to different proportions, and the mixture ratio is shown in Table 2; and (5) mixing, and scraping the uniformly mixed materials after mixing.
TABLE 1 PP-g-MA/M/LDHs flame retardant material proportion Table
TABLE 1 proportion Table of PP/PP-g-MA/M/LDHs flame retardant materials
Taking each proportion as an example, mixing and granulating, extruding the pipe after granulating, and uniformly dividing an extruder into 6 heating sections, wherein the temperature of each section of a machine barrel of the extruder is as follows: the 1-section heating temperature is 200+/-5 ℃, the 2-section heating temperature is 205+/-5 ℃, the 3-section heating temperature is 210+/-5 ℃, the 4-section heating temperature is 215+/-5 ℃, the 5-section heating temperature is 220+/-5 ℃, and the 6-section heating temperature is 225+/-5 ℃;
sample testing and characterization
The flame retardant property of the material is tested by using TGA, limiting oxygen index and horizontal and vertical combustion test, the flame retardant property of the material is tested practically, and the formula with relatively good flame retardant property in various proportions is analyzed.
TGA thermogravimetry is a method of measuring mass of a substance as a function of temperature or time at a programmed temperature. By analyzing the thermogravimetric curve, information related to the quality of the sample and possibly the intermediate products, such as composition, thermal stability, thermal decomposition and the products produced can be obtained.
Limiting oxygen index (LOI test) refers to the volume fraction concentration of oxygen in a polymer in a mixture of oxygen and nitrogen when it is just capable of supporting its combustion. Is an index that characterizes the combustion behavior of a material. Limiting oxygen index can be measured by a candling test, where a polymer rod is burned downward under specified conditions. It is generally believed that at a limiting oxygen index of 22, the material can burn in air. A high oxygen index indicates that the material is not flammable, a low oxygen index indicates that the material is easy to burn, and it is believed that an oxygen index of <22% is a flammable material, an oxygen index between 22% -27% is a flammable material, and an oxygen index of >27% is a flame retardant material.
UL94 horizontal vertical burn test is used mainly to determine the burn performance of plastics, rubber or film under a specified fire source to determine its fire rating.
Analysis of results
TGA test analysis
And (3) researching the thermal decomposition temperature (Td) of the PP-g-MA flame-retardant composite material and the content change of final carbon residue by using a TGA (thermal decomposition A) to flame-retardant composite material test, wherein the thermal decomposition temperature is the temperature reached by 5% of the weight loss of the composite material, and the carbon residue is the final carbon residue of the composite material at 700 ℃.
Table 3 shows the data of the thermal decomposition temperature and the final carbon residue content of the flame retardant composite materials of Raw PP-g-MA and PP-g-MA50-1 to PP-g-MA50-5, and the thermal decomposition temperature of the Raw PP-g-MA material without adding non-halogen flame retardant and filler is 321 ℃ and the carbon residue content is 0.6%. After the addition of 50wt% of LDHs and 50wt% of non-halogen flame retardant, the initial thermal decomposition temperature was reduced to 173 ℃ and 310 ℃, respectively, because LDHs and non-halogen flame retardant have a lower melting point than maleic anhydride grafted polypropylene, they melt and volatilize first and a char layer is generated on the surface, increasing the char content from 0.6% to 36.7% and 22.3%, respectively.
When the PP-g-MA 50-3-PP-g-MA 50-5 flame retardant composite material is added into LDHs and non-halogen flame retardants in a certain proportion, the carbon residue is respectively increased from 0.6% to 28.7%, 30.7% and 51.4%, and the carbon residue has a great increasing trend, so that the carbon residue can be greatly increased, and the thermal stability of the PP-g-MA can be effectively improved by adding the filling material and the non-halogen flame retardants into the composite material to form a coke protection layer at high temperature.
TABLE 2 thermal decomposition temperature and final carbon residue content of Raw PP-g-MA and PP-g-MA50-1 to PP-g-MA50-5 flame retardant composite materials
Table 4 shows the data of the thermal decomposition temperature and the final carbon residue content of the flame retardant composite materials of Raw PP-g-MA and PP-g-MA30-1 to PP-g-MA30-5 together, and the thermal decomposition temperature of the Raw PP-g-MA material is 321 ℃ and the carbon residue content is 0.6 percent. After 70wt% of LDHs and 70wt% of non-halogen flame retardant are added, the thermal decomposition temperature is respectively reduced to 156 ℃ and 289 ℃, because the LDHs and the non-halogen flame retardant are decomposed in advance, so that the thermal decomposition temperature of the whole composite material is reduced, and in addition, the carbon residue is respectively increased from 0.6% to 52.4% and 42.3%, which indicates that the addition of the LDHs and the non-halogen flame retardant can effectively promote the formation of a carbon layer of the material and improve the flame retardant property.
After LDHs and non-halogen flame retardant are added into the PP-g-MA 30-3-PP-g-MA 30-5 flame retardant composite material in a certain proportion, the tendency of improving the carbon residue amount is observed to be 51.5%, 55.9% and 60.7%, which shows that the addition of a small amount of LDHs and the reduction of the proportion of the non-halogen flame retardant are beneficial to improving the carbon residue content and playing a flame retardant effect.
TABLE 3 thermal decomposition temperature and final carbon residue content of Raw PP-g-MA and PP-g-MA30-1 to PP-g-MA30-5 flame retardant composite materials
Table 5 is a summary of the thermal decomposition temperatures and final char content data for the PP flame retardant composites (A0, B1-B5), from which it can be observed that the A0 material without the addition of non-halogen flame retardant and filler had an initial thermal decomposition temperature of 404℃and a char content of 4%. After 70wt% of LDHs and 70wt% of non-halogen flame retardant are added respectively, the thermal decomposition temperature is reduced to 172 ℃ and 293 ℃, respectively, because the LDHs and the non-halogen flame retardant have lower melting points than polypropylene, decomposition is advanced and a carbon layer is generated on the surface, and the carbon residue is increased from 4% to 42.2% and 36%, respectively.
Along with the addition of a certain proportion of LDHs and a non-halogen flame retardant into the B3-B5 flame retardant composite material, the trend of improving the carbon residue amount is observed to be 39.8%, 44.3% and 45.2%, which shows that the addition of a small amount of LDHs and the reduction of the proportion of the non-halogen flame retardant can form a coke protection layer at high temperature, and the flame retardant property of the PP substrate can be effectively improved.
Table 5 PP thermal decomposition temperature and final carbon residue content data for flame retardant composite (A0, B1-B5) Table
Limiting oxygen index test and horizontal vertical Combustion test
As can be seen from the results of LOI detection and UL-94 combustion test of ZnMgAl-LDHs/M/PP-g-MA (Raw PP-g-MA, PP-g-MA 50-1-PP-g-MA 50-5), the LOI value of the Raw PP-g-MA is 18% after the combustion test of the Raw PP-g-MA test piece, and the UL-94 is NR grade, which shows that the Raw PP-g-MA has very poor flame retardant property; when 50wt% of LDHs is added into the PP-g-MA50-1 test piece, the LOI value can reach 23%, the self-extinguishing grade is reached, and the UL-94 test is improved to V-2 grade; when 50wt% of non-halogen flame retardant is added into the PP-g-MA50-2 test piece, the LOI value can reach 23%, the self-extinguishing grade is reached, and the UL-94 test is improved to V-2 grade; however, when small amounts of LDHs were added to the PP-g-MA50-3, PP-g-MA50-4 and PP-g-MA50-5 test pieces, the LOI values were maintained at 23%, indicating that the materials were raised from the original flammability level to the self-extinguishing level, and the UL-94 test was V-2, indicating that the materials were self-extinguished within 30 seconds after the fire source was removed, but still had the phenomenon of dripping.
TABLE 6 LOI detection and UL-94 Combustion test results of ZnMgAl-LDHs/M/PP-g-MA (Raw PP-g-MA, PP-g-MA 50-1-PP-g-MA 50-5)
Table 7 shows the results of LOI detection and UL-94 combustion test of ZnMgAl-LDHs/M/PP-g-MA (Raw PP-g-MA, PP-g-MA 30-1-PP-g-MA 30-5), and it can be observed from the table that the LOI value of the Raw PP-g-MA is 18%, the UL-94 is NR grade, and the flame retardant property of the Raw PP-g-MA is very poor, and the material cannot be self-extinguished within 30 seconds after a fire source is removed; after 70wt% of LDHs is added to the PP-g-MA30-1 test piece, the LOI value is increased to 33%, the flame retardance grade is reached, and the UL-94 is increased to V-0 grade; after 70wt% of non-halogen flame retardant is added into the PP-g-MA30-2 test piece, the LOI value is increased to 37%, the flame retardance grade is achieved, and the UL-94 test is also increased to V-0 grade; however, when 3wt%, 6wt% and 9wt% of LDHs are respectively added into the PP-g-MA30-3, PP-g-MA30-4 and PP-g-MA30-5 test pieces, the LOI values of the LDHs are 33%, 34% and 36% respectively along with the increase of the addition amount of the LDHs, the LOI values of the PP-g-MA30-3 to PP-g-MA30-5 respectively reach the flame retardance grades, the UL-94 test is V-0 grade, the material can be automatically extinguished within 10 seconds after the fire source is removed, no molten drop is generated, and the test results of the LOI and UL-94 test prove that the ratio of the LDHs with a small amount of components to the reduced non-halogen flame retardant is increased, so that the flame retardance of the Raw PP-g-MA can be remarkably improved.
TABLE 7 LOI detection and UL-94 Combustion test results of ZnMgAl-LDHs/M/PP-g-MA (Raw PP-g-MA, PP-g-MA 30-1-PP-g-MA 30-5)
Table 8 shows the results of LOI detection and UL-94 combustion test data of flame retardant composite materials (A0, B1-B5), from which it can be observed that the LOI value of A0 is 18%, which is a flammable grade, and that UL-94 is an NR grade, indicating that the material cannot self-extinguish within 30 seconds after the fire source is removed; after 70wt% of LDHs is added with B1, the LOI value can be increased to 36%, the flame retardance grade is achieved, and the UL-94 test is increased to V-0 grade; after 70wt% of non-halogen flame retardant is added into B2, the LOI value can be increased to 42%, the flame retardance grade is achieved, and the UL-94 is also increased to V-0 grade; after 3wt%, 6wt% and 9wt% of LDHs are added to the test pieces B3, B4 and B5 respectively, the LOI values of B3-B5 respectively reach the flame retardancy grades at 41%, 43% and 43% along with the increase of the LDHs amount, and the UL-94 test shows that the material can be automatically extinguished within 10 seconds after the fire source is removed and no molten drop is generated. The LOI and UL-94 test results prove that the addition of PP-g-MA and LDHs with a small amount of components and the reduction of the proportion of non-halogen flame retardant can improve the flame retardance.
TABLE 8 LOI detection and UL-94 burn test data for flame retardant composites (A0, B1-B5)
The flame retardant mechanism of the invention is that the flame retardant is combined with the polymer material at high temperature to form a compact and smooth carbon layer, and the basic elements of combustion are broken to a certain extent, thereby preventing further combustion of organic matters.
According to the technical scheme, the ZnMgAl-LDHs compound is used as a filling material, the non-halogen flame retardant (M) is added as a flame retardant and is mixed with the maleic anhydride grafted polypropylene (PP-g-MA), so that the flame retardant with good performance can be obtained, the use of the halogen flame retardant is reduced, and harmful substances which are harmful to the environment and human health and are generated by hydrogen halide are avoided. In addition, the polypropylene is subjected to maleic anhydride grafting treatment, so that the dispersibility of the flame retardant material in the material is better, the distribution is more uniform, and the flame retardant material is more beneficial to preventing combustion. In addition, the process has the advantages of convenient raw material selection, low price and production cost reduction.
Claims (6)
1. The non-halogen flame-retardant polypropylene pipe is characterized by comprising the following components:
the flame retardant comprises the following components in percentage by mass:
18-22% of polypropylene
Maleic anhydride grafted polypropylene 8-12%
61-64% of non-halogen flame retardant
ZnMgAl-LDHs compound 6-9%
The non-halogen flame retardant is an aluminophosphate.
2. A method for preparing the non-halogen flame retardant polypropylene pipe according to claim 1, comprising the steps of:
(1) Preparing ZnMgAl-LDHs compound;
(2) Adding polypropylene granules, maleic anhydride grafted polypropylene, a non-halogen flame retardant and a ZnMgAl-LDHs compound into a mixer according to a proportion for mixing;
(3) And (3) adding the premix obtained in the step (2) into an extruder, controlling the temperature of each section of the extruder, and carrying out melt plasticization and extrusion molding.
3. The preparation method of the non-halogen flame-retardant polypropylene pipe according to claim 2, wherein the preparation process of the ZnMgAl-LDHs compound in the step (1) is specifically as follows: zinc salt, magnesium salt and aluminum salt are mixed according to a mole ratio of 1:3:2 dissolving the precipitate into deionized water, starting a magnetic stirring water bath kettle, stirring uniformly, regulating the pH value to be 10.3-10.7, standing after the reaction is finished, centrifuging, washing the obtained precipitate with deionized water, placing the precipitate in an oven for drying, and grinding the obtained powder after the drying is finished to obtain the ZnMgAl-LDHs compound.
4. The method for preparing the non-halogen flame-retardant polypropylene pipe according to claim 2, wherein the mixing process parameters of the mixer in the step (2) are as follows: the rotation speed is 60-80rpm, the mixing temperature is 170-185 ℃, and the mixing time is 5-10 minutes.
5. The method for preparing the non-halogen flame-retardant polypropylene pipe according to claim 2, wherein in the step (3), the extruder is uniformly divided into 6 heating sections, and the temperature of each section of the extruder barrel is as follows: the 1-section heating temperature is 200+/-5 ℃, the 2-section heating temperature is 205+/-5 ℃, the 3-section heating temperature is 210+/-5 ℃, the 4-section heating temperature is 215+/-5 ℃, the 5-section heating temperature is 220+/-5 ℃, and the 6-section heating temperature is 225+/-5 ℃.
6. The method for producing a non-halogen flame retardant polypropylene pipe according to claim 2, wherein the extruder is one of a single screw extruder, a twin screw extruder or a planetary screw extruder.
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