CN114940780B - Tetra-amide nucleating agent and polypropylene composition - Google Patents

Tetra-amide nucleating agent and polypropylene composition Download PDF

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CN114940780B
CN114940780B CN202210243749.3A CN202210243749A CN114940780B CN 114940780 B CN114940780 B CN 114940780B CN 202210243749 A CN202210243749 A CN 202210243749A CN 114940780 B CN114940780 B CN 114940780B
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polypropylene
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benzene
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CN114940780A (en
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张文龙
于捷
王艳丽
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Puenejing New Energy Materials Shanghai Co ltd
Pulan Polyolefin Technology Development Shanghai Co ltd
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00Use of organic ingredients
    • C08K5/16Nitrogen-containing compounds
    • C08K5/20Carboxylic acid amides
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    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C233/00Carboxylic acid amides
    • C07C233/01Carboxylic acid amides having carbon atoms of carboxamide groups bound to hydrogen atoms or to acyclic carbon atoms
    • C07C233/02Carboxylic acid amides having carbon atoms of carboxamide groups bound to hydrogen atoms or to acyclic carbon atoms having nitrogen atoms of carboxamide groups bound to hydrogen atoms or to carbon atoms of unsubstituted hydrocarbon radicals
    • C07C233/04Carboxylic acid amides having carbon atoms of carboxamide groups bound to hydrogen atoms or to acyclic carbon atoms having nitrogen atoms of carboxamide groups bound to hydrogen atoms or to carbon atoms of unsubstituted hydrocarbon radicals with carbon atoms of carboxamide groups bound to acyclic carbon atoms of an acyclic saturated carbon skeleton
    • C07C233/07Carboxylic acid amides having carbon atoms of carboxamide groups bound to hydrogen atoms or to acyclic carbon atoms having nitrogen atoms of carboxamide groups bound to hydrogen atoms or to carbon atoms of unsubstituted hydrocarbon radicals with carbon atoms of carboxamide groups bound to acyclic carbon atoms of an acyclic saturated carbon skeleton having the nitrogen atom of at least one of the carboxamide groups bound to a carbon atom of a six-membered aromatic ring
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    • C08L2205/24Crystallisation aids

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Abstract

The invention provides a tetra-amide nucleating agent, which at least comprises a tetra-amide benzene derivative with a structure shown as a formula (I), wherein R 1 、R 2 、R 3 And R is 4 Independently selected from alkyl, aryl, cycloalkyl or alkylated substituted aryl. The present invention also provides a polypropylene composition comprising an effective amount of a tetra-amide type nucleating agent in polypropylene. The tetra-amide nucleating agent has the unexpected effect and can effectively improve the mechanical properties such as crystallinity, forming speed, rigidity and the like of the polypropylene material. The tetra-amide nucleating agent disclosed by the invention has the advantages of no peculiar smell, good compatibility with materials, easiness in dispersion and no precipitation, improves the performance of polypropylene materials, and widens the application field of the polypropylene materials.

Description

Tetra-amide nucleating agent and polypropylene composition
Technical Field
The invention relates to the technical field of polymer preparation, in particular to a tetra-amide nucleating agent and a polypropylene composition prepared by adopting the nucleating agent.
Background
Polypropylene as a general thermoplastic resin has the advantages of no toxicity, good heat resistance, good corrosion resistance, excellent electrical insulation, higher heat distortion temperature, easy processing, low cost and the like, and is widely applied to life, but has many defects and drawbacks such as brittleness, easy fracture, low heat resistance temperature, low bending strength, poor transparency, poor conductive performance and the like, which lead to a narrower practical application range. The above disadvantages can be effectively ameliorated by synergistic action through the addition of high efficiency nucleating agents. The polypropylene modified by the nucleating agent has higher crystallinity, and the crystallization speed and the crystallization temperature are also improved, thereby being convenient for rapid processing and forming; and the nucleating agent can lead the spherulitic size of the polypropylene to be smaller and uniform, and improve the mechanical property and the optical property of the polypropylene. Further widens the application field, and has good rigidity, transparency, surface gloss and heat deformation resistance under relatively low concentration.
The nucleating agent is mainly classified into an inorganic nucleating agent and an organic nucleating agent. The organic nucleating agent has good compatibility with the polypropylene matrix and high nucleating efficiency, and is widely used all the time. Wherein the aromatic amide is an organic nucleating agent with high nucleating efficiency, difficult decomposition at high temperature and excellent comprehensive performance, and is a product prepared by the reaction of an amine compound and an acylating agent. The nucleating agent has good nucleating effect and low cost, and can endow polypropylene with good transparency, rigidity and heat deformation resistance. Along with the expansion of polypropylene application, the market puts higher demands on various properties of polypropylene materials including mechanical properties. Although the existing nucleating agents provide a certain improvement, they are not fully satisfactory, and therefore how to develop new nucleating agents further to improve the performance of polypropylene materials is a problem to be solved.
Disclosure of Invention
The invention aims to provide a tetra-amide type nucleating agent and a polypropylene composition prepared by adopting the tetra-amide type nucleating agent, so as to solve the defects in the prior art.
In a first aspect, the present invention provides a tetra-amide type nucleating agent, which at least comprises a tetra-amide benzene derivative having a structure as shown in formula (I):
Figure SMS_1
wherein R is 1 、R 2 、R 3 And R is 4 Independently selected from alkyl, aryl, cycloalkyl or alkylated substituted aryl. Preferably, R 1 、R 2 、R 3 And R is 4 Independently selected from isopropyl, n-butyl, isobutyl, 2-ethylhexyl. More preferably, R 1 、R 2 、R 3 And R is 4 Is the same substituent and is selected from isopropyl, n-butyl, isobutyl, 2-ethylhexyl. As a more preferable technical scheme, R 1 、R 2 、R 3 And R is 4 Is isobutyl.
The tetra-amide type nucleating agent of the present invention may contain only a single tetra-amide benzene derivative, for example, 1,3,4, 6-tetra-isobutyl amide benzene, or may contain more than one tetra-amide benzene derivative. Of course, other polypropylene nucleating agents commonly used in the art, such as polycyclic aromatic hydrocarbon nucleating agents, organic acid and salt nucleating agents, inorganic oxide nucleating agents, and the like, may also be further included.
The preparation method of the tetra-amide benzene derivative comprises the following steps:
s1, taking m-dichlorobenzene as a raw material, and performing nitration reaction to obtain an intermediate 1, 5-dichloro-2, 4-dinitrobenzene;
s2, subjecting the intermediate 1, 5-dichloro-2, 4-dinitrobenzene obtained in the step S1 to amination reaction to obtain an intermediate 4, 6-dinitro-1, 3-phenylenediamine;
s3, carrying out reduction reaction on the intermediate 4, 6-binitro-1, 3-phenylenediamine obtained in the step S2 to obtain an intermediate 1,2,4, 5-benzene tetramine tetrahydrochloride;
and S4, carrying out acylation reaction on the intermediate 1,2,4, 5-benzene tetramine tetra-hydrochloride obtained in the step S3 to obtain the tetra-amide benzene derivative.
As a preferable technical scheme, the preparation method of the tetra-amide benzene derivative specifically comprises the following steps:
s1, adding m-dichlorobenzene into a nitrifying reagent, heating and stirring for reaction, and separating and purifying to obtain an intermediate 1, 5-dichloro-2, 4-dinitrobenzene after the reaction is completed;
s2, dispersing the intermediate 1, 5-dichloro-2, 4-dinitrobenzene obtained in the step S1 in a proper amount of ethylene glycol, heating and stirring, adding an amination reagent, separating solids after the reaction is completed, and drying to obtain an intermediate 4, 6-dinitro-1, 3-phenylenediamine;
s3, dispersing the intermediate 4, 6-dinitro-1, 3-phenylenediamine obtained in the step S2 in a mixed solution of concentrated HC (hydrogen chloride) and ethanol, heating and stirring, dissolving a reducing reagent in a proper amount of ethanol, adding the ethanol into a reaction solution, stirring for reaction, and separating a white powder product after the reaction is completed to obtain an intermediate 1,2,4, 5-benzene tetramine tetrahydrochloride;
s4, dissolving the intermediate 1,2,4, 5-benzene tetramine tetra-hydrochloride obtained in the step S3 in acetonitrile, stirring, adding acyl chloride, slowly dripping weak base, stirring for reaction, and separating to obtain the tetra-amide benzene derivative after the reaction is completed.
Preferably, the nitrifying reagent in step S1 is a concentrated sulfuric acid/potassium nitrate mixture or a concentrated sulfuric acid/concentrated nitric acid mixture;
preferably, the amination reagent in step S2 is ammonia gas;
preferably, in step S3, the reducing agent is tin dichloride or metallic tin;
preferably, the weak base in step S4 is triethylamine, pyridine or a homologue thereof.
The acyl chloride in the step S4 is selected from one or more of alkyl acyl chloride, aryl acyl chloride, cycloalkyl acyl chloride or alkylated substituted aryl acyl chloride.
Preferably, the acyl chloride is selected from one or more of isobutyryl chloride, n-pentanoyl chloride, isopentanoyl chloride or 2-ethylhexanoyl chloride.
In a second aspect of the present invention, there is provided a polypropylene composition comprising an effective amount of the tetra-amide type nucleating agent in polypropylene.
The polypropylene is a polypropylene homopolymer or a polypropylene random copolymer, alternating copolymer, segmented copolymer or block copolymer containing one or more comonomers selected from the group consisting of: ethylene, C 4 -C 20 Alpha-olefins, vinylcyclohexane, vinylcyclohexene, C 4 -C 20 Alkadienes, C 5 -C 12 Cyclic dienes and norbornene derivatives; wherein the total amount of propylene and comonomer is 100% for polypropylene random, alternating, segmented or block copolymers.
Preferably, the polypropylene is a random copolymer polypropylene.
The effective amount of the tetra-amide type nucleating agent added to the polypropylene composition can be determined by one of ordinary skill in the art through routine experimental testing. Preferably, the nucleating agent is used in an amount of 0.02 to 0.08 parts by weight based on 100 parts by weight of polypropylene.
Functional additives commonly used in the art may also be included in the polypropylene composition in a concentration range that does not adversely affect the beneficial effects of the present invention. Such additives include lubricants, stabilizers, antioxidants, ultraviolet light absorbers, heat stabilizers, light stabilizers, neutralizing agents, acid-binding agents, antistatic agents, antiblocking agents, heavy metal deactivators, flame retardants, nucleating agents, transparencies, foaming agents, processing aids, peroxides, silane compounds, fluorine compounds, hydrotalcites, elastomers, pigments, fillers, reinforcing materials, and the like.
As a preferable technical scheme, the polypropylene composition of the invention also comprises the following additives: antioxidant 1010, antioxidant 168 and calcium stearate. The additive is used in the following amount based on 100 parts by weight of polypropylene: 0.04-0.06 part by weight of antioxidant 1010,0.05-0.2 part by weight of antioxidant 168 and 0.03-0.07 part by weight of calcium stearate.
A third aspect of the present invention provides a method for preparing the polypropylene composition, comprising the steps of: and simultaneously adding the polypropylene, the amide nucleating agent and the additive into a high-speed mixer for mixing, extruding and granulating by a double-screw extruder to obtain blend granules, and drying the blend granules to obtain the polypropylene composition.
Preferably, the rotating speed of the high-speed mixer is 700-1000rpm, and the extrusion temperature of the double-screw extruder is 190-210 ℃.
Aiming at the problems of low crystallinity and defective mechanical properties of the common polypropylene material, the tetra-amide nucleating agent has the unexpected effect and can effectively improve the mechanical properties such as crystallinity, forming speed, rigidity and the like of the polypropylene material. The tetra-amide nucleating agent disclosed by the invention has the advantages of no peculiar smell, good compatibility with materials, easiness in dispersion and no precipitation, improves the performance of polypropylene materials, and widens the application field of the polypropylene materials.
Detailed Description
The following description is presented to enable one of ordinary skill in the art to make and use the invention. The preferred embodiments in the following description are by way of example only and are not intended to limit the scope of the invention, as other obvious variations will occur to those skilled in the art. The basic principles of the invention defined in the following description may be applied to other embodiments, variations, modifications, equivalents, and other technical solutions without departing from the spirit and scope of the invention.
The apparatus or reagents in the examples of the present invention are not manufacturer-specific, and are conventional commercial apparatus or reagents.
Example 1
Preparation of 1,3,4, 6-tetraisopropyl amide benzene nucleating agent:
step 1: 25g of m-dichlorobenzene was added to a solution containing 80mL of concentrated sulfuric acid and 7.3g of potassium nitrate, and the mixture was heated and stirred for reaction. After the reaction is completed, extracting, spin drying, and separating and purifying the crude product by column chromatography to obtain an intermediate product 1, 5-dichloro-2, 4-dinitrobenzene.
Step 2: dispersing 1g of the intermediate 1, 5-dichloro-2, 4-dinitrobenzene obtained in the step 1 in 7mL of ethylene glycol, heating and stirring, continuously bubbling ammonia gas, filtering and drying the solid to obtain the intermediate 4, 6-dinitro-1, 3-phenylenediamine.
Step 3: dispersing 0.5g of intermediate 4, 6-binitro-1, 3-phenylenediamine obtained in the step 2 into a mixed solution of 26mL of concentrated HCl and 13mL of ethanol, heating and stirring the mixture, and obtaining 4.3g of SnCl 2 Dissolving in proper amount of ethanol, adding into the reaction solution, and stirring for reaction. And after the reaction is finished, filtering and collecting a white powder product to obtain an intermediate 1,2,4, 5-benzene tetramine tetra hydrochloride.
Step 4: dissolving 0.24g of intermediate 1,2,4, 5-benzene tetramine tetra-hydrochloride in 30mL of acetonitrile, stirring, adding 0.78g of isobutyryl chloride, slowly dripping 2mL of triethylamine, stirring for reaction, filtering, collecting white solid powder, fully washing, and drying to obtain the nucleating agent 1,3,4, 6-tetraisopropyl amide benzene.
End product structure data: 1 H NMR(400MHz,DMSO-d 6 ):δ9.30(s,4H),7.60(s,2H), 2.62-2.55(m,4H),1.23-1.09(m,24H).HRMS m/z calcd for C 22 H 34 N 4 O 4 [M+H] + 419.26; found 419.3 melting Point Range: 215-240 ℃.
Example 2
Preparation of 1,3,4, 6-tetra-n-butylamide benzene nucleating agent:
step 1: 25g of m-dichlorobenzene was added to a solution containing 80mL of concentrated sulfuric acid and 7.3g of potassium nitrate, and the mixture was heated and stirred for reaction. After the reaction is completed, extracting, spin drying, and separating and purifying the crude product by column chromatography to obtain an intermediate product 1, 5-dichloro-2, 4-dinitrobenzene.
Step 2: dispersing 1g of the intermediate 1, 5-dichloro-2, 4-dinitrobenzene obtained in the step 1 in 7mL of ethylene glycol, heating and stirring, continuously bubbling ammonia gas, filtering and drying the solid to obtain the intermediate 4, 6-dinitro-1, 3-phenylenediamine.
Step 3: dispersing 0.5g of intermediate 4, 6-binitro-1, 3-phenylenediamine obtained in the step 2 into a mixed solution of 26mL of concentrated HCl and 13mL of ethanol, heating and stirring the mixture, and obtaining 4.3g of SnC l 2 Dissolving in proper amount of ethanol, adding into the reaction solution, and stirring for reaction. And after the reaction is finished, filtering and collecting a white powder product to obtain an intermediate 1,2,4, 5-benzene tetramine tetra hydrochloride.
Step 4: dissolving 1g of intermediate 1,2,4, 5-benzene tetramine tetra-hydrochloride in 125mL of acetonitrile, stirring, adding 3.67g of n-pentanoyl chloride, slowly dripping 8.3mL of triethylamine, stirring for reaction, filtering to collect white solid powder, fully washing, and drying to obtain the nucleating agent 1,3,4, 6-tetra-n-butyl amide benzene.
End product structure data: 1 H NMR(400MHz,DMSO-d 6 ):δ9.46(s,4H),7.62(s,2H), 2.25-2.32(m,8H),1.51-1.53(m,8H),1.26-1.28(m,8H),0.84-0.87(m,12H).HRMS m/z calcd for C 26 H 42 N 4 O 4 [M+H] + 475.32; found 475.44 melting Point Range: 215-240 ℃.
Example 3
Preparation of 1,3,4, 6-tetraisobutylamide benzene nucleating agent:
step 1: 25g of m-dichlorobenzene was added to a solution containing 80mL of concentrated sulfuric acid and 7.3g of potassium nitrate, and the mixture was heated and stirred for reaction. After the reaction is completed, extracting, spin drying, and separating and purifying the crude product by column chromatography to obtain an intermediate product 1, 5-dichloro-2, 4-dinitrobenzene.
Step 2: dispersing 1g of the intermediate 1, 5-dichloro-2, 4-dinitrobenzene obtained in the step 1 in 7mL of ethylene glycol, heating and stirring, continuously bubbling ammonia gas, filtering and drying the solid to obtain the intermediate 4, 6-dinitro-1, 3-phenylenediamine.
Step 3: dispersing 0.5g of intermediate 4, 6-binitro-1, 3-phenylenediamine obtained in the step 2 into a mixed solution of 26mL of concentrated HCl and 13mL of ethanol, heating and stirring the mixture, and obtaining 4.3g of SnCl 2 Dissolving in proper amount of ethanol, adding into the reaction solution, and stirring for reaction. And after the reaction is finished, filtering and collecting a white powder product to obtain an intermediate 1,2,4, 5-benzene tetramine tetra hydrochloride.
Step 4: dissolving 1g of intermediate 1,2,4, 5-benzene tetramine tetra-hydrochloride in 125mL of acetonitrile, stirring, adding 3.67g of isovaleryl chloride, slowly dripping 8.3mL of triethylamine, stirring for reaction, filtering to collect white solid powder, fully washing, and drying to obtain the nucleating agent 1,3,4, 6-tetraisobutyramide benzene.
End product structure data: 1 H NMR(400MHz,DMSO-d 6 ):δ9.39(s,4H),7.59(s,2H), 2.14-2.15(m,8H),1.97-2.12(m,4H),0.86-1.14(m,24H).HRMS m/z calcd for C 26 H 42 N 4 O 4 [M+H] + 475.32; found 475.35 melting Point Range: 215-240 ℃.
Example 4
Preparation of N, N' - (benzene-1, 2,4, 5-tetrayl) tetrakis (2-ethylhexanamide) nucleating agent:
step 1: 25g of m-dichlorobenzene was added to a solution containing 80mL of concentrated sulfuric acid and 7.3g of potassium nitrate, and the mixture was heated and stirred for reaction. After the reaction is completed, extracting, spin drying, and separating and purifying the crude product by column chromatography to obtain an intermediate product 1, 5-dichloro-2, 4-dinitrobenzene.
Step 2: dispersing 1g of the intermediate 1, 5-dichloro-2, 4-dinitrobenzene obtained in the step 1 in 7mL of ethylene glycol, heating and stirring, continuously bubbling ammonia gas, filtering and drying the solid to obtain the intermediate 4, 6-dinitro-1, 3-phenylenediamine.
Step 3: dispersing 0.5g of intermediate 4, 6-binitro-1, 3-phenylenediamine obtained in the step 2 into a mixed solution of 26mL of concentrated HCl and 13mL of ethanol, heating and stirring the mixture, and obtaining 4.3g of SnCl 2 Dissolving in proper amount of ethanol, adding into the reaction solution, and stirring for reaction. And after the reaction is finished, filtering and collecting a white powder product to obtain an intermediate 1,2,4, 5-benzene tetramine tetra hydrochloride.
Step 4: 1g of intermediate 1,2,4, 5-benzene tetramine tetra-hydrochloride is dissolved in 125mL of acetonitrile, and is stirred, 9.42g of 2-ethylhexanoyl chloride is added, 8.3mL of triethylamine is slowly dripped into the mixture, the mixture is stirred for reaction, white solid powder is collected by suction filtration, and the white solid powder is dried after being fully washed, so as to obtain a nucleating agent N, N' - (benzene-1, 2,4, 5-tetrayl) tetra (2-ethylhexanamide).
End product structure data: 1 H NMR(400MHz,DMSO-d 6 ):δ9.27(s,4H),7.56(s,2H), 2.43-2.41(m,4H),1.69-1.71(m,8H),1.56-1.58(m,8H),1.27-1.25(m,8H),1.21-1.17(m,8H),0.88-0.85(m,12H),0.84-0.83(m,12H).HRMS m/z calcd for C 38 H 66 N 4 O 4 [M+H] + 643.51; found 643.77 melting Point Range: 215-240 ℃.
Application examples E1 to E4
Preparation of a Polypropylene composition: 100 parts by weight of random copolymer polypropylene (Yangzi petrochemical) is taken, uniformly mixed with 0.08 part by weight of nucleating agent prepared in examples 1-4, 0.05 part by weight of antioxidant 1010,0.1 part by weight of antioxidant 168,0.05 parts by weight of calcium stearate, and the mixture is extruded and granulated in a twin-screw extruder after being mixed for 10 minutes in a high-speed mixer with the speed of 800 r/min, the melt extrusion temperature is 190-210 ℃, and the blend granules are dried and then are prepared into samples on an injection molding machine, so that polypropylene compositions E1-E4 are respectively obtained. The sample numbers are consistent with the nucleating agent used, such as the polypropylene composition number E1 using the nucleating agent of example 1, and so on. The random copolymer polypropylene without the nucleating agent was subjected to the same treatment as a blank sample.
The mechanical properties of the prepared samples were tested, and the test results are shown in Table 1. The higher the flexural modulus, the better the rigidity of the polymer. Wherein MFR (230 ℃,2.16 kg) was measured according to GB/T3682.1-2018 and flexural modulus was measured according to GB/T9341-2008.
TABLE 1 mechanical property test of samples E1-E4
Figure SMS_2
As shown by the test data of E1-E4 in Table 1, the flexural modulus of polypropylene was improved after the addition of an effective amount of a nucleating agent to the random copolymer polypropylene material. The unexpected trend of increasing and then decreasing flexural modulus is that the flexural modulus of E3 is most unexpectedly increased. At the same level (0.08%), the stiffening properties of example 3 are best.
Application examples E5 to E8
The nucleating agents prepared in example 3 were used in the amounts listed in Table 2, and the polypropylene compositions E5 to E8 were obtained according to the preparation method of application example E3, respectively. The same amounts of antioxidant 1010, antioxidant 168 and calcium stearate were added to the random copolymer polypropylene as a blank sample.
TABLE 2 mechanical property test of samples E3, E5-E8
Figure SMS_3
Figure SMS_4
We have found that, surprisingly, the effect is particularly excellent when the amount added is 0.08%. As shown in the test data of Table 2, the addition amount of 0-0.20% was set, wherein the flexural modulus at 0-0.08% was gradually increased, while the flexural modulus at 0.08% -0.20% was gradually decreased, and the flexural modulus at 0.08% was increased to peak value, indicating that 800ppm was the optimum addition amount, and the performance was the best.
In conclusion, the novel tetra-amide nucleating agent disclosed by the invention has stiffening performance, is an effective polypropylene stiffening additive, can greatly expand the application field of polypropylene and meets the market demands.
It will be appreciated by persons skilled in the art that the embodiments of the invention shown in the foregoing description are by way of example only and are not limiting. The objects of the present invention have been fully and effectively achieved. The functional and structural principles of the present invention have been shown and described in the examples and embodiments of the invention may be modified or practiced without departing from the principles described.

Claims (11)

1. A tetra-amide nucleating agent, which is characterized by at least comprising a tetra-amide benzene derivative with a structure shown as a formula (I):
Figure FDA0004257552070000011
wherein R is 1 、R 2 、R 3 And R is 4 Is the same substituent and is selected from n-butyl, isobutyl or 1-ethylpentyl;
the preparation method of the tetra-amide benzene derivative comprises the following steps:
s1, taking m-dichlorobenzene as a raw material, and performing nitration reaction to obtain an intermediate 1, 5-dichloro-2, 4-dinitrobenzene;
s2, subjecting the intermediate 1, 5-dichloro-2, 4-dinitrobenzene obtained in the step S1 to amination reaction to obtain an intermediate 4, 6-dinitro-1, 3-phenylenediamine;
s3, carrying out reduction reaction on the intermediate 4, 6-binitro-1, 3-phenylenediamine obtained in the step S2 to obtain an intermediate 1,2,4, 5-benzene tetramine tetrahydrochloride;
and S4, carrying out acylation reaction on the intermediate 1,2,4, 5-benzene tetramine tetra-hydrochloride obtained in the step S3 to obtain the tetra-amide benzene derivative.
2. The tetra-amide type nucleating agent as defined in claim 1, wherein R 1 、R 2 、R 3 And R is 4 Is isobutyl.
3. A polypropylene composition comprising an effective amount of a tetra-amide type nucleating agent selected from any one of 1,3,4, 6-tetraisopropylamide benzene, 1,3,4, 6-tetra-N-butylamide benzene, 1,3,4, 6-tetraisobutylamide benzene, N ', N ", N'" - (benzene-1, 2,4, 5-tetrayl) tetra (2-ethylhexanamide) in polypropylene.
4. A polypropylene composition according to claim 3, wherein the polypropylene is a polypropylene homopolymer or comprises one or more of the followingA polypropylene random copolymer, alternating copolymer or block copolymer of a comonomer selected from the group consisting of: ethylene, C 4 -C 20 Alpha-olefins, vinylcyclohexene, C 4 -C 20 Alkadienes, C 5 -C 12 Cyclic dienes and norbornene derivatives; wherein the total amount of propylene and comonomer is 100% for polypropylene random, alternating or block copolymers.
5. A polypropylene composition according to claim 3, wherein the polypropylene is a random copolymer polypropylene.
6. The polypropylene composition according to claim 3, wherein the tetra-amide type nucleating agent is used in an amount of 0.02 to 0.08 parts by weight based on 100 parts by weight of polypropylene.
7. The polypropylene composition according to claim 3, further comprising an additive selected from one or more of lubricants, stabilizers, antioxidants, ultraviolet absorbers, neutralizing agents, acid-binding agents, antistatic agents, antiblocking agents, heavy metal deactivators, flame retardants, transparencies, foaming agents, pigments, fillers, reinforcing materials.
8. The polypropylene composition according to claim 7, wherein the additives are antioxidant 1010, antioxidant 168 and calcium stearate.
9. The polypropylene composition according to claim 8, wherein the additives are used in the following amounts: 0.04-0.06 part by weight of antioxidant 1010,0.05-0.2 part by weight of antioxidant 168,0.03-0.07 part by weight of calcium stearate.
10. A process for preparing a polypropylene composition according to any one of claims 3 to 9, comprising the steps of: and simultaneously adding polypropylene, a tetra-amide nucleating agent and optional additives into a high-speed mixer for mixing, extruding and granulating by a double-screw extruder to obtain blend granules, and drying the blend granules to obtain the polypropylene composition.
11. The method of claim 10, wherein the speed of the high speed mixer is 700-1000rpm and the extrusion temperature of the twin screw extruder is 190-210 ℃.
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ES2680625T3 (en) * 2015-06-23 2018-09-10 Omya International Ag Load material product surface treated for polyolefins alpha-nucleation

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