CN111286128B - Quickly-molded polybutylene resin and preparation method thereof - Google Patents
Quickly-molded polybutylene resin and preparation method thereof Download PDFInfo
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- 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
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
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Abstract
The invention relates to a quickly-formed polybutylene resin and a preparation method thereof, belonging to the field of high polymer materials. The components of the color masterbatch comprise polybutylene, an antioxidant, a halogen absorbing agent, a light stabilizer, a color masterbatch, a nucleating agent and a filler; the preparation method comprises the steps of uniformly mixing the polybutene, the antioxidant, the halogen absorbing agent, the light stabilizer, the color master batch, the nucleating agent and the filler by a high-speed stirring mixer, and carrying out melt extrusion granulation to obtain the polybutene resin. The resin has the characteristics of high crystal form transformation speed, high heat-resistant temperature and the like, and can be used as a cold and hot water pipe material.
Description
Technical Field
The invention relates to a polybutylene resin with rapid crystal form transformation and high thermal deformation temperature, a preparation method and application thereof, belonging to the field of high polymer materials, in particular to the processing and application of the high polymer materials.
Background
The high Isotactic Polybutene (iPB) has outstanding thermal creep resistance, environmental stress cracking resistance, high heat resistance temperature and good toughness, and is one of the best materials for the pipe and the connecting piece thereof.
Different from other pipes, the polybutene is melt processed to directly form a metastable crystal form II, and the crystal form II is gradually converted into a stable crystal form I at room temperature. The crystal form of the polybutene is slowly transformed, the transformation time is long (more than 7 days), and in the process of transforming the crystal form, the size of the product is reduced and the strength is increased. Therefore, the polybutene can be transported and applied after being placed at room temperature for more than one week until the crystal form transformation is completed, so that the molding time of the polybutene product is greatly prolonged, and the turnover period of the product is remarkably prolonged. Therefore, the development of a polybutene material with rapid forming (rapid crystal transformation) is of great significance.
CN105273320A discloses a method for adding graphene into polybutene, which accelerates the II-I crystal form transformation of polybutene and improves the mechanical properties of polybutene, but expensive graphene makes the cost of the product higher. The Chinese patent ZL200410032739.7 discloses that acetylene black is used as a nucleating agent to promote the crystal form transformation of a 1-butene homopolymer or a 1-butene copolymer and improve the chlorine water resistance of the copolymer. CN104629195B discloses that polybutene in-kettle alloy containing polypropylene component is prepared by in-kettle polymerization technology, and the crystal form transformation rate can be accelerated. Japanese patent 2618469 discloses a method of adding propylene homopolymer and HDPE to polybutene to shorten the crystal transition period, but the addition of propylene homopolymer and HDPE deteriorates some of its properties.
CN101020777B discloses a high thermal conductivity polybutene coil prepared by adding graphite with surface treatment, which improves the pressure resistance and heat resistance of the product, but does not relate to the problems of crystal transformation and rapid forming of polybutene. CN105504552B, CN105754233A, CN1016151774A discloses a reinforced polybutylene pipeline material and a preparation method thereof, but none of the above patents relate to the problem of quick forming of polybutylene.
Disclosure of Invention
One of the purposes of the invention is to solve the problem that the crystal form of the polybutene is slowly changed (more than one week), and provide a formula of the polybutene resin for quick forming.
The invention also aims to further improve the heat deformation temperature of the polybutylene resin and improve the heat resistance of the polybutylene resin.
The invention also aims to provide a preparation method of the quick-forming polybutylene resin.
A fast-forming polybutene resin is composed of the following components in parts by weight:
polybutene 100 parts
0.1-5 parts of antioxidant
0.01-2 parts of halogen absorbing agent
0.01-2 parts of light stabilizer
0.1-5 parts of color masterbatch
0.01-5 parts of nucleating agent
0.1 to 10 portions of filler
The isotactic degree of polybutene in the polybutene resin is more than 96wt.%, and the melt mass flow rate is 0.2-3g/10min (190 ℃,2.16 kg). The antioxidant comprises a main antioxidant and an auxiliary antioxidant, the weight ratio of the main antioxidant to the auxiliary antioxidant is 1.5-4, wherein the main antioxidant is selected from one or more of BHT, hostanox3, 3114, 1010 and 1076, and the auxiliary antioxidant is selected from one or more of 168, 626, 9228, DLTDP, DSTP, DMTDP and DTDTP.
The halogen absorbing agent is one or more of hydrotalcite, calcium stearate, sodium stearate or zinc stearate.
The light stabilizer is one or more of benzophenone or hindered amine.
The nucleating agent is one or a mixture of two or more of 3,4-dimethyl benzyl sorbitol, bicyclo [2,2,1] disodium heptadicarboxylate, sodium bis (p-tert-butylphenyl) phosphate, aromatic amide compounds and derivatives thereof.
The color master batch comprises the following components in parts by weight: 40-95 parts of high isotactic polybutene (isotacticity greater than 96 wt.%); 0.1-6 parts of polyethylene wax or polypropylene wax; 0.1-6 parts of titanium dioxide; 0.001-6 parts of pigment; 0.01-3 parts of an anti-aging agent.
The filler is one or more of calcium carbonate, talcum powder, mica and kaolin.
A preparation method of quickly molded polybutylene resin comprises the following specific preparation steps:
(1) All the raw materials (polybutene, antioxidant, halogen absorbing agent, light stabilizer, color masterbatch, nucleating agent and filler) weighed according to the proportion are uniformly mixed in a high-speed stirring mixer;
(2) Adding the uniformly mixed materials in the step (1) into a double-screw extruder with the length-diameter ratio of 30-50, and performing melt extrusion, wherein the extrusion process comprises the following steps: the first zone is 150-160 ℃, the second zone is 160-170 ℃, the third zone is 170-180 ℃, the fourth zone is 180-190 ℃, the fifth zone is 190-210 ℃, the head is 180-200 ℃, the rotating speed is 5-30r/min, and the melt pressure is 10-20MPa.
(3) And (3) granulating and drying the extrudate obtained in the step (2) to obtain the polybutene resin.
The polybutene resin prepared by the invention maintains the excellent shock resistance, excellent heat creep resistance and outstanding environmental stress cracking resistance of polybutene, meanwhile, the crystal form transformation speed is obviously improved, the heat resistance is obviously improved, and the polybutene resin can be used as cold and hot water pipes and pipe fittings.
Detailed Description
The following examples are presented to better illustrate the invention and are not to be construed as limiting the claims of the invention.
The isotactic degree of polybutene in the polybutene alloy resin used was 98.wt%, and the melt flow rate (190 ℃ C., load 2.16 kg) was 0.5g/10min. Measuring the characteristic peak-peak high variation curve of the polybutene crystal form I by using an online infrared spectrum to obtain the t of crystal form conversion 1/2 And the appearance time of the crystal form I, and the Vicat softening point of the polybutene is measured by a Vicat heat distortion tester (GB/T1633-2000 A50 method).
Comparative example 1
Weighing the materials according to the components and the formula (in parts by weight) provided in the table 1, wherein the main antioxidant is 1010 and the auxiliary antioxidant is 168, mixing the materials in a high-speed mixer for 5 minutes, and then extruding and granulating the mixture in a double-screw extruder with the length-diameter ratio of 45 and the diameter of 50 millimeters to obtain the polybutene material. The temperature of each section of the extruder is as follows: 150 ℃ in the first zone, 160 ℃ in the second zone, 170 ℃ in the third zone, 180 ℃ in the fourth zone, 190 ℃ in the fifth zone, 180 ℃ at the head, 20 revolutions per minute at the speed of the extruder and 15MPa of melt pressure.
The results of the performance tests are shown in table 1.
Example 1
The materials were weighed according to the components and formulations provided in table 1 (in parts by weight, the same in the following examples), wherein the filler was calcium carbonate, the nucleating agent was 3,4-dimethyldibenzyl sorbitol (nucleating agent 1), the primary antioxidant was 1010, the secondary antioxidant was 168, the halogen absorbing agent was calcium stearate, and the light stabilizer was benzophenone grease. The color master batch (color master 1) comprises the following components in parts by weight: 90 parts of high isotactic polybutene (98 wt.% of isotacticity), 3 parts of polypropylene wax, 3 parts of titanium dioxide, 0.01 part of pigment and 0.03 part of anti-aging agent.
After mixing for 5 minutes in a high-speed stirrer, extruding and granulating in a double-screw extruder with the length-diameter ratio of 45 and the diameter of 50 millimeters to obtain the polybutene resin. The temperature of each section of the extruder is as follows: 150 ℃ in the first region, 160 ℃ in the second region, 170 ℃ in the third region, 180 ℃ in the fourth region, 190 ℃ in the fifth region, 180 ℃ at the head, 20 revolutions per minute at the rotation speed of the extruder and 15MPa of melt pressure.
The results of the performance tests are shown in Table 1.
Example 2
The materials were weighed according to the components and formulations (in parts by weight) provided in table 1, wherein the filler was calcium carbonate, the nucleating agent was 3,4-dimethylbenzyl sorbitol (nucleating agent 1), the primary antioxidant was 1010, the secondary antioxidant was 168, the halogen absorbing agent was calcium stearate, and the light stabilizer was benzophenone grease. The color master batch (color master 1) comprises the following components in parts by weight: 90 parts of high isotactic polybutene (98 wt.% of isotacticity), 3 parts of polypropylene wax, 3 parts of titanium dioxide, 0.01 part of pigment and 0.03 part of anti-aging agent.
The rest was the same as in example 1. The results of the performance tests are shown in Table 1.
Example 3
The materials were weighed according to the components and formulations (in parts by weight) provided in table 1, wherein the filler was calcium carbonate, the nucleating agent was 3,4-dimethylbenzyl sorbitol (nucleating agent 1), the primary antioxidant was 1010, the secondary antioxidant was 168, the halogen absorbing agent was calcium stearate, and the light stabilizer was benzophenone grease. The color master batch (color master 2) comprises the following components in parts by weight: 90 parts of high isotactic polybutene (98 wt.% of isotacticity), 1 part of polypropylene wax, 3 parts of titanium dioxide, 0.01 part of pigment and 0.03 part of anti-aging agent.
The rest is the same as example 1. The results of the performance tests are shown in Table 1.
Example 4
The materials were weighed according to the components and formulation (in parts by weight) provided in table 1, wherein the filler was calcium carbonate, the nucleating agent was an aromatic amide compound (nucleating agent 2), the primary antioxidant was 1010, the secondary antioxidant was 168, the halogen absorbing agent was calcium stearate, and the light stabilizer was benzophenone grease. The color master batch (color master 1) comprises the following components in parts by weight: 90 parts of high isotactic polybutene (98 wt.% of isotacticity), 3 parts of polypropylene wax, 3 parts of titanium dioxide, 0.01 part of pigment and 0.03 part of anti-aging agent.
The rest is the same as example 1. The results of the performance tests are shown in table 1.
Example 5
The materials were weighed according to the components and formulations (in parts by weight) provided in table 1, wherein the filler was calcium carbonate, the nucleating agent was 3,4-dimethylbenzyl sorbitol (nucleating agent 1), the primary antioxidant was 1010, the secondary antioxidant was 168, the halogen absorbing agent was calcium stearate, and the light stabilizer was benzophenone grease. The color master batch (color master 1) comprises the following components in parts by weight: 90 parts of high isotactic polybutene (98 wt.% of isotacticity), 3 parts of polypropylene wax, 3 parts of titanium dioxide, 0.01 part of pigment and 0.03 part of anti-aging agent.
After mixing for 5 minutes in a high-speed stirrer, extruding and granulating in a double-screw extruder with the length-diameter ratio of 45 and the diameter of 50 millimeters to obtain the polybutene resin. The temperature of each section of the extruder is as follows: 155 ℃ in the first zone, 165 ℃ in the second zone, 175 ℃ in the third zone, 185 ℃ in the fourth zone, 195 ℃ in the fifth zone, 185 ℃ in the head, 25 revolutions per minute in the extruder and 15MPa in the melt pressure.
The results of the performance tests are shown in table 1.
As can be seen from the results of the examples and comparative example 1, the crystal transformation speed of the polybutene resin of the present invention is greatly increased as compared with polybutene, and the heat resistance can be increased by 7.1 ℃.
TABLE 1 Components and formulations of the examples and comparative examples
| Components | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Comparative example 1 |
| Polybutene/part by weight | 100 | 100 | 100 | 100 | 100 | 100 |
| Fillers/parts by weight | 5 | 5 | 5 | 5 | 5 | 0 |
| Nucleating agent 1/part by weight | 0.3 | 0.5 | 0.3 | 0 | 0.3 | 0 |
| Nucleating agent 2/part by weight | 0 | 0 | 0 | 0.3 | 0 | 0 |
| Main antioxidant per weight portion | 0.1 | 0.1 | 0.1 | 0.1 | 0.1 | 0.1 |
| Auxiliary antioxidant/part by weight | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 |
| Halogen-absorbing agent/part by weight | 0.1 | 0.1 | 0.1 | 0.1 | 0.1 | 0 |
| Light stabilizer per part by weight | 0.8 | 0.8 | 0.8 | 0.8 | 0.8 | 0 |
| 1 part by weight of color master batch | 2 | 2 | 0 | 2 | 2 | 0 |
| 2 parts by weight of color master batch | 0 | 0 | 2 | 0 | 0 | 0 |
| T of crystal form transformation 1/2 Hour per hour | 15.9 | 15.6 | 15.9 | 21.2 | 18.2 | 58.4 |
| Time of appearance/hour of form I | 3.0 | 2.8 | 3.0 | 4.1 | 3.6 | 19.7 |
| Vicat softening point/. Degree C | 121.5 | 120.9 | 120.1 | 118.8 | 119.8 | 114.4 |
Claims (6)
1. A polybutylene resin for rapid prototyping is characterized by comprising the following components in parts by weight:
polybutene 100 parts
0.1-5 parts of antioxidant
0.01-2 parts of halogen absorbing agent
0.01-2 parts of light stabilizer
Color masterbatch 0.1-5 parts
0.01-5 parts of nucleating agent
0.1-10 parts of a filler;
wherein the isotactic degree of said polybutene is greater than 96wt.%,190 o C, the mass flow rate of the melt under 2.16kg is 0.2-3g/10min; the color master batch comprises the following components in parts by weight: 40-95 parts of high isotactic polybutene with an isotacticity greater than 96 wt.%; 0.1-6 parts of polyethylene wax or polypropylene wax; 0.1-6 parts of titanium dioxide; 0.001-6 parts of pigment; 0.01-3 parts of an anti-aging agent; the nucleating agent is 3,4-dimethyl benzyl sorbitol;
the polybutylene resin is prepared by the following steps:
(1) All the raw materials weighed according to the proportion are uniformly mixed in a high-speed stirring mixer;
(2) Adding the uniformly mixed material obtained in the step (1) into a double-screw extruder with the length-diameter ratio of 45: a region 150 o C, second zone 160 o C, three region 170 o C, four zone 180 o C, five zone 190 o C, the aircraft nose 180 o C, rotating speed of 20r/min and melt pressure of 15 MPa;
(3) Granulating and drying the extrudate obtained in the step (2) to obtain polybutene resin;
or
The polybutylene resin is prepared by the following steps:
(1) All the raw materials weighed according to the proportion are uniformly mixed in a high-speed stirring mixer;
(2) Adding the uniformly mixed material obtained in the step (1) into a double-screw extruder with the length-diameter ratio of 45: a region 155 o C, zone two 165 o C, three zone 175 o C, four zone 185 o C, five zone 195 o C, handpiece 185 o C, rotating speed of 25r/min and melt pressure of 15 MPa;
(3) And (3) granulating and drying the extrudate obtained in the step (2) to obtain the polybutene resin.
2. The polybutylene resin with rapid prototyping of claim 1, wherein the antioxidant comprises a primary antioxidant and a secondary antioxidant, the weight ratio of the primary antioxidant to the secondary antioxidant is 1.5-4, wherein the primary antioxidant is selected from one or more of BHT, hostanox3, 3114, 1010 and 1076, and the secondary antioxidant is selected from one or more of 168, 626, 9228, DLTDP, DSTP, DMTDP and DTDTDTP.
3. The polybutylene resin for rapid prototyping according to claim 1, wherein the halogen-absorbing agent is one or more of hydrotalcite, calcium stearate, sodium stearate, or zinc stearate.
4. The polybutylene resin for rapid prototyping according to claim 1, wherein the light stabilizer is one or more of benzophenones and hindered amines.
5. The polybutylene resin for rapid prototyping according to claim 1, wherein the filler is one or more of calcium carbonate, talc, mica, and kaolin.
6. The polybutene resin as claimed in claim 1, wherein the polybutene resin has the characteristics of high crystal transformation speed, high heat resistance, etc., and can be used as a material for cold and hot water pipes.
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| CN116144121A (en) * | 2023-03-27 | 2023-05-23 | 青岛科技大学 | Shape memory pipeline material with high heat creep resistance and preparation method thereof |
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