CN113321795A - PBT/artificial granite waste residue composite material and preparation method thereof - Google Patents
PBT/artificial granite waste residue composite material and preparation method thereof Download PDFInfo
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- CN113321795A CN113321795A CN202110662859.9A CN202110662859A CN113321795A CN 113321795 A CN113321795 A CN 113321795A CN 202110662859 A CN202110662859 A CN 202110662859A CN 113321795 A CN113321795 A CN 113321795A
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- waste residue
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- 239000002699 waste material Substances 0.000 title claims abstract description 58
- 239000010438 granite Substances 0.000 title claims abstract description 53
- 239000002131 composite material Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- WOZVHXUHUFLZGK-UHFFFAOYSA-N dimethyl terephthalate Chemical compound COC(=O)C1=CC=C(C(=O)OC)C=C1 WOZVHXUHUFLZGK-UHFFFAOYSA-N 0.000 claims abstract description 24
- 150000002148 esters Chemical group 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 8
- CDQSJQSWAWPGKG-UHFFFAOYSA-N butane-1,1-diol Chemical compound CCCC(O)O CDQSJQSWAWPGKG-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000003054 catalyst Substances 0.000 claims abstract description 5
- 239000012760 heat stabilizer Substances 0.000 claims abstract description 5
- 239000002685 polymerization catalyst Substances 0.000 claims abstract description 5
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 5
- 239000002994 raw material Substances 0.000 claims abstract description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 24
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 claims description 18
- 238000006068 polycondensation reaction Methods 0.000 claims description 16
- 238000006243 chemical reaction Methods 0.000 claims description 10
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Chemical compound O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 claims description 8
- 238000001291 vacuum drying Methods 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 5
- WVLBCYQITXONBZ-UHFFFAOYSA-N trimethyl phosphate Chemical compound COP(=O)(OC)OC WVLBCYQITXONBZ-UHFFFAOYSA-N 0.000 claims description 5
- XZZNDPSIHUTMOC-UHFFFAOYSA-N triphenyl phosphate Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)(=O)OC1=CC=CC=C1 XZZNDPSIHUTMOC-UHFFFAOYSA-N 0.000 claims description 5
- 229910020491 K2TiF6 Inorganic materials 0.000 claims description 4
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims description 4
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical group [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims description 4
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 claims description 4
- UEGPKNKPLBYCNK-UHFFFAOYSA-L magnesium acetate Chemical compound [Mg+2].CC([O-])=O.CC([O-])=O UEGPKNKPLBYCNK-UHFFFAOYSA-L 0.000 claims description 4
- 239000011654 magnesium acetate Substances 0.000 claims description 4
- 229940069446 magnesium acetate Drugs 0.000 claims description 4
- 235000011285 magnesium acetate Nutrition 0.000 claims description 4
- 239000004246 zinc acetate Substances 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000002893 slag Substances 0.000 claims 1
- 238000002425 crystallisation Methods 0.000 abstract description 13
- 230000008025 crystallization Effects 0.000 abstract description 13
- 238000010907 mechanical stirring Methods 0.000 abstract description 8
- 230000007613 environmental effect Effects 0.000 abstract description 4
- 238000003912 environmental pollution Methods 0.000 abstract description 4
- 230000008859 change Effects 0.000 abstract description 3
- 238000011065 in-situ storage Methods 0.000 abstract description 2
- 239000011347 resin Substances 0.000 abstract description 2
- 229920005989 resin Polymers 0.000 abstract description 2
- 230000009286 beneficial effect Effects 0.000 abstract 1
- 229920000642 polymer Polymers 0.000 abstract 1
- 229920001707 polybutylene terephthalate Polymers 0.000 description 23
- 230000008901 benefit Effects 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 3
- 229920000728 polyester Polymers 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- 239000002969 artificial stone Substances 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 229920006351 engineering plastic Polymers 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000004579 marble Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- -1 Polybutylene terephthalate Polymers 0.000 description 1
- 238000003915 air pollution Methods 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
- C08G63/12—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/16—Dicarboxylic acids and dihydroxy compounds
- C08G63/18—Dicarboxylic acids and dihydroxy compounds the acids or hydroxy compounds containing carbocyclic rings
- C08G63/181—Acids containing aromatic rings
- C08G63/183—Terephthalic acids
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/78—Preparation processes
-
- 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
- C08K11/00—Use of ingredients of unknown constitution, e.g. undefined reaction products
- C08K11/005—Waste materials, e.g. treated or untreated sewage sludge
-
- 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
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
-
- 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
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)
- Polyesters Or Polycarbonates (AREA)
Abstract
The invention relates to a PBT/artificial granite waste residue composite material and a preparation method thereof, wherein the composite material is prepared from the following raw materials in parts by weight: 100 parts of dimethyl terephthalate, 2-13 parts of artificial granite waste residues, 95-120 parts of butanediol, 0.01-0.5 part of ester exchange catalyst, 0.01-0.5 part of polymerization catalyst and 0.01-0.5 part of heat stabilizer. The composite material prepared by the invention is prepared by in-situ polymerization, and due to the low viscosity and violent mechanical stirring of the system in the polymerization process and the addition of the unsaturated resin coated on the surface of the artificial granite waste residue, the artificial granite waste residue is uniformly dispersed in the polymer system, so that the obtained composite material has excellent comprehensive mechanical property, and the thermal stability, the crystallization rate and the impact strength are obviously improved. The method can efficiently treat the artificial granite waste residue, eliminate the environmental pollution, change waste into valuable, is beneficial to environmental protection and conforms to the concept of green economic development.
Description
Technical Field
The invention belongs to the technical field of material chemistry, and relates to a PBT/artificial granite waste residue composite material and a preparation method thereof.
Background
The artificial granite serving as an internationally popular decorative material has the characteristics of high smoothness, compression resistance, wear resistance, environmental friendliness and the like. The artificial granite is prepared by using main raw materials, namely over 92 wt% of natural marble crushed aggregates, and the balance of unsaturated resin, a small amount of pigment and the like through the processes of vacuum stirring, high-pressure oscillation, curing molding, cutting and polishing and the like. However, in the production process of cutting, grinding and polishing the artificial granite, a large amount of waste stone slurry containing calcium carbonate waste residues is generated, the content of solid waste after precipitation and drying is about 20%, and the part is called as the artificial stone waste residues.
Because the surface of the waste residue contains unsaturated thermosetting polyester residues, the waste residue is difficult to process secondarily, cannot be degraded in natural environment, causes serious environmental pollution, is always a problem that the waste residue cannot be properly treated, and restricts the green sustainable development of the artificial stone industry. China has abundant marble resources, wide distribution, annual output of about 150 ten thousand tons and only about 35 percent of utilization rate, thereby not only greatly wasting resources, but also causing serious air pollution and water pollution. How to realize the reclamation and the harmlessness of the artificial granite waste residue becomes the biggest problem of green sustainable development of the industry.
Polybutylene terephthalate (PBT) is a polyester obtained by polymerizing dimethyl terephthalate or 1, 4-butanediol. PBT is an important thermoplastic polyester and is one of five engineering plastics. The excellent mechanical property and corrosion resistance of the PBT are widely applied to the fields of automobile manufacturing, mechanical parts and the like. However, its development is limited by the disadvantage of low heat distortion temperature, weak impact strength and poor dimensional stability
So far, no relevant report about the preparation of the PBT/artificial granite waste residue composite material exists.
Disclosure of Invention
The invention aims to solve the technical problem of providing the PBT/artificial granite waste residue composite material and the preparation method thereof, the composite material prepared by the method not only can efficiently treat the artificial granite waste residue and eliminate environmental pollution, but also can change waste into valuable, realize resource utilization, has very important practical significance for comprehensive environmental management and the like, and can obtain good social benefit and economic benefit.
The technical scheme of the invention is as follows:
the PBT/artificial granite waste residue composite material is prepared from the following raw materials in parts by weight:
further, the butanediol is 1, 4-butanediol.
Further, the ester exchange catalyst is selected from tetrabutyl titanate, antimony trioxide or K2TiF6One kind of (1).
Further, the polymerization catalyst is selected from one of zinc acetate, magnesium acetate or copper acetate.
Further, the heat stabilizer is selected from one of triphenyl phosphate or trimethyl phosphate.
The invention also provides a method for preparing the PBT/artificial granite waste residue composite material, which comprises the following steps:
(1) ester exchange: putting dimethyl terephthalate, butanediol and an ester exchange catalyst into a reactor with stirring, starting stirring, controlling the reaction temperature to be 190-210 ℃, and carrying out an ester exchange reaction;
(2) polymerization: and (2) when the mass of the methanol evaporated in the step (1) is 1.8 times of that of the dimethyl terephthalate, adding a polymerization catalyst, a heat stabilizer and the artificial granite waste residue, controlling the temperature to be 240-270 ℃, adjusting the vacuum degree to be below 40Pa to perform polycondensation reaction, controlling the reaction time to be 30-60min, controlling the temperature to be 60-80 ℃ after the polycondensation is finished, and performing vacuum drying for 10-12h to obtain the PBT/artificial granite waste residue composite material with the content of the artificial granite waste residue accounting for 1-10 wt%.
The reactor is a three-neck flask.
The invention has the advantages that:
compared with the prior art, the PBT/artificial granite waste residue composite material and the preparation method thereof well utilize the special surface characteristics of the artificial granite waste residue and the characteristics of relatively low viscosity and violent mechanical stirring of an in-situ polymerization system, so that the artificial granite waste residue is uniformly dispersed in the system and has better interface compatibility with a PBT matrix, and the obtained composite material has better comprehensive mechanical properties than pure PBT, and the thermal stability, the crystallization rate and the impact strength are obviously improved. The composite material can expand the wider application of PBT in the original field of engineering plastics.
The method can efficiently treat the artificial granite waste residue, eliminate the environmental pollution, change waste into valuable, realize resource utilization, has very important practical significance for comprehensive environmental treatment and the like, and can obtain good social benefit and economic benefit.
Drawings
FIG. 1(a) is a heat distortion temperature diagram;
FIG. 1(b) is a graph of time to maximum crystallization rate at different crystallization temperatures;
FIG. 1(c) is a graph of impact strength.
Detailed Description
The invention will now be further illustrated by reference to the following examples. The artificial granite waste residue used in the examples was obtained from Guangxi Lisheng Stone Co., Ltd and was sieved through a 1000 mesh sieve to remove coarser particles and dried before use.
Example 1:
(1) adding 100g of dimethyl terephthalate, 95g of 1, 4-butanediol and 0.01g of tetrabutyl titanate into a 250ml three-neck flask with mechanical stirring, and controlling the reaction temperature to 190 ℃ for ester exchange;
(2) and (3) after the amount of methanol evaporated by ester exchange reaches 36.4ml, adding 0.01g of zinc acetate, adding 0.01g of triphenyl phosphate and 2g of artificial granite waste residue, controlling the temperature to be 250 ℃, carrying out polycondensation reaction for 30min under the pressure of less than 40Pa, and carrying out vacuum drying for 10h at 80 ℃ after polycondensation to obtain the product, namely the PBT/artificial granite waste residue composite material. The content of the artificial granite waste residue in the composite material is about 1 wt%. The heat distortion temperature, maximum rate isothermal crystallization time and impact strength of the samples were measured as shown in FIG. 1. The values are given in Table 1.
Example 2:
(1) adding 100g of dimethyl terephthalate, 100g of 1, 4-butanediol and 0.05g of antimony trioxide into a 250ml three-neck flask with mechanical stirring, and controlling the reaction temperature to be 195 ℃ for ester exchange;
(2) and after the amount of methanol evaporated by ester exchange reaches 36.4ml, adding 0.05g of magnesium acetate, adding 0.05g of triphenyl phosphate and 4g of artificial granite waste residue, controlling the temperature to be 250 ℃, carrying out polycondensation reaction for 40min under the pressure of less than 40Pa, and after the polycondensation is finished, carrying out vacuum drying for 10h at 80 ℃ to obtain the product, namely the PBT/artificial granite waste residue composite material. The content of the artificial granite waste residue in the composite material is about 3 wt%. The heat distortion temperature, maximum rate isothermal crystallization time and impact strength of the samples were measured as shown in FIG. 1. The values are given in Table 1.
Example 3:
(1) adding 100g of dimethyl terephthalate, 100g of 1, 4-butanediol and 0.1g of antimony trioxide into a 250ml three-neck flask with mechanical stirring, and controlling the reaction temperature to be 195 ℃ for ester exchange;
(2) and after the amount of methanol evaporated by ester exchange reaches 36.4ml, adding 0.1g of magnesium acetate, adding 0.1g of trimethyl phosphate and 7g of artificial granite waste residue, controlling the temperature to be 250 ℃, carrying out polycondensation reaction for 40min under the pressure of less than 40Pa, and after the polycondensation is finished, carrying out vacuum drying for 10h at 80 ℃ to obtain the product, namely the PBT/artificial granite waste residue composite material. The content of the artificial granite waste residue in the composite material is about 5 wt%. The heat distortion temperature, maximum rate isothermal crystallization time and impact strength of the samples were measured as shown in FIG. 1. The values are given in Table 1.
Example 4:
(1) 100g of dimethyl terephthalate, 105g of 1, 4-butanediol and 0.3g of K2TiF6Adding into a 250ml three-neck flask with mechanical stirring, controlling the reaction temperature at 195 ℃ for ester cross-linkingChanging;
(2) and (3) after the amount of methanol evaporated by ester exchange reaches 36.4ml, adding 0.3g of copper acetate, 0.3g of trimethyl phosphate and 9g of artificial granite waste residue, controlling the temperature to be 250 ℃, carrying out polycondensation reaction for 40min under the pressure of less than 40Pa, and after the polycondensation is finished, carrying out vacuum drying for 10h at 80 ℃ to obtain the product, namely the PBT/artificial granite waste residue composite material. The content of the artificial granite waste residue in the composite material is about 7 wt%. The heat distortion temperature, maximum rate isothermal crystallization time and impact strength of the samples were measured as shown in FIG. 1. The values are given in Table 1.
Example 5:
(1) 100g of dimethyl terephthalate, 120g of 1, 4-butanediol and 0.5g of K2TiF6Adding into a 250ml three-neck flask with mechanical stirring, and controlling the reaction temperature at 210 ℃ for ester exchange;
(2) and (3) after the amount of methanol evaporated by ester exchange reaches 36.4ml, adding 0.5g of copper acetate, adding 0.5g of trimethyl phosphate and 13g of artificial granite waste residue, controlling the temperature to be 260 ℃, carrying out polycondensation reaction for 60min under the pressure of less than 40Pa, and carrying out vacuum drying for 10h at 80 ℃ after polycondensation, thus obtaining the product, namely the PBT/artificial granite waste residue composite material. The content of the artificial granite waste residue in the composite material is about 10 wt%. The heat distortion temperature, maximum rate isothermal crystallization time and impact strength of the samples were measured as shown in FIG. 1. The values are given in Table 1.
Comparative example:
the difference between the comparative example and the example 1 is that the comparative example does not add artificial granite waste residue in the step (2), and the specific steps are as follows:
(1) 100g of dimethyl terephthalate, 95g of 1, 4-butanediol and 0.01g of tetrabutyl titanate are added into a 250ml three-neck flask with mechanical stirring, and the reaction temperature is controlled at 190 ℃ for ester exchange;
(2) and (3) after the amount of methanol evaporated by ester exchange reaches 36.4ml, adding 0.01g of zinc acetate and 0.01g of triphenyl phosphate, controlling the temperature to be 250 ℃, carrying out polycondensation reaction for 30min under the pressure of less than 40Pa, and carrying out vacuum drying for 10h at 80 ℃ after polycondensation reaction to obtain the product, namely the pure PBT. The heat distortion temperature, maximum rate isothermal crystallization time and impact strength of the samples were measured as shown in FIG. 1. The values are given in Table 1.
TABLE 1
Note: the heat distortion temperature TEST was carried out by means of an HDT/V-1103(JJ-TEST, China) apparatus, the isothermal crystallization time TEST by means of a DSC25(TA, USA) apparatus and the impact strength TEST by means of a CEAST 9050(INSTRON, USA) apparatus in accordance with the ISO 180 standard.
From FIG. 1 and Table 1 we have found that the addition of artificial granite waste residue greatly improves the thermal stability of PBT, significantly reduces its isothermal crystallization time, increases crystallization rate and increases impact strength. Therefore, the PBT/artificial granite waste residue composite material has excellent comprehensive performance.
The embodiments described above are intended to facilitate one of ordinary skill in the art in understanding and using the present invention. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the embodiments described herein, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (7)
1. The PBT/artificial granite waste residue composite material is characterized by being prepared from the following raw material components in parts by weight:
2. the PBT/artificial granite waste residue composite material as claimed in claim 1, wherein: the butanediol is 1, 4-butanediol.
3. The PBT/artificial granite waste residue composite material of claim 1,the method is characterized in that: the ester exchange catalyst is selected from tetrabutyl titanate, antimony trioxide or K2TiF6One kind of (1).
4. The PBT/artificial granite waste residue composite material as claimed in claim 1, wherein: the polymerization catalyst is selected from one of zinc acetate, magnesium acetate or copper acetate.
5. The PBT/artificial granite waste residue composite material as claimed in claim 1, wherein: the heat stabilizer is one of triphenyl phosphate or trimethyl phosphate.
6. A process for the preparation of the PBT/artificial granite slag composite material of any one of claims 1 to 5, characterized by comprising the following steps:
(1) ester exchange: putting dimethyl terephthalate, butanediol and an ester exchange catalyst into a reactor with stirring, starting stirring, controlling the reaction temperature to be 190-210 ℃, and carrying out an ester exchange reaction;
(2) polymerization: and (2) when the mass of the methanol evaporated in the step (1) is 1.8 times of that of the dimethyl terephthalate, adding a polymerization catalyst, a heat stabilizer and the artificial granite waste residue, controlling the temperature to be 240-270 ℃, adjusting the vacuum degree to be below 40Pa to perform polycondensation reaction, controlling the reaction time to be 30-60min, controlling the temperature to be 60-80 ℃ after the polycondensation is finished, and performing vacuum drying for 10-12h to obtain the PBT/artificial granite waste residue composite material with the content of the artificial granite waste residue accounting for 1-10 wt%.
7. The preparation method of the PBT/artificial granite waste residue composite material as claimed in claim 6, wherein the preparation method comprises the following steps: the reactor is a three-neck flask.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101245230A (en) * | 2008-02-21 | 2008-08-20 | 上海天洋热熔胶有限公司 | Method for manufacturing linear copolyester hot melt adhesive |
| CN111995846A (en) * | 2020-09-16 | 2020-11-27 | 贺州学院 | PTT/artificial granite waste residue composite material and preparation method thereof |
| CN112048159A (en) * | 2020-09-16 | 2020-12-08 | 贺州学院 | Aromatic polyester/artificial stone waste residue composite material and preparation method thereof |
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- 2021-06-15 CN CN202110662859.9A patent/CN113321795A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101245230A (en) * | 2008-02-21 | 2008-08-20 | 上海天洋热熔胶有限公司 | Method for manufacturing linear copolyester hot melt adhesive |
| CN111995846A (en) * | 2020-09-16 | 2020-11-27 | 贺州学院 | PTT/artificial granite waste residue composite material and preparation method thereof |
| CN112048159A (en) * | 2020-09-16 | 2020-12-08 | 贺州学院 | Aromatic polyester/artificial stone waste residue composite material and preparation method thereof |
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Application publication date: 20210831 |