CN115584116A - Preparation method and application of environment-friendly inorganic powder dispersant - Google Patents
Preparation method and application of environment-friendly inorganic powder dispersant Download PDFInfo
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- 239000002270 dispersing agent Substances 0.000 title claims abstract description 49
- 239000000843 powder Substances 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 239000004721 Polyphenylene oxide Substances 0.000 claims abstract description 39
- 229920000570 polyether Polymers 0.000 claims abstract description 39
- 229920005862 polyol Polymers 0.000 claims abstract description 38
- 150000003077 polyols Chemical class 0.000 claims abstract description 38
- 229920001610 polycaprolactone Polymers 0.000 claims abstract description 31
- 239000004632 polycaprolactone Substances 0.000 claims abstract description 31
- 150000002148 esters Chemical class 0.000 claims abstract description 23
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000002253 acid Substances 0.000 claims abstract description 22
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 22
- 239000011737 fluorine Substances 0.000 claims abstract description 22
- 238000002156 mixing Methods 0.000 claims abstract description 22
- 229920000642 polymer Polymers 0.000 claims abstract description 16
- 238000001816 cooling Methods 0.000 claims abstract description 15
- 239000000203 mixture Substances 0.000 claims abstract description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000004321 preservation Methods 0.000 claims abstract description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 6
- 239000006057 Non-nutritive feed additive Substances 0.000 claims abstract description 5
- 238000000034 method Methods 0.000 claims description 14
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 9
- 150000008064 anhydrides Chemical class 0.000 claims description 5
- 238000007599 discharging Methods 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000000945 filler Substances 0.000 claims description 3
- 239000000049 pigment Substances 0.000 claims description 3
- 150000008065 acid anhydrides Chemical class 0.000 claims 1
- 230000000996 additive effect Effects 0.000 abstract description 8
- 239000011347 resin Substances 0.000 abstract description 8
- 229920005989 resin Polymers 0.000 abstract description 8
- 239000000654 additive Substances 0.000 abstract description 7
- 239000004595 color masterbatch Substances 0.000 abstract description 7
- 238000012545 processing Methods 0.000 abstract description 3
- 238000011049 filling Methods 0.000 abstract description 2
- 239000002202 Polyethylene glycol Substances 0.000 description 11
- 229920001223 polyethylene glycol Polymers 0.000 description 11
- 229920001451 polypropylene glycol Polymers 0.000 description 11
- 239000012752 auxiliary agent Substances 0.000 description 10
- XSTXAVWGXDQKEL-UHFFFAOYSA-N Trichloroethylene Chemical compound ClC=C(Cl)Cl XSTXAVWGXDQKEL-UHFFFAOYSA-N 0.000 description 9
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 8
- 239000004811 fluoropolymer Substances 0.000 description 7
- 229920002313 fluoropolymer Polymers 0.000 description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- 239000004594 Masterbatch (MB) Substances 0.000 description 5
- 239000006229 carbon black Substances 0.000 description 5
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 4
- 229920002593 Polyethylene Glycol 800 Polymers 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000004220 aggregation Methods 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 238000011534 incubation Methods 0.000 description 3
- 229920003023 plastic Polymers 0.000 description 3
- 239000004033 plastic Substances 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 239000012986 chain transfer agent Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 1
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 1
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 1
- LSDPWZHWYPCBBB-UHFFFAOYSA-N Methanethiol Chemical compound SC LSDPWZHWYPCBBB-UHFFFAOYSA-N 0.000 description 1
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 description 1
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 1
- 239000005642 Oleic acid Substances 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 238000009775 high-speed stirring Methods 0.000 description 1
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
- C08J3/226—Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2367/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2400/00—Characterised by the use of unspecified polymers
- C08J2400/10—Polymers characterised by the presence of specified groups, e.g. terminal or pendant functional groups
- C08J2400/102—Polymers characterised by the presence of specified groups, e.g. terminal or pendant functional groups containing halogen atoms
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2467/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2467/04—Polyesters derived from hydroxy carboxylic acids, e.g. lactones
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2471/00—Characterised by the use of polyethers obtained by reactions forming an ether link in the main chain; Derivatives of such polymers
-
- 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
- C08K3/02—Elements
- C08K3/04—Carbon
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Emulsifying, Dispersing, Foam-Producing Or Wetting Agents (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention relates to the technical field of dispersing agents, in particular to a preparation method and application of an environment-friendly inorganic powder dispersing agent, which at least comprise the following steps: (1) Mixing polyether acid ester and polycaprolactone polyol under the protection of nitrogen, and preserving heat for a certain time to obtain a mixture A; (2) And (3) after cooling, adding a processing aid into the mixture A, and mixing to obtain the dispersing agent. The inorganic powder dispersing agent obtained by the specific preparation method has good fluidity, not only can improve the dispersibility of the inorganic powder filling resin, but also well improves the compatibility of the inorganic powder and a polymer in the preparation process of the color master batch, and promotes the mechanical property and the processing property of the color master batch; by controlling the proportion of the specific polyether acid ester and the polycaprolactone polyol and the temperature and time for heat preservation and cooling, the generation of pungent smell in the preparation of the inorganic powder dispersing agent is well avoided, and the environment is protected; according to the invention, the fluorine-containing polymer additive with specific fluorine content is added into the dispersing agent, so that the fluidity of the prepared color master batch can be improved.
Description
Technical Field
The invention relates to the technical field of dispersants, in particular to an IPC (International patent Classification) No. C08F222/06, and more particularly relates to a preparation method and application of an environment-friendly inorganic powder dispersant.
Background
In the field of polymer materials such as rubber, plastics, chemical fibers, coatings and the like, inorganic powder such as filler or pigment is often added to endow the materials with excellent performance, but because an interfacial region exists between a resin matrix and the inorganic powder, the compatibility between the resin matrix and the inorganic powder is poor, so that the inorganic powder materials cannot be uniformly dispersed in organic resin, and the phenomenon of agglomeration is easy to occur.
Therefore, the appearance of the hyperdispersant has a remarkable effect on the dispersion of inorganic powder, however, some hyperdispersants on the market at present have relatively weak dispersing ability, and some hyperdispersants even contain a lot of toxic substances, so that the requirements on green environmental protection are not met. Chinese patent CN201510102492 discloses an amphiphilic hyper-dispersant and a preparation method thereof, wherein oleic acid, maleic anhydride, methyl methacrylate, azobisisobutyronitrile and isopropanol are mixed to obtain a solution A, the solution A is dropwise added into an acetone solution in an N2 protective environment and in a stirring state, the acetone solution is heated in a water bath at 60-80 ℃, the temperature is kept for 5-8 h after dropwise addition, the product is filtered, washed and dried to obtain the hyper-dispersant, nano copper powder and the hyper-dispersant are dissolved in an acetone solvent, the nano copper powder and the hyper-dispersant are heated in the water bath at 60-80 ℃ after ultrasonic dispersion, the high-speed stirring is carried out for 2-6 h, the product is filtered, washed and dried to obtain the amphiphilic hyper-dispersant, the dispersant has super-dispersing capacity, the non-environmental protection property of using mercaptan as a chain transfer agent is avoided by using the isopropanol as the chain transfer agent, but the azobisisobutyronitrile is still used in the dispersant, so that gas can be generated in the processing process, and the problem of environmental protection is not completely solved.
Disclosure of Invention
In view of the above-mentioned technical problems, one aspect of the present invention provides a method for preparing an environmentally friendly inorganic powder dispersant, which at least comprises the following steps:
(1) Mixing polyether acid ester and polycaprolactone polyol under the protection of nitrogen, and preserving heat for a certain time to obtain a mixture A;
(2) And (3) after cooling, adding a processing aid into the mixture A, and mixing to obtain the dispersing agent.
In some embodiments, the temperature of the incubation in step (1) is 70-80 ℃.
Preferably, the temperature for the incubation in step (1) is 75 ℃.
In some embodiments, the incubation time in step (1) is 30-60min.
Preferably, the time for heat preservation in the step (1) is 45min.
In some embodiments, the reduced temperature in step (2) is 40-50 ℃.
Preferably, the temperature reduction temperature in the step (2) is 40-45 ℃.
More preferably, the temperature reduction temperature in the step (2) is 43 ℃.
In some embodiments, the time for mixing in step (2) is 60-120min.
Preferably, the mixing time in the step (2) is 90min.
In some embodiments, the weight ratio of the polyetherester to polycaprolactone polyol is (0.6-1.5): 1.
in some embodiments, the polycaprolactone polyol is a polycaprolactone triol having a number average molecular weight of 1000 to 3000.
Preferably, the number average molecular weight of the polycaprolactone triol is 2000.
More preferably, the polycaprolactone triol is purchased from Henkel Handa Biotech, inc.
Preferably, the weight ratio of the polyetherester to the polycaprolactone polyol is 1.1:1.
in some embodiments, the preparation of the polyetherester comprises: mixing polyether polyol and anhydride, heating, keeping the temperature for a period of time, discharging, cooling and grinding to obtain the polyether acid ester.
In some embodiments, the molar ratio of polyether polyol to anhydride is 1: (1.05-1.2).
Preferably, the molar ratio of polyether polyol to anhydride is 1:1.15.
in some embodiments, the temperature is increased to 100-120 ℃ and the holding time is 2-4h.
Preferably, the temperature of the temperature rise is 105 ℃, and the time of heat preservation is 3h.
In some embodiments, the polyether polyol comprises polyethylene glycol and/or polypropylene glycol.
Preferably, the polyether polyol comprises polyethylene glycol and polypropylene glycol in a weight ratio of (1-2): 1.
more preferably, the polyether polyol comprises polyethylene glycol and polypropylene glycol in a weight ratio of 1.5:1.
in some embodiments, the polyethylene glycol has a number average molecular weight of 720 to 880 and a hydroxyl number of 127 to 156mgKOH/g.
Preferably, the polyethylene glycol is available from Shanghai chain aggregation chemical Co., ltd, and is PEG800.
In some embodiments, the polypropylene glycol has a number average molecular weight of 3000 and a hydroxyl number of 34 to 42mgKOH/g.
Preferably, the polypropylene glycol is available from Shanghai chain-concentrated chemical Co., ltd, and has a model number of PPG3000.
In some embodiments, the anhydride comprises maleic anhydride.
In some embodiments, the processing aid comprises a fluoropolymer aid having a fluorine content of 65% to 80%.
Preferably, the fluorine content of the fluorine-containing polymer auxiliary agent is 70-75%.
In some embodiments, the weight ratio of fluoropolymer coagent to polycaprolactone polyol is 1: (1.4-1.8).
Preferably, the weight ratio of the fluoropolymer auxiliary agent to the polycaprolactone polyol is 1:1.6.
the source of the fluoropolymer coagent is not particularly limited in this invention and includes, but is not limited to, the fluoropolymer coagent is available from Shanxi (Shanghai) Chemicals Co., ltd under the brand name of Japan Dajin DA912.
The applicant finds that the proportion of specific polyether acid ester and polycaprolactone polyol and the temperature and time for heat preservation and cooling are controlled, and particularly the weight ratio of the polyether acid ester to the polycaprolactone polyol is controlled to be (0.6-1.5): 1, the temperature of heat preservation in the step (1) is 70-80 ℃, the time of heat preservation is 30-60min, the temperature of cooling in the step (2) is controlled to be 40-45 ℃, and the time of mixing is 60-120min, so that the generation of pungent odor in the preparation of the inorganic powder dispersing agent is well avoided, and the inorganic powder dispersing agent is more environment-friendly. Although the applicant avoids the generation of unpleasant odor by controlling the raw material proportion and the process conditions, the applicant unexpectedly finds that the flowability of the masterbatch prepared after the dispersant is used in the masterbatch preparation process is low, and meanwhile, some masterbatch on the market at present has the problem of poor flowability, so that the production period of the prepared plastic product is prolonged, and the appearance quality of the plastic product is also affected.
The invention also provides a method for preparing the environment-friendly inorganic powder dispersing agent, and the dispersing agent prepared by the method is used for dispersing the pigment and the filler in the color master batch.
Has the advantages that:
the inorganic powder dispersing agent obtained by the specific preparation method has good fluidity, not only can improve the dispersibility of the inorganic powder filling resin, but also well improves the compatibility of the inorganic powder and a polymer in the preparation process of the color master batch, and promotes the mechanical property and the processing property of the color master batch; by controlling the proportion of the specific polyether acid ester and the polycaprolactone polyol and the temperature and time for heat preservation and cooling, the generation of pungent odor in the preparation of the inorganic powder dispersing agent is well avoided, and the environment is protected; according to the invention, the fluorine-containing polymer auxiliary agent with specific fluorine content is added into the dispersing agent, and particularly, the fluidity of the prepared color master batch can be improved when the fluorine content is 70-75%; the inorganic powder dispersant is used in a small amount of 0.5 to 2% by mass.
Detailed Description
Example 1
A preparation method of an environment-friendly inorganic powder dispersing agent comprises the following steps:
(1) Mixing the polyether acid ester and the polycaprolactone polyol under the protection of nitrogen, and keeping the temperature at 75 ℃ for 45min to obtain a mixture A;
(2) And (3) cooling to 43 ℃, adding a fluorine-containing polymer auxiliary agent into the mixture A, and mixing for 90min to obtain the dispersing agent.
The weight ratio of the polyether acid ester to the polycaprolactone polyol is 1.1:1.
the polycaprolactone polyol is polycaprolactone triol with the number average molecular weight of 2000 and is purchased from Hubei Handafei Biotech limited.
The weight ratio of the fluorine-containing polymer auxiliary agent to the polycaprolactone triol is 1:1.6.
the preparation of the polyether acid ester comprises the following steps: mixing polyether polyol and maleic anhydride, heating to 105 ℃, keeping the temperature for 3 hours, discharging, cooling and grinding to obtain the polyether acid ester.
The molar ratio of the polyether polyol to the maleic anhydride is 1:1.15.
the polyether polyol comprises polyethylene glycol and polypropylene glycol, and the weight ratio is 1.5:1.
the polyethylene glycol is purchased from Shanghai chain-aggregation chemical Co., ltd, and has the type of PEG800, the number average molecular weight of 720-880 and the hydroxyl value of 127-156mgKOH/g; the number average molecular weight of the polypropylene glycol is 3000, and the hydroxyl value is 34-42mgKOH/g.
The fluorine-containing polymer additive is purchased from Shangxi (Shanghai) chemical additive Co., ltd, and is of a brand of Japanese gold DA912, and the fluorine content is 70-75%.
Example 2
A preparation method of an environment-friendly inorganic powder dispersing agent comprises the following steps:
(1) Mixing the polyether acid ester and the polycaprolactone polyol under the protection of nitrogen, and keeping the temperature at 70 ℃ for 60min to obtain a mixture A;
(2) And (3) cooling to 40 ℃, adding a fluorine-containing polymer auxiliary agent into the mixture A, and mixing for 120min to obtain the dispersing agent.
The weight ratio of the polyether acid ester to the polycaprolactone polyol is 0.6:1.
the polycaprolactone polyol is polycaprolactone triol with the number average molecular weight of 2000, and is purchased from Henkel Handa Daifei Biotech, inc.
The weight ratio of the fluoropolymer additive to the polycaprolactone triol is 1:1.4.
the preparation of the polyether acid ester comprises the following steps: mixing polyether polyol and maleic anhydride, heating to 100 ℃, keeping the temperature for 4 hours, discharging, cooling and grinding to obtain the polyether acid ester.
The molar ratio of the polyether polyol to the maleic anhydride is 1:1.15.
the polyether polyol comprises polyethylene glycol and polypropylene glycol, and the weight ratio is 1:1.
the polyethylene glycol is purchased from Shanghai chain-aggregation chemical Co., ltd, and has the type of PEG800, the number average molecular weight of 720-880 and the hydroxyl value of 127-156mgKOH/g; the number average molecular weight of the polypropylene glycol is 3000, and the hydroxyl value is 34-42mgKOH/g.
The fluorine-containing polymer additive is purchased from Shanxi (Shanghai) chemical additive limited company, and is of a brand of Japan Dajin DA912, and the fluorine content is 70-75%.
Example 3
A preparation method of an environment-friendly inorganic powder dispersing agent comprises the following steps:
(1) Mixing the polyether acid ester and the polycaprolactone polyol under the protection of nitrogen, and keeping the temperature at 80 ℃ for 30min to obtain a mixture A;
(2) And (3) cooling to 45 ℃, adding a fluorine-containing polymer auxiliary agent into the mixture A, and mixing for 90min to obtain the dispersing agent.
The weight ratio of the polyether acid ester to the polycaprolactone polyol is 1.5:1.
the polycaprolactone polyol is polycaprolactone triol with the number average molecular weight of 2000, and is purchased from Henkel Handa Daifei Biotech, inc.
The weight ratio of the fluorine-containing polymer auxiliary agent to the polycaprolactone triol is 1:1.8.
the preparation of the polyether acid ester comprises the following steps: mixing polyether polyol and maleic anhydride, heating to 120 ℃, keeping the temperature for 2h, discharging, cooling and grinding to obtain the polyether acid ester.
The molar ratio of the polyether polyol to the maleic anhydride is 1:1.15.
the polyether polyol comprises polyethylene glycol and polypropylene glycol, and the weight ratio is 2:1.
the polyethylene glycol is purchased from Shanghai chain chemical Co., ltd, the type is PEG800, the number average molecular weight is 720-880, and the hydroxyl value is 127-156mgKOH/g; the number average molecular weight of the polypropylene glycol is 3000, and the hydroxyl value is 34-42mgKOH/g.
The fluorine-containing polymer additive is purchased from Shanxi (Shanghai) chemical additive limited company, and is of a brand of Japan Dajin DA912, and the fluorine content is 70-75%.
Example 4
The embodiment provides a preparation method of an environment-friendly inorganic powder dispersing agent, and the specific implementation manner is the same as that of embodiment 1, except that no fluoropolymer auxiliary agent is added.
Example 5
The embodiment of the present invention provides a method for preparing an environment-friendly inorganic powder dispersant, which is the same as embodiment 1 except that the mixing time in step (2) is 50min.
Performance testing
The inorganic powder dispersing agent and the carbon black described in the embodiments 1 to 5 were added to PET resin, and the mixture was mixed, extruded, and granulated to obtain carbon black master batch.
The carbon black master batch comprises, by mass, 0.6% of an inorganic powder auxiliary agent, 30% of carbon black and the balance of PET resin.
The melt index of the PET resin under the condition of 260 ℃/2.16kg is 14g/10min.
1. Melt flow rate
The carbon black master batches corresponding to examples 1 to 5 were subjected to melt flow rate measurement according to GB/T3682, and the results are shown in Table 1.
TABLE 1
| Number of | Melt flow Rate (g/10 min) |
| Example 1 | 2.8 |
| Example 2 | 2.5 |
| Example 3 | 2.7 |
| Example 4 | 1.5 |
| Example 5 | 2.0 |
| Without adding dispersant | 0.3 |
Claims (10)
1. The preparation method of the environment-friendly inorganic powder dispersant is characterized by at least comprising the following steps:
(1) Mixing polyether acid ester and polycaprolactone polyol under the protection of nitrogen, and preserving heat for a certain time to obtain a mixture A;
(2) And (3) after cooling, adding a processing aid into the mixture A, and mixing to obtain the dispersing agent.
2. The method for preparing the environment-friendly inorganic powder dispersing agent as claimed in claim 1, wherein the temperature for heat preservation in the step (1) is 70-80 ℃.
3. The method for preparing the environment-friendly inorganic powder dispersing agent as claimed in claim 1, wherein the heat preservation time in the step (1) is 30-60min.
4. The method for preparing the environment-friendly inorganic powder dispersant according to claim 1, wherein the temperature reduction temperature in the step (2) is 40-50 ℃.
5. The method for preparing the environment-friendly inorganic powder dispersant of claim 1, wherein the mixing time in the step (2) is 60-120min.
6. The method for preparing the environment-friendly inorganic powder dispersing agent as claimed in any one of claims 1 to 5, wherein the weight ratio of the polyether ester to the polycaprolactone polyol is (0.6-1.5): 1.
7. the method for preparing the environment-friendly inorganic powder dispersant of claim 6, wherein the preparation of the polyether acid ester comprises: mixing polyether polyol and anhydride, heating, keeping the temperature for a period of time, discharging, cooling and grinding to obtain the polyether acid ester.
8. The method of claim 6, wherein the acid anhydride comprises maleic anhydride.
9. The method for preparing the environment-friendly inorganic powder dispersant of claim 1, wherein the processing aid comprises a fluorine-containing polymer aid, and the fluorine content of the fluorine-containing polymer aid is 65-80%.
10. The dispersant prepared by the preparation method of the environment-friendly inorganic powder dispersant of any one of claims 1 to 9 is used for dispersing pigments and fillers in polymers.
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| US5565497A (en) * | 1995-12-07 | 1996-10-15 | The Celotex Corporation | Dispersant for filled, rigid cellular polymers |
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