CN106083915A - A kind of synthetic method of polarity polyether-type titanate coupling agent - Google Patents
A kind of synthetic method of polarity polyether-type titanate coupling agent Download PDFInfo
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- CN106083915A CN106083915A CN201610419975.7A CN201610419975A CN106083915A CN 106083915 A CN106083915 A CN 106083915A CN 201610419975 A CN201610419975 A CN 201610419975A CN 106083915 A CN106083915 A CN 106083915A
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- coupling agent
- polarity
- polyether
- titanate coupling
- organic solvent
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- 239000007822 coupling agent Substances 0.000 title claims abstract description 33
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 238000010189 synthetic method Methods 0.000 title claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims abstract description 13
- 239000000463 material Substances 0.000 claims abstract description 13
- 229920000570 polyether Polymers 0.000 claims abstract description 13
- 239000003960 organic solvent Substances 0.000 claims abstract description 12
- DLYUQMMRRRQYAE-UHFFFAOYSA-N tetraphosphorus decaoxide Chemical compound O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 claims abstract description 10
- XPPKVPWEQAFLFU-UHFFFAOYSA-J diphosphate(4-) Chemical compound [O-]P([O-])(=O)OP([O-])([O-])=O XPPKVPWEQAFLFU-UHFFFAOYSA-J 0.000 claims abstract description 9
- 235000011180 diphosphates Nutrition 0.000 claims abstract description 9
- 239000004721 Polyphenylene oxide Substances 0.000 claims abstract description 8
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 claims abstract description 6
- 150000001298 alcohols Chemical class 0.000 claims abstract description 5
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 3
- 230000006837 decompression Effects 0.000 claims description 6
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 3
- LQZZUXJYWNFBMV-UHFFFAOYSA-N dodecan-1-ol Chemical class CCCCCCCCCCCCO LQZZUXJYWNFBMV-UHFFFAOYSA-N 0.000 claims description 2
- 150000008282 halocarbons Chemical class 0.000 claims description 2
- 239000001294 propane Substances 0.000 claims description 2
- 239000002131 composite material Substances 0.000 abstract description 12
- 238000000034 method Methods 0.000 abstract description 10
- 230000000694 effects Effects 0.000 abstract description 8
- 230000008569 process Effects 0.000 abstract description 3
- 229920006112 polar polymer Polymers 0.000 abstract description 2
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 12
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 11
- 238000003786 synthesis reaction Methods 0.000 description 9
- 230000015572 biosynthetic process Effects 0.000 description 8
- 239000013078 crystal Substances 0.000 description 6
- 239000000945 filler Substances 0.000 description 6
- 239000011159 matrix material Substances 0.000 description 6
- 239000003795 chemical substances by application Substances 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 239000002202 Polyethylene glycol Substances 0.000 description 4
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 4
- 230000003993 interaction Effects 0.000 description 4
- 229920001223 polyethylene glycol Polymers 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 229920001971 elastomer Polymers 0.000 description 3
- 239000000806 elastomer Substances 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 239000011256 inorganic filler Substances 0.000 description 3
- 229910003475 inorganic filler Inorganic materials 0.000 description 3
- 238000012805 post-processing Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- KNKRKFALVUDBJE-UHFFFAOYSA-N 1,2-dichloropropane Chemical compound CC(Cl)CCl KNKRKFALVUDBJE-UHFFFAOYSA-N 0.000 description 2
- KBPLFHHGFOOTCA-UHFFFAOYSA-N 1-Octanol Chemical compound CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000012675 alcoholic extract Substances 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000002329 infrared spectrum Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- BWDBEAQIHAEVLV-UHFFFAOYSA-N 6-methylheptan-1-ol Chemical compound CC(C)CCCCCO BWDBEAQIHAEVLV-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- WYRGOSDNPFGZFG-UHFFFAOYSA-K [bis(2-ethylhexoxy)-oxidophosphaniumyl] dihydrogen phosphate [bis(2-ethylhexoxy)-oxidophosphaniumyl] hydrogen phosphate [bis(2-ethylhexoxy)-oxidophosphaniumyl] phosphate propan-2-olate titanium(4+) Chemical compound [Ti+4].CC(C)[O-].CCCCC(CC)CO[P+]([O-])(OCC(CC)CCCC)OP(O)(O)=O.CCCCC(CC)CO[P+]([O-])(OCC(CC)CCCC)OP(O)([O-])=O.CCCCC(CC)CO[P+]([O-])(OCC(CC)CCCC)OP([O-])([O-])=O WYRGOSDNPFGZFG-UHFFFAOYSA-K 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 150000004645 aluminates Chemical class 0.000 description 1
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- IKRMZAOEXULJQX-UHFFFAOYSA-N calcium;3,7-dioxido-2,4,6,8,9-pentaoxa-1,3,5,7-tetraborabicyclo[3.3.1]nonane Chemical compound [Ca+2].O1B([O-])OB2OB([O-])OB1O2 IKRMZAOEXULJQX-UHFFFAOYSA-N 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 230000003750 conditioning effect Effects 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000009863 impact test Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000010128 melt processing Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229920013657 polymer matrix composite Polymers 0.000 description 1
- 239000011160 polymer matrix composite Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920000098 polyolefin Polymers 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/003—Compounds containing elements of Groups 4 or 14 of the Periodic Table without C-Metal linkages
-
- 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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/08—Oxygen-containing compounds
-
- 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
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/02—Compounds of alkaline earth metals or magnesium
- C09C1/025—Calcium sulfates
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/08—Treatment with low-molecular-weight non-polymer organic compounds
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses the synthetic method of a kind of polarity polyether-type titanate coupling agent, synthetic reaction route is divided into two steps: the ratio of low molecule alcohols material and little molecule polyethers 1:1 to 10:1 in molar ratio is mixed by the first step, add and account for the organic solvent that total weight percent is 10% to 100%, under the temperature conditions of 40 90 DEG C, the phosphorus pentoxide with 0.1 1.0 moles reacts 15 hours, obtains the pyrophosphate containing polarity segment.Gained polarity pyrophosphate is mixed mutually with the molar ratio of 1:1 to 10:1 in the organic solvent accounting for gross weight 1% 100% by second step with isopropyl titanate, reacts 15 hours, obtain end product polarity polyether titanate coupling agent at 30 95 DEG C.The building-up process of coupling agent of the present invention is simple, and polar polymer based composites is had good modified effect.
Description
Technical field
The present invention relates to chemical synthesis technique field, the synthesis of a kind of polarity polyether-type titanate coupling agent
Method.
Background technology
Inorganic filler has obtained being widely applied very much as the activeness and quietness modifying agent of polymeric material, and it can improve material
The elastic modelling quantity of material, impact flexibility and reduce the manufacturing cost of material.And interface between filler and polymeric matrix is mutual
Act on the combination property on composite and affect the biggest.It is typically due to the difference of polarity and aggregated structure, filler and polymerization
The compatibility of thing matrix is poor, and the combination property causing composite is poor, it is therefore desirable to filler is carried out certain surface
Managing to improve interface adhesion therebetween, research novel surface inorganic agent is an important research of current research worker
Direction.
The stuffing surface modification agent being typically used for has silane, titanate esters, aluminate coupling agent etc., although they can be certain
Degree improves the dispersibility of filler, but the most weak with the interaction of polymeric matrix, does not has the strongest specific aim.According to
The report of patent (CN1036787C), uses coupling agent can improve with reactive elastomer oligomer Combined Processing filling surface
Interface adhesion between filler and polymeric matrix, improves the combination property of material.But the system due to reactive elastomer
Standby cost is high, so being unfavorable for large-scale application, and patent (CN1597749A) proposes to use end hydroxy polyether oligomer with low
Molecule alcohol is as Material synthesis polyether titanate coupling agent, and its preparation process is simpler than the former, but the end hydroxyl used due to it
Base pfpe molecule amount is between 200-5000, and higher molecular weight can make the reaction viscosity of system raise, post processing difficulty.
Summary of the invention
It is an object of the invention to provide the synthetic method of a kind of polarity polyether-type titanate coupling agent, utilize little molecule to gather
The reaction preparation between alcoholic extract hydroxyl group and phosphorus pentoxide and isopropyl titanate in the ether coupling containing polarized organo-functional group
Agent, utilizes the polarity ehter bond in pfpe molecule chain and alcoholic extract hydroxyl group, the interaction between reinforcer and polar polymer matrix,
So improving the combination property of composite.This preparation method is very simple, and treatment effect is good, it is possible to significantly improve polarity
The impact strength of polymer matrix composite, elastic modelling quantity, play the effect of activeness and quietness.
For realizing above-mentioned technical purpose, reach above-mentioned technique effect, the invention discloses a kind of polarity polyether-type titanate esters
The synthetic method of coupling agent, synthetic route is divided into two steps:
The first step: the ratio of low molecule alcohols material and little molecule polyethers 1:1-10:1 in molar ratio mixed, adds and accounts for gross weight
Amount percentage ratio is the organic solvent of 10-100%, and under the temperature conditions of 40-90 DEG C, the phosphorus pentoxide with 0.1-1.0 mole is anti-
Answering 1-5 hour, after reaction terminates, decompression is distilled off organic solvent, obtains the pyrophosphate containing polarity segment；
Second step: by gained polarity pyrophosphate and isopropyl titanate with 1:1-in the organic solvent account for gross weight 1-100%
The molar ratio of 10:1 mixes mutually, reacts 1-5 hour at 30-95 DEG C, and after reaction terminates, decompression is distilled off organic solvent,
To end product polarity polyether titanate coupling agent.
Wherein, low molecule alcohols material is that propane is to any one of dodecyl mono-alcohols.
Wherein, the molecular weight of little molecule polyethers is less than or equal to 200.
Wherein, one or more the mixture during organic solvent is halogenated hydrocarbons.
The method have the advantages that
1. the present invention passes through optimization of synthesis, compared with traditional high molecular weight polyether synthesis technique, coupling agent of the present invention
Building-up process system viscosity is less, and reaction compares easily, and product postprocessing is simple.
After coupling agent treatment inorganic filler the most of the present invention, polar polyolefin plastics there are is good modified effect, be better than commercially available
Titanate coupling agent, and with coupling agent compared with the method for reactive elastomer oligomer Combined Processing, this method operation letter
Single easy, experimental cost is relatively low, has good storage stability.
Accompanying drawing explanation
Fig. 1 is the schematic flow sheet of the present invention.
Fig. 2 is the infrared spectrum characterization figure of product of the present invention, and wherein Fig. 2 (a) pyrophosphate, (b) make polyether-type metatitanic acid by oneself
The infrared spectrogram of ester coupling agent
Fig. 3 is different calcium sulfate crystal whiskers/PVC composite Tensile fracture scanning electron microscope (SEM) photographs, and wherein Fig. 3 (a) is unmodified, (b) ratio
Relatively example, (c) embodiment 1.
Detailed description of the invention
In order to make the purpose of the present invention, technical scheme and advantage clearer, below in conjunction with drawings and Examples, right
The present invention is further elaborated.
Embodiment 1
As it is shown in figure 1, the invention discloses the synthetic method of a kind of polarity polyether-type titanate coupling agent, synthetic route is divided into two
Step:
The synthesis of polarity pyrophosphate: be separately added into 50ml dichloropropane in 250ml there-necked flask, mol ratio is the different of 1:1
Capryl alcohol and Polyethylene Glycol, with the phosphorus pentoxide that mol ratio is 1:1 of isooctanol and Polyethylene Glycol, reaction temperature is less than 60 DEG C,
Response time is 2 hours.After reaction terminates, decompression is distilled off solvent, obtains colorless viscous shape liquid.
The synthesis of polarity polyether titanate coupling agent: add 40ml solvent dichloropropane in 250ml there-necked flask, add afterwards
Enter isopropyl titanate, and at the pyrophosphate of the room temperature above-mentioned synthesis of dropping, the mol ratio of the two is 2:1, reaction temperature 80 DEG C, instead
After answering time 2 h, reaction to terminate, decompression is distilled off solvent, obtains faint yellow viscous liquid.
Embodiment 2
The invention discloses the synthetic method of a kind of polarity polyether-type titanate coupling agent, concrete synthetic method with embodiment 1,
Wherein Polyethylene Glycol replaces with diethylene glycol.
Embodiment 3
The invention discloses the synthetic method of a kind of polarity polyether-type titanate coupling agent, concrete synthetic method with embodiment 1,
Wherein Polyethylene Glycol replaces with diethylene glycol.
Embodiment 4
The invention discloses the synthetic method of a kind of polarity polyether-type titanate coupling agent, concrete synthetic method with embodiment 1,
Wherein isopropyl titanate replaces with tetrabutyl titanate.
Embodiment 5
Experiment purpose: synthesize feasibility and the effectiveness of polarity polyether titanate coupling agent, the present embodiment in order to contrast the present invention
Obtain, synthesized by embodiment 1, the titanate coupling agent (NDZ-201, Nanjing Dao Ning chemical company) that product contrast is commercially available, with
Calcium sulfate crystal whiskers filling pvc composite is that experimental subject is modified performance comparison experiment.
Experimental technique:
The surface of calcium sulfate crystal whiskers processes: by coupling agent fully dispersed hydrolysis in ethanol water, join afterwards equipped with sulfur
In the there-necked flask of acid calcium pyroborate, coupling agent consumption is 2.5%, mixture reacts at 75 DEG C 4h, by product after having reacted
Sucking filtration, is placed in 100 DEG C of baking ovens and is dried, the calcium sulfate crystal whiskers after being processed.
The preparation of composite: the whisker handled well is mixed with Corvic, molten in two-roll mill
Melt processing, be prepared as composite board, cut out sample, prepare test bars.
Material properties test: the batten of preparation is carried out Mechanics Performance Testing.Tension test is entered according to ISO 527 standard
OK, impact test is carried out according to ISO 180:2000 standard.
Experimental result:
Table 1 surface conditioning agent is on calcium sulfate crystal whiskers/PVC composite property impact (Whisker Content 10%)
| Sample | Hot strength (MPa) | Elastic modelling quantity (MPa) | Elongation at break (%) | Impact strength kJ m<sup>-2</sup> |
| Unmodified calcium sulfate crystal whiskers/PVC | 55±0.7 | 1727±36 | 95±16 | 7.7±0.4 |
| Comparative example | 56±0.8 | 1742±20 | 213±2.8 | 8.5±2.0 |
| Embodiment 1 | 67±0.5 | 1926±27 | 233±14 | 12.8±1.9 |
By data in table 1 it can be seen that the hot strength of sample, elastic modelling quantity, elongation at break and impact strength in embodiment 1
It is all remarkably higher than unmodified composite and comparative example, especially elongation at break and impact strength, is unmodified composite
2.5 and 1.7 times, also improve a lot compared with comparative example.Treatment effect is the most notable.The synthesis of coupling agent of the present invention
Journey is simple, and reaction is easily carried out, and product postprocessing is easy.Obvious to filler treatment effect, it is possible to be effectively improved inorganic filler
And the interfacial interaction between polar organic polymer, improves the combination property of composite, and the application of Suitable commercial level pushes away
Extensively.
Fig. 2 is the infrared spectrum that embodiment 1 prepares coupling agent, and the characteristic absorption peak from figure can be seen that and successfully makes
For having obtained target product.And the tensile fracture-surface contrast of three kinds of materials more can significantly be found out through embodiment 1 in Fig. 3
Interfacial interaction between modified whisker and matrix is obviously enhanced, and obvious agglomeration does not occurs in whisker, so showing
The modified effect that embodiment 1 is good.
The above, the only present invention preferably detailed description of the invention, but protection scope of the present invention is not limited thereto,
Any those familiar with the art in the technical scope that the invention discloses, the change that can readily occur in or replacement,
All should contain within protection scope of the present invention.
Claims (4)
1. the synthetic method of a polarity polyether-type titanate coupling agent, it is characterised in that synthetic route is divided into two steps:
The first step: the ratio of low molecule alcohols material and little molecule polyethers 1:1-10:1 in molar ratio mixed, adds and accounts for gross weight
Amount percentage ratio is the organic solvent of 10-100%, and under the temperature conditions of 40-90 DEG C, the phosphorus pentoxide with 0.1-1.0 mole is anti-
Answering 1-5 hour, after reaction terminates, decompression is distilled off organic solvent, obtains the pyrophosphate containing polarity segment；
Second step: by gained polarity pyrophosphate and isopropyl titanate with 1:1-in the organic solvent account for gross weight 1-100%
The molar ratio of 10:1 mixes mutually, reacts 1-5 hour at 30-95 DEG C, and after reaction terminates, decompression is distilled off organic solvent,
To end product polarity polyether titanate coupling agent.
The synthetic method of a kind of polarity polyether-type titanate coupling agent the most as claimed in claim 1, it is characterised in that: described
Low molecule alcohols material is that propane is to any one of dodecyl mono-alcohols.
The synthetic method of a kind of polarity polyether-type titanate coupling agent the most as claimed in claim 1 or 2, it is characterised in that: institute
The molecular weight of the little molecule polyethers stated is less than or equal to 200.
The synthetic method of a kind of polarity polyether-type titanate coupling agent the most as claimed in claim 3, it is characterised in that: described
Organic solvent is one or more the mixture in halogenated hydrocarbons.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610419975.7A CN106083915A (en) | 2016-06-13 | 2016-06-13 | A kind of synthetic method of polarity polyether-type titanate coupling agent |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610419975.7A CN106083915A (en) | 2016-06-13 | 2016-06-13 | A kind of synthetic method of polarity polyether-type titanate coupling agent |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106083915A true CN106083915A (en) | 2016-11-09 |
Family
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610419975.7A Pending CN106083915A (en) | 2016-06-13 | 2016-06-13 | A kind of synthetic method of polarity polyether-type titanate coupling agent |
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| Country | Link |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111718641A (en) * | 2020-06-30 | 2020-09-29 | 莆田学院 | Preparation method of P/Si synergistic flame-retardant acrylate coating |
| CN114806403A (en) * | 2022-04-14 | 2022-07-29 | 湖南石油化工职业技术学院 | Surface treating agent capable of improving adhesive property, preparation method and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2947774A (en) * | 1956-04-25 | 1960-08-02 | Charles A Levine | Preparation of alkyl pyrophosphate extractants |
| US4338220A (en) * | 1979-08-29 | 1982-07-06 | Kenrich Petrochemicals, Inc. | Pyrophosphato titanate adducts |
| CN1597749A (en) * | 2004-08-19 | 2005-03-23 | 南京工业大学 | Synthesis method of polyether titanate coupling agent |
-
2016
- 2016-06-13 CN CN201610419975.7A patent/CN106083915A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2947774A (en) * | 1956-04-25 | 1960-08-02 | Charles A Levine | Preparation of alkyl pyrophosphate extractants |
| US4338220A (en) * | 1979-08-29 | 1982-07-06 | Kenrich Petrochemicals, Inc. | Pyrophosphato titanate adducts |
| CN1597749A (en) * | 2004-08-19 | 2005-03-23 | 南京工业大学 | Synthesis method of polyether titanate coupling agent |
Non-Patent Citations (2)
| Title |
|---|
| 朱凤娥: "聚醚钛酸酯偶联剂的合成及其增韧聚烯烃的研究", 《南京理工大学硕士学位论文》 * |
| 朱凤娥等: "聚醚钛酸酯合成及其对聚烯烃/CaCO3力学性能影响", 《南京工业大学学报(自然科学版)》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111718641A (en) * | 2020-06-30 | 2020-09-29 | 莆田学院 | Preparation method of P/Si synergistic flame-retardant acrylate coating |
| CN111718641B (en) * | 2020-06-30 | 2021-11-23 | 莆田学院 | Preparation method of P/Si synergistic flame-retardant acrylate coating |
| CN114806403A (en) * | 2022-04-14 | 2022-07-29 | 湖南石油化工职业技术学院 | Surface treating agent capable of improving adhesive property, preparation method and application thereof |
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