CN107602607A - A kind of water-soluble titanate coupling agent and preparation method thereof - Google Patents
A kind of water-soluble titanate coupling agent and preparation method thereof Download PDFInfo
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- CN107602607A CN107602607A CN201710712047.4A CN201710712047A CN107602607A CN 107602607 A CN107602607 A CN 107602607A CN 201710712047 A CN201710712047 A CN 201710712047A CN 107602607 A CN107602607 A CN 107602607A
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- 0 **ON*(*)C1C*C1 Chemical compound **ON*(*)C1C*C1 0.000 description 1
Abstract
This case discloses a kind of water-soluble titanate coupling agent and preparation method thereof, and chelating agent is put into reaction vessel by it at 60 80 DEG C, and pH is between 6.5 7.5 for regulation, and control rotating speed is in 1000 3000rpm, stirring, and 0.5 2h of backflow is to be preheated；Nitrogen is passed through to reaction vessel, and temperature is risen to 80 100 DEG C, adds titanium ion, control rotating speed is in 1000 3000rpm, stirring, the 5h of back flow reaction 3, acrylic acid is then added, continue the 5h of back flow reaction 3, stop stirring, stand 1 5h, be cooled to room temperature, produce water-soluble titanate coupling agent.This case is as obtained by titanium ion organic compound and chelating agent exchange alkoxy preparation, and its raw material is simple and easy to get, and preparation method is simple and easy to do；It can be applied in the water-soluble chemical products such as water paint, water-based ink, there is excellent crosslinking ability and dispersibility.
Description
Technical field
The present invention relates to a kind of titanate coupling agent, and in particular to a kind of water-soluble titanate coupling agent and its preparation side
Method.
Background technology
Titanate coupling agent is to grow up in the latter stage seventies, a kind of to be used for coating, ink, the auxiliary agent of new type rubber,
Itself has the organic titanic compound of two kinds of differential responses active groups, and it can carry out reactivity with organic matter or inorganic matter
Crosslinking, as organic matter and organic matter, organic matter and inorganic matter, or even the friendship of inorganic matter and inorganic matter in many industrial productions
The bridge of connection；Because its preparation is simple, excellent effect, it is easy to use the advantages that be widely used.
In recent years, because environmental pressure is increasing, many chemical products, such as：Coating, ink etc. are all changed by solvent-borne type
To be water-based, because conventional solvent is changed as water as solvent, so as to mitigate environmental pressure.For titanate coupling agent, it can
To dissolve in a solvent, so as to play a part of crosslinking, and titanate coupling agent easily hydrolyzes in water, the titanium after hydrolysis
Acid esters coupling agent and then lose crosslinking ability.
To cater to environmental requirement, searching can be very urgent in water miscible titanate coupling agent.Water-soluble titanium acid esters is even
It is exactly to slow down its hydrolysis rate in water to join preparing most important for agent, improves its stability in aqueous.For gold
Belong to ionic reaction for, chemical reaction be and its acutely.
The content of the invention
In view of the deficiencies of the prior art, it is an object of the invention to provide a kind of water-soluble titanate coupling agent and its
Preparation method, it makes it have more stable structure, come real by being chemically modified to traditional solvent-borne titanate coupling agent
Now to the improvement of hydrolytic stability, and ensure that titanate coupling agent possesses two or more active groups.
To achieve the above object, technical scheme is summarized as follows：
A kind of water-soluble titanate coupling agent, it has following chemical formula：
Wherein ,-OR1CH(R2) O- is chelation group, its from ethylene glycol, 1,3-PD, glycerine, 1,2- butanediols,
Any of lactic acid, ethanedioic acid, glycine.
A kind of preparation method of water-soluble titanate coupling agent as described above, it comprises the following steps：
Step 1：Chelating agent is put into reaction vessel at 60-80 DEG C, pH is between 6.5-7.5 for regulation, controls rotating speed
In 1000-3000rpm, stirring, 0.5-2h is flowed back to be preheated；
Step 2：Nitrogen is passed through to reaction vessel, and temperature is risen to 80-100 DEG C, adds the titanium ion (titanium described in this case
Ion refers generally to titanium ion organic compound, and formula is Ti (OR)4, this case may be selected from butyl titanate or tetra isopropyl metatitanic acid
Ester), control rotating speed stirring, back flow reaction 3-5h, then adds acrylic acid in 1000-3000rpm, continues back flow reaction 3-5h,
Stop stirring, stand 1-5h, be cooled to room temperature, produce water-soluble titanate coupling agent.
Preferably, the preparation method of described water-soluble titanate coupling agent, wherein, the acrylic acid and titanium ion
Mol ratio is 2: 1.
Preferably, the preparation method of described water-soluble titanate coupling agent, wherein, the chelating agent and titanium ion
Mol ratio is 1-2: 1.
The beneficial effects of the invention are as follows：(1) this case exchanges alkoxy by titanium ion organic compound and chelating agent and prepared
Gained, its raw material is simple and easy to get, and preparation method is simple and easy to do, and reaction condition facilitates easily-controllable；(2) titanate coupling agent described in this case
Water solubility can be fully achieved, there is very high hydrolytic stability in water；(3) titanate coupling agent described in this case can be applied to
In the water-soluble chemical products such as water paint, water-based ink, there is excellent crosslinking ability and dispersibility.
Embodiment
With reference to embodiment, the present invention is described in further detail, to make those skilled in the art with reference to specification
Word can be implemented according to this.
Embodiment 1
A kind of preparation method of water-soluble titanate coupling agent, is comprised the following steps that：
Step 1, at 60 DEG C chelating agent (1,3-PD) is put into container, regulation pH is 6.5, and control rotating speed exists
1000r/min uniform stirrings, back flow reaction 1h are preheated.
Step 2, it is passed through protective gas N2, and temperature is warming up to 80 DEG C, it is slowly added to titanium ion (tetra isopropyl metatitanic acid
Ester), control rotating speed back flow reaction 3h, then adds acrylic acid in 1000rpm uniform stirrings, continues back flow reaction 3h, stops stirring
Mix, stand 1h, be cooled to room temperature and be transferred in beaker, produce titanate coupling agent.
Chelating agent, titanium ion, the mol ratio of acrylic acid are 1: 1: 2.
Embodiment 2
A kind of preparation method of water-soluble titanate coupling agent, is comprised the following steps that：
Step 1, at 80 DEG C chelating agent (1,3-PD) is put into container, regulation pH is 7.5, and control rotating speed exists
3000r/min uniform stirrings, back flow reaction 0.5h are preheated.
Step 2, it is passed through protective gas N2, and temperature is warming up to 100 DEG C, it is slowly added to titanium ion (tetra isopropyl metatitanic acid
Ester), control rotating speed back flow reaction 5h, then adds acrylic acid in 3000rpm uniform stirrings, continues back flow reaction 5h, stops stirring
Mix, stand 3h, be cooled to room temperature and be transferred in beaker, produce titanate coupling agent.
Chelating agent, titanium ion, the mol ratio of acrylic acid are 2: 1: 2.
Embodiment 3
A kind of preparation method of water-soluble titanate coupling agent, is comprised the following steps that：
Step 1, at 70 DEG C chelating agent (1,3-PD) is put into container, regulation pH is 7, and control rotating speed is in 2000r/
Min uniform stirrings, back flow reaction 2h are preheated.
Step 2, it is passed through protective gas N2, and temperature is warming up to 89 DEG C, it is slowly added to titanium ion (tetra isopropyl metatitanic acid
Ester), control rotating speed back flow reaction 3.5h, then adds acrylic acid in 2500rpm uniform stirrings, continues back flow reaction 4h, stops
Stirring, 4h is stood, room temperature is cooled to and is transferred in beaker, produce titanate coupling agent.
Chelating agent, titanium ion, the mol ratio of acrylic acid are 1: 1: 2.
Embodiment 4
A kind of preparation method of water-soluble titanate coupling agent, is comprised the following steps that：
Step 1, at 75 DEG C chelating agent (1,3-PD) is put into container, between regulation pH is 7, control rotating speed exists
2800r/min uniform stirrings, back flow reaction 2h are preheated.
Step 2, it is passed through protective gas N2, and temperature is warming up to 95 DEG C, it is slowly added to titanium ion (tetra isopropyl metatitanic acid
Ester), control rotating speed back flow reaction 3h, then adds acrylic acid in 2600rpm uniform stirrings, continues back flow reaction 5h, stops stirring
Mix, stand 2h, be cooled to room temperature and be transferred in beaker, produce titanate coupling agent.
Chelating agent, titanium ion, the mol ratio of acrylic acid are 1: 1: 2.
Embodiment 5
A kind of preparation method of water-soluble titanate coupling agent, is comprised the following steps that：
Step 1, at 75 DEG C chelating agent (1,3-PD) is put into container, regulation pH is 7, and control rotating speed is in 2400r/
Min uniform stirrings, back flow reaction 1.5h are preheated.
Step 2, it is passed through protective gas N2, and temperature is warming up to 100 DEG C, it is slowly added to titanium ion (tetra isopropyl metatitanic acid
Ester), control rotating speed back flow reaction 5h, then adds acrylic acid in 2800rpm uniform stirrings, continues back flow reaction 5h, stops stirring
Mix, stand 3h, be cooled to room temperature and be transferred in beaker, produce titanate coupling agent.
Chelating agent, titanium ion, the mol ratio of acrylic acid are 2: 1: 2.
Embodiment 6
A kind of preparation method of water-soluble titanate coupling agent, is comprised the following steps that：
Step 1, at 60 DEG C chelating agent (1,3-PD) is put into container, regulation pH is 6.5, and control rotating speed exists
2690r/min uniform stirrings, 0.5~2h of back flow reaction are preheated.
Step 2, it is passed through protective gas N2, and temperature is warming up to 85 DEG C, it is slowly added to titanium ion (tetra isopropyl metatitanic acid
Ester), control rotating speed back flow reaction 3h, then adds acrylic acid in 2300rpm uniform stirrings, continues back flow reaction 4h, stops stirring
Mix, stand 2h, be cooled to room temperature and be transferred in beaker, produce titanate coupling agent.
Chelating agent, titanium ion, the mol ratio of acrylic acid are 1: 1: 2.
Stability test is hydrolyzed in the water-soluble titanate coupling agent that embodiment 1~6 is prepared.
Above-mentioned titanate coupling agent hydrolytic stability test, it is as a result as shown in the table：
Although embodiment of the present invention is disclosed as above, it is not restricted in specification and embodiment listed
With it can be applied to various suitable the field of the invention completely, can be easily for those skilled in the art
Other modification is realized, therefore under the universal limited without departing substantially from claim and equivalency range, it is of the invention and unlimited
In specific details.
Claims (4)
1. a kind of water-soluble titanate coupling agent, it is characterised in that there is following chemical formula：
Wherein ,-OR1CH(R2) O- is chelation group, it is from ethylene glycol, 1,3-PD, glycerine, 1,2- butanediols, breast
Any of acid, ethanedioic acid, glycine.
2. a kind of preparation method of water-soluble titanate coupling agent as claimed in claim 1, it is characterised in that including following step
Suddenly：
Step 1：Chelating agent is put into reaction vessel at 60-80 DEG C, pH is between 6.5-7.5 for regulation, and control rotating speed exists
1000-3000rpm, stirring, 0.5-2h is flowed back to be preheated；
Step 2：Nitrogen is passed through to reaction vessel, and temperature is risen to 80-100 DEG C, adds titanium ion, control rotating speed is in 1000-
3000rpm, stirring, back flow reaction 3-5h, acrylic acid is then added, continues back flow reaction 3-5h, stop stirring, stand 1-5h,
Room temperature is cooled to, produces water-soluble titanate coupling agent.
3. the preparation method of water-soluble titanate coupling agent as claimed in claim 2, it is characterised in that the acrylic acid and titanium
The mol ratio of ion is 2: 1.
4. the preparation method of water-soluble titanate coupling agent according to claim 2, it is characterised in that the chelating agent with
The mol ratio of titanium ion is 1-2: 1.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108276767A (en) * | 2018-04-03 | 2018-07-13 | 芜湖超科机电设备有限公司 | A kind of fibre reinforced PA materials for common aero vehicle wing |
| CN113337003A (en) * | 2021-07-05 | 2021-09-03 | 扬州市立达树脂有限公司 | Chelate titanate coupling agent and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4087402A (en) * | 1975-09-30 | 1978-05-02 | Kenrich Petrochemicals, Inc. | Organo-titanate chelates and their uses |
-
2017
- 2017-08-18 CN CN201710712047.4A patent/CN107602607A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4087402A (en) * | 1975-09-30 | 1978-05-02 | Kenrich Petrochemicals, Inc. | Organo-titanate chelates and their uses |
Non-Patent Citations (1)
| Title |
|---|
| 金正中等: "乳酸型钛酸酯偶联剂的合成和应用", 《高等学校化学学报》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108276767A (en) * | 2018-04-03 | 2018-07-13 | 芜湖超科机电设备有限公司 | A kind of fibre reinforced PA materials for common aero vehicle wing |
| CN113337003A (en) * | 2021-07-05 | 2021-09-03 | 扬州市立达树脂有限公司 | Chelate titanate coupling agent and preparation method thereof |
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