CN108250063A - A kind of isooctyl acid titanium preparation method - Google Patents
A kind of isooctyl acid titanium preparation method Download PDFInfo
- Publication number
- CN108250063A CN108250063A CN201810144493.4A CN201810144493A CN108250063A CN 108250063 A CN108250063 A CN 108250063A CN 201810144493 A CN201810144493 A CN 201810144493A CN 108250063 A CN108250063 A CN 108250063A
- Authority
- CN
- China
- Prior art keywords
- reaction kettle
- dry gas
- preparation
- butanol
- isooctyl acid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/41—Preparation of salts of carboxylic acids
- C07C51/412—Preparation of salts of carboxylic acids by conversion of the acids, their salts, esters or anhydrides with the same carboxylic acid part
Abstract
The present invention provides a kind of isooctyl acid titanium preparation method, including：Step S1：Butyl titanate is put into reaction kettle；After feeding intake, dry gas is passed through in reaction kettle；Reaction kettle is equipped with air inlet and exhaust outlet, and dry gas enters reaction kettle from air inlet, reaction kettle is left from exhaust outlet；Step S2：Under normal pressure, reaction kettle is directly heated 110-120 DEG C；Then isooctyl acid is added dropwise in reaction kettle, isooctyl acid reacts with butyl titanate, generates isooctyl acid titanium and butanol；Step S3：Byproduct of reaction butanol gasifies at high temperature, and under the extruding of dry gas, reaction kettle is left from exhaust outlet；Step S4：Gaseous state butanol, by liquefying after condenser, enters receiver with dry gas by connecting line；When not having liquid butanol to enter receiver, reaction terminates.The present invention can prevent raw material hydrolysis and side reaction from occurring；The butanol in isooctyl acid titanium is dispelled simultaneously, prevents its etching apparatus during subsequent working process.
Description
Technical field
The present invention relates to a kind of isooctyl acid titanium preparation methods.
Background technology
The preparation of isooctyl acid titanium needs to use butyl titanate as raw material, butyl titanate exposure in air when easily
Hydrolysis, so as to influence the water resistance of isooctyl acid titanium；In addition, with isooctyl acid esterification can occur for byproduct of reaction butanol, from
And influence product quality.
Currently used preparation method is：By butyl titanate and isooctyl acid input reactor, and vacuumize；Treat vacuum degree
After stabilization, 50 degree are to slowly warm up to, is evaporated under reduced pressure 0.5 hour；It is warming up to 70 degree again, is evaporated under reduced pressure 0.5 hour；Finally it is warming up to
It 90 degree, is evaporated under reduced pressure 0.5 hour, reaction terminates.
The defects of aforesaid way, is：Vacuum distillation can be pumped into the vapor in air in kettle, cause butyl titanate
Hydrolysis, so as to influence product quality；In addition, esterification, while four fourth of metatitanic acid can occur with isooctyl acid for byproduct of reaction butanol
Ester can be used as catalyst for esterification reaction, accelerate esterification, can also influence product quality.
Therefore, how providing one kind can prevent raw material from hydrolyzing, and preventing the preparation method that side reaction occurs from becoming industry needs
It solves the problems, such as.
Invention content
In view of the shortcomings of the prior art, the object of the present invention is to provide a kind of isooctyl acid titanium preparation method, original can be prevented
Material hydrolysis, prevents side reaction.
To achieve these goals, the present invention provides a kind of isooctyl acid titanium preparation method, preparation method includes：
Step S1：Butyl titanate is put into reaction kettle；After feeding intake, dry gas is passed through in reaction kettle；Instead
Kettle is answered to be equipped with air inlet and exhaust outlet, dry gas enters reaction kettle from air inlet, reaction kettle is left from exhaust outlet；
Step S2：Under normal pressure, reaction kettle is directly heated 110-120 DEG C；Then it is added dropwise in reaction kettle different pungent
Acid, isooctyl acid react with butyl titanate, generate isooctyl acid titanium and butanol；
Step S3：Byproduct of reaction butanol gasifies at high temperature, and under the extruding of dry gas, reaction is left from exhaust outlet
Kettle；
Step S4：Gaseous state butanol, by liquefying after condenser, enters receiver with dry gas by connecting line；When not having
When having the liquid butanol to enter receiver, reaction terminates.
In the present invention, isooctyl acid titanium is oily liquids, is stored in reactor bottom.
In the present invention, in reaction kettle in dry gas atmosphere.
In the present invention, liquid butanol is stored in receiver bottom.
In the present invention, it need to ensure not containing butanol in the isooctyl acid titanium finally obtained, otherwise butanol can be after isooctyl acid titanium
Corrode plastic components during continuous working process, cause damages.
In the present invention, tetrabutyl titanate hydrolysis can be prevented using dry gas.
In the present invention, with isooctyl acid esterification can occur for butanol, while butyl titanate can be used as esterification catalytic
Agent；Butanol gasifies under high temperature, can not be deposited in reaction kettle, can prevent side reaction.
The present invention can prevent raw material hydrolysis and side reaction from occurring in isooctyl acid titanium preparation process；Dispel isooctyl acid simultaneously
Butanol in titanium prevents its etching apparatus during subsequent working process.
According to another specific embodiment of the present invention, in whole preparation process, dry gas is in circulation status always.
According to another specific embodiment of the present invention, in step S1, the inventory of butyl titanate is 60-70g.
According to another specific embodiment of the present invention, in step S2, the inventory of isooctyl acid is 110-120g.
According to another specific embodiment of the present invention, dry gas is dry air.
According to another specific embodiment of the present invention, dry gas is dry inert gas.
According to another specific embodiment of the present invention, in step S4, after dry gas is by condenser, pass through connecting line
Receiver is left into receiver, and from the bleeding point on receiver.
According to another specific embodiment of the present invention, vacuum pump is connected with outside bleeding point, by vacuum pumping, is generated negative
Pressure accelerates dry gas flowing, improves efficiency.
According to another specific embodiment of the present invention, reactor bottom is equipped with material taking mouth；After reaction, isooctyl acid titanium from
Material taking mouth is discharged.
According to another specific embodiment of the present invention, dry gas enters reaction kettle by air pump.
Compared with prior art, the present invention has following advantageous effect：
The present invention can prevent raw material hydrolysis and side reaction from occurring in isooctyl acid titanium preparation process；Dispel isooctyl acid simultaneously
Butanol in titanium prevents its etching apparatus during subsequent working process.
Specific embodiment
Embodiment 1
A kind of isooctyl acid titanium preparation method is present embodiments provided, including：
Step S1：65g butyl titanates are put into reaction kettle；After feeding intake, dry gas is passed through in reaction kettle；
Dry gas enters reaction kettle by air pump；Reaction kettle is equipped with air inlet and exhaust outlet, and dry gas enters anti-from air inlet
Kettle is answered, reaction kettle is left from exhaust outlet；In reaction kettle in dry gas atmosphere；Dry gas is dry air.
Step S2：Under normal pressure, reaction kettle is directly heated to 115 DEG C；Then 115g isooctyl acids are added dropwise in reaction kettle,
Isooctyl acid reacts with butyl titanate, generates isooctyl acid titanium and butanol.
Step S3：Byproduct of reaction butanol gasifies at high temperature, and under the extruding of dry gas, reaction is left from exhaust outlet
Kettle.
Step S4：Gaseous state butanol, by liquefying after condenser, enters receiver, liquid with dry gas by connecting line
Butanol is stored in receiver bottom；When not having liquid butanol to enter receiver, reaction terminates.
After dry gas is by condenser, receiver is entered, and leave from the bleeding point on receiver by connecting line
Receiver；Vacuum pump is connected with outside bleeding point.
Reactor bottom is equipped with material taking mouth；After reaction, isooctyl acid titanium is discharged from material taking mouth.
In whole preparation process, dry gas is in circulation status always.
Embodiment 2
The present embodiment and embodiment 1 difference lies in：Dry gas is dry argon gas.
Although the present invention is disclosed above with preferred embodiment, it is not limited to the range that the present invention is implemented.Any
The those of ordinary skill in field in the invention scope for not departing from the present invention, improves when can make a little, i.e., every according to this hair
Bright done equal improvement, should be the scope of the present invention and is covered.
Claims (10)
1. a kind of isooctyl acid titanium preparation method, wherein, the preparation method includes：
Step S1：Butyl titanate is put into reaction kettle；After feeding intake, dry gas is passed through in reaction kettle；Reaction kettle
Air inlet and exhaust outlet are equipped with, dry gas enters reaction kettle from air inlet, reaction kettle is left from exhaust outlet；
Step S2：Under normal pressure, reaction kettle is directly heated 110-120 DEG C；Then isooctyl acid is added dropwise in reaction kettle, it is different
Octanoic acid reacts with butyl titanate, generates isooctyl acid titanium and butanol；
Step S3：Byproduct of reaction butanol gasifies at high temperature, and under the extruding of dry gas, reaction kettle is left from exhaust outlet；
Step S4：Gaseous state butanol, by liquefying after condenser, enters receiver with dry gas by connecting line；When there is no liquid
When state butanol enters receiver, reaction terminates.
2. preparation method as described in claim 1, wherein, in whole preparation process, dry gas is in circulation status always.
3. preparation method as described in claim 1, wherein, in the step S1, the inventory of butyl titanate is 60-
70g。
4. preparation method as described in claim 1, wherein, in the step S2, the inventory of isooctyl acid is 110-120g.
5. preparation method as described in claim 1, wherein, the dry gas is dry air.
6. preparation method as described in claim 1, wherein, the dry gas is dry inert gas.
7. preparation method as described in claim 1, wherein, in the step S4, after dry gas is by condenser, pass through company
It takes over road and enters receiver, and receiver is left from the bleeding point on receiver.
8. preparation method as claimed in claim 7, wherein, it is connected with vacuum pump outside the bleeding point.
9. preparation method as described in claim 1, wherein, the reactor bottom is equipped with material taking mouth；After reaction, it is different pungent
Sour titanium is discharged from material taking mouth.
10. preparation method as described in claim 1, wherein, dry gas enters reaction kettle by air pump.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810144493.4A CN108250063A (en) | 2018-02-11 | 2018-02-11 | A kind of isooctyl acid titanium preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810144493.4A CN108250063A (en) | 2018-02-11 | 2018-02-11 | A kind of isooctyl acid titanium preparation method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108250063A true CN108250063A (en) | 2018-07-06 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201810144493.4A Pending CN108250063A (en) | 2018-02-11 | 2018-02-11 | A kind of isooctyl acid titanium preparation method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109734744A (en) * | 2018-12-26 | 2019-05-10 | 佛山市天宇安贝尔新材料有限公司 | A kind of preparation method of 2- base caproic acid titanium |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB395406A (en) * | 1931-01-16 | 1933-07-17 | Titanium Pigment Co Inc | Improvements in or relating to the manufacture of metallic soaps |
| US4720352A (en) * | 1985-11-01 | 1988-01-19 | Nuodex Inc. | Process for the preparation of vanadium-containing mixed metal soap solutions |
| CN1178795A (en) * | 1996-08-22 | 1998-04-15 | 埃勒夫阿托化学有限公司 | Unsaturated metal-organic compound derived from titanium and its preparing method |
| CN105541600A (en) * | 2014-10-28 | 2016-05-04 | 日油株式会社 | A method of producing fatty acid titanium |
-
2018
- 2018-02-11 CN CN201810144493.4A patent/CN108250063A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB395406A (en) * | 1931-01-16 | 1933-07-17 | Titanium Pigment Co Inc | Improvements in or relating to the manufacture of metallic soaps |
| US4720352A (en) * | 1985-11-01 | 1988-01-19 | Nuodex Inc. | Process for the preparation of vanadium-containing mixed metal soap solutions |
| CN1178795A (en) * | 1996-08-22 | 1998-04-15 | 埃勒夫阿托化学有限公司 | Unsaturated metal-organic compound derived from titanium and its preparing method |
| CN105541600A (en) * | 2014-10-28 | 2016-05-04 | 日油株式会社 | A method of producing fatty acid titanium |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109734744A (en) * | 2018-12-26 | 2019-05-10 | 佛山市天宇安贝尔新材料有限公司 | A kind of preparation method of 2- base caproic acid titanium |
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| PB01 | Publication | ||
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| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20180706 |
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| RJ01 | Rejection of invention patent application after publication |