CN108276281A - A kind of continuous producing apparatus of isobornyl methacrylate - Google Patents
A kind of continuous producing apparatus of isobornyl methacrylate Download PDFInfo
- Publication number
- CN108276281A CN108276281A CN201810058379.XA CN201810058379A CN108276281A CN 108276281 A CN108276281 A CN 108276281A CN 201810058379 A CN201810058379 A CN 201810058379A CN 108276281 A CN108276281 A CN 108276281A
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- CN
- China
- Prior art keywords
- kettle
- isobornyl methacrylate
- semi
- finished product
- amphene
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/04—Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides onto unsaturated carbon-to-carbon bonds
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
- C07C67/52—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
- C07C67/54—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of continuous producing apparatus of isobornyl methacrylate, including reaction kettle, secondary response kettle, intermediate maturity tank, short-path distillation kettle, washing kettle and finished pot, methacrylic acid, amphene, catalyst and polymerization inhibitor respectively enter reaction kettle, it is reacted in reaction kettle, obtained semi-finished product enter intermediate maturity tank；Semi-finished product are delivered to progress short distance rectifying in short-path distillation kettle from intermediate finished pot, obtain isobornyl methacrylate and unreacted methacrylic acid and amphene；Isobornyl methacrylate enters washing kettle and washes off acid solution, subsequently into finished pot；Unreacted methacrylic acid and amphene enter secondary response kettle, are reacted in secondary response kettle, and obtained semi-finished product are again introduced into intermediate maturity tank.The advantage of the invention is that：With the high advantage of raw material availability, and the loss of raw material is reduced, improve the conversion ratio of raw material, realizes continuous production.
Description
Technical field
The present invention relates to organic compound production equipment technologies, are more particularly to a kind of isobornyl methacrylate
Continuous producing apparatus.
Background technology
Isobornyl methacrylate category special esters of methacrylic acid has carbon-carbon double bond and special isobornyl thiocyanoacetate alkane
Oxygroup, than the T value highers of acrylic acid hydroxy alkyl ester, polymer that can be excellent with many other monomer polymerization forming properties, also because
Its refractive index is big, can be used as optical resin.
It is isoborneol route that isobornyl methacrylate, which synthesizes main route,.Isoborneol route is using isoborneol as raw material
Including direct esterification and ester-interchange method.Due to the shortcomings of borneol and isoborneol price are high, source is few, while there is by-product H2O
Or methanol generates, and on the one hand leads to the reduction of atom utility value, in addition, the release environmental pollution of methanol is larger, and water
Generation can make moisture in product higher.Currently, for realizing industrial production isobornyl methacrylate, existing device
There are high energy consumption, it is seriously polluted, cannot achieve the problems such as continuous production.
Invention content
Technical problem to be solved by the present invention lies in provide a kind of company of free of contamination isobornyl methacrylate
Continuous production equipment.
The present invention is to solve above-mentioned technical problem by the following technical programs：
A kind of continuous producing apparatus of isobornyl methacrylate, including reaction kettle, secondary response kettle, intermediate maturity
Tank, short-path distillation kettle, washing kettle and finished pot, methacrylic acid, amphene, catalyst and polymerization inhibitor respectively enter reaction kettle,
It is reacted in reaction kettle, obtained semi-finished product enter intermediate maturity tank；Semi-finished product are delivered to short-path distillation kettle from intermediate finished pot
Middle progress short distance rectifying obtains isobornyl methacrylate and unreacted methacrylic acid and amphene；Methacrylic acid
Isobornyl thiocyanoacetate enters washing kettle and washes off acid solution, subsequently into finished pot；Unreacted methacrylic acid and amphene enter secondary counter
Kettle is answered, is reacted in secondary response kettle, obtained semi-finished product are again introduced into intermediate maturity tank.
Preferably, semi-finished product enter intermediate maturity tank after filtration treatment recycles catalyst.
Preferably, polymerization inhibitor is added into intermediate maturity tank, to prevent from reacting in intermediate maturity tank.
Preferably, semi-finished product are delivered to progress short distance rectifying in short-path distillation kettle by pumping from intermediate finished pot.
Preferably, semi-finished product are delivered to progress short distance rectifying in short-path distillation kettle by pumping from intermediate finished pot.
Preferably, reaction kettle and secondary response kettle are stirring-type reaction kettle.
Preferably, stirring-type reaction kettle includes semi-circular tube reaction kettle or jacket reactor.
The method that isobornyl methacrylate is prepared using the continuous producing apparatus of above-mentioned isobornyl methacrylate,
Include the following steps：So that methacrylic acid and amphene is entered reaction kettle, dissolve at room temperature, catalyst is added until completely dissolved
And polymerization inhibitor, it is reacted in reaction kettle, obtained semi-finished product enter intermediate maturity tank；Semi-finished product are delivered to from intermediate finished pot
Short distance rectifying is carried out in short-path distillation kettle, obtains isobornyl methacrylate and unreacted methacrylic acid and amphene；
Isobornyl methacrylate enters washing kettle and washes off acid solution, subsequently into finished pot；Unreacted methacrylic acid and amphene
It into secondary response kettle, is reacted in secondary response kettle, obtained semi-finished product are again introduced into intermediate maturity tank.
Preferably, reaction temperature is 50~70 DEG C.
Preferably, semi-finished product enter intermediate maturity tank after filtration treatment recycles catalyst.
Preferably, polymerization inhibitor is added into intermediate maturity tank.
The present invention has the following advantages compared with prior art：The reaction temperature of the production equipment of the present invention is low, and side reaction subtracts
It is few, the loss of raw material is reduced, the conversion ratio of raw material is improved, so that product quality has obtained further being promoted；And
And entire production link all carries out in closed environment, is generated without exhaust gas, waste water, by-product, does not have any dirt to environment
Dye.
Description of the drawings
Fig. 1 is the continuous producing apparatus figure of the isobornyl methacrylate of the application.
Specific implementation mode
It elaborates below to the embodiment of the present invention, the present embodiment is carried out lower based on the technical solution of the present invention
Implement, gives detailed embodiment and specific operating process, but protection scope of the present invention is not limited to following implementation
Example.
Embodiment 1
As shown in Figure 1, a certain amount of methacrylic acid and refined amphene are put into reaction kettle, dissolves, waited at room temperature
A certain amount of polymerization inhibitor and catalyst are added after fully dissolved, is heated up to 60 degrees Celsius of reactions, does not release heat in reaction process, instead
Reaction should be stopped, catalyst is recovered by filtration and obtains semi-finished product, semi-finished product enter intermediate maturity tank after a certain period of time.To semi-finished product tank
In add a certain amount of polymerization inhibitor, semi-finished product are pumped into short-path distillation kettle and steam unreacted amphene at negative pressure 0.01MPa
With excessive methacrylic acid；Fraction when collecting 113~120 DEG C at 0.6kPa, as isobornyl methacrylate
(IBOMA), obtained isobornyl methacrylate is then washed off into the acid solution in product by washing kettle water, controls product acid
Degree can be pumped to finished pot 0.05, subsequently into bagging area.And unreacted amphene and excessive methacrylic acid then into
Enter secondary response kettle, is reacted in secondary response kettle to recycle reaction raw materials, obtained semi-finished product are again introduced into centre
Then finished pot sequentially enters short-path distillation kettle, washing kettle and finished pot, making short-path distillation and washing, cycle carries out successively, with
High level finished product is made, realizes continuous production.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
All any modification, equivalent and improvement etc., should all be included in the protection scope of the present invention made by within refreshing and principle.
Claims (10)
1. a kind of continuous producing apparatus of isobornyl methacrylate, which is characterized in that including reaction kettle, secondary response kettle,
Intermediate maturity tank, short-path distillation kettle, washing kettle and finished pot, methacrylic acid, amphene, catalyst and polymerization inhibitor respectively enter instead
Kettle is answered, is reacted in reaction kettle, obtained semi-finished product enter intermediate maturity tank；Semi-finished product are delivered to short distance from intermediate finished pot
Short distance rectifying is carried out in distillation still, obtains isobornyl methacrylate and unreacted methacrylic acid and amphene；Methyl
Isobornyl acrylate enters washing kettle and washes off acid solution, subsequently into finished pot；Unreacted methacrylic acid and amphene enter
Secondary response kettle is reacted in secondary response kettle, and obtained semi-finished product are again introduced into intermediate maturity tank.
2. the continuous producing apparatus of isobornyl methacrylate according to claim 1, which is characterized in that semi-finished product pass through
Filtration treatment enters intermediate maturity tank after recycling catalyst.
3. the continuous producing apparatus of isobornyl methacrylate according to claim 2, which is characterized in that centre at
Polymerization inhibitor is added in product tank.
4. the continuous producing apparatus of isobornyl methacrylate according to claim 1, which is characterized in that semi-finished product by
Pump is delivered to progress short distance rectifying in short-path distillation kettle from intermediate finished pot.
5. the continuous producing apparatus of isobornyl methacrylate according to claim 1, which is characterized in that the reaction
Kettle and secondary response kettle are stirring-type reaction kettle.
6. the continuous producing apparatus of isobornyl methacrylate according to claim 5, which is characterized in that the stirring
Formula reaction kettle includes semi-circular tube reaction kettle or jacket reactor.
7. prepared by a kind of continuous producing apparatus using isobornyl methacrylate according to any one of claims 1 to 6
The method of isobornyl methacrylate, which is characterized in that include the following steps：Methacrylic acid and amphene is set to enter reaction
Kettle dissolves at room temperature, and catalyst and polymerization inhibitor are added until completely dissolved, is reacted in reaction kettle, and semi-finished product are made
Into intermediate maturity tank；Semi-finished product are delivered to progress short distance rectifying in short-path distillation kettle from intermediate finished pot, obtain metering system
Sour isobornyl thiocyanoacetate and unreacted methacrylic acid and amphene；Isobornyl methacrylate enters washing kettle and washes off acid solution,
Subsequently into finished pot；Unreacted methacrylic acid and amphene enter secondary response kettle, are reacted in secondary response kettle,
Obtained semi-finished product are again introduced into intermediate maturity tank.
8. the method according to claim 7 for preparing isobornyl methacrylate, which is characterized in that reaction temperature 50
~70 DEG C.
9. the method according to claim 7 for preparing isobornyl methacrylate, which is characterized in that semi-finished product are through filtering
Enter intermediate maturity tank after processing recycling catalyst.
10. the method according to claim 7 for preparing isobornyl methacrylate, which is characterized in that intermediate maturity
Polymerization inhibitor is added in tank.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810058379.XA CN108276281A (en) | 2018-01-22 | 2018-01-22 | A kind of continuous producing apparatus of isobornyl methacrylate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810058379.XA CN108276281A (en) | 2018-01-22 | 2018-01-22 | A kind of continuous producing apparatus of isobornyl methacrylate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108276281A true CN108276281A (en) | 2018-07-13 |
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ID=62804419
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810058379.XA Pending CN108276281A (en) | 2018-01-22 | 2018-01-22 | A kind of continuous producing apparatus of isobornyl methacrylate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108276281A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114805061A (en) * | 2022-05-25 | 2022-07-29 | 佛山市三水精泽化工有限公司 | Process for producing isobornyl methacrylate and isobornyl methacrylate |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101863763A (en) * | 2010-06-04 | 2010-10-20 | 南京林业大学 | Catalytic synthesis method of isobornyl methacrylate supported by activated carbon |
-
2018
- 2018-01-22 CN CN201810058379.XA patent/CN108276281A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101863763A (en) * | 2010-06-04 | 2010-10-20 | 南京林业大学 | Catalytic synthesis method of isobornyl methacrylate supported by activated carbon |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114805061A (en) * | 2022-05-25 | 2022-07-29 | 佛山市三水精泽化工有限公司 | Process for producing isobornyl methacrylate and isobornyl methacrylate |
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| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20180713 |