CN211487670U - Device for preparing pivalic acid - Google Patents
Device for preparing pivalic acid Download PDFInfo
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- CN211487670U CN211487670U CN201922288490.0U CN201922288490U CN211487670U CN 211487670 U CN211487670 U CN 211487670U CN 201922288490 U CN201922288490 U CN 201922288490U CN 211487670 U CN211487670 U CN 211487670U
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Abstract
The utility model belongs to the technical field of the chemical industry, concretely relates to device of preparation pivalic acid, including the high-pressure reaction cauldron body, high-pressure reaction cauldron body top is provided with mixes feedstock line, CO air inlet line and carbonylation material discharging pipeline, mixes feedstock line, and carbonylation material discharging pipeline all stretch into the inside of the high-pressure reaction cauldron body, and the external side cladding of high-pressure reaction cauldron has the cauldron overcoat cover, and the internal portion of high-pressure reaction cauldron is provided with agitator and cauldron internal coil pipe, and agitator upper portion is provided with first stirring rake, and the agitator bottom is provided with the second stirring rake, is provided with the solid acid coating on the internal wall of high-pressure reaction cauldron. The utility model discloses can use solid acid catalysis to replace concentrated sulfuric acid catalysis preparation pivalic acid, reduce the corruption of reaction process to equipment, stop the production of a large amount of by-product concentrated sulfuric acid, reduction in production cost reduces environmental pollution.
Description
Technical Field
The utility model belongs to the technical field of the chemical industry, concretely relates to device of preparation pivalic acid.
Background
Pivalic acid (trimethylacetic acid and 2, 2-dimethylpropionic acid) shows special physical and chemical properties due to the fact that a carbonyl functional group is connected to a tertiary carbon atom, is an important chemical product, is widely used as an intermediate of pesticides, medicines and dyes, and has application in the fields of high-grade coatings, polymerization initiators, photosensitive materials, spices, lubricating oil, pivaloyl chloride, high polymer material synthesis, spices, adhesives and the like.
Chinese patent CN 1778788A discloses a process for producing pivalic acid, which comprises mixing butadiene-free C-IV fraction with sulfuric acid in a reactor, esterifying at a certain temperature and pressure, removing the raffinate containing little isobutene in the upper layer, carbonylating the lower layer with carbon monoxide, hydrolyzing, and separating.
Chinese patent CN 106187735A discloses a method for synthesizing pivalic acid and 2,2,4, 4-tetramethylvaleric acid by diisobutylene carbonyl, which adopts a carbonyl synthesis method and comprises the following steps: A. carbonylation reaction: diisobutylene, carbon monoxide and water are used as raw materials, 65-80% sulfuric acid aqueous solution is used as a catalyst, and the mixture of pivalic acid sulfonate and 2,2,4, 4-tetramethyl valeric acid sulfonate is obtained by pressurizing and reacting at the temperature of 20-30 ℃; B. hydrolysis: and D, hydrolyzing the mixture of the pivalic acid sulfonate and the 2,2,4, 4-tetramethyl valeric acid sulfonate obtained in the step A at the temperature of 5-10 ℃, standing for layering, extracting and concentrating the water phase, recycling, and rectifying the organic phase to obtain pivalic acid and 2,2,4, 4-tetramethyl valeric acid.
It can be known from the above patents that the existing pivalic acid production process falls behind, the Koch carbonylation method is mainly adopted for producing pivalic acid at home and abroad, but concentrated sulfuric acid is mostly used as a catalyst in the reaction, so that not only is the apparatus greatly corroded, but also the environment is greatly polluted, the production cost is high, the market price of pivalic acid is continuously increased, and the research on synthesis of pivalic acid by using solid acid as a catalyst is increasingly active.
At present, it is needed to provide a device for preparing pivalic acid by using a solid acid catalyst instead of the existing concentrated sulfuric acid catalyst, so as to solve the above problems.
SUMMERY OF THE UTILITY MODEL
The utility model aims at providing a device of preparation pivalic acid uses solid acid catalysis to replace concentrated sulfuric acid catalysis preparation pivalic acid, reduces the corruption of reaction process to equipment, stops the production of a large amount of by-product concentrated sulfuric acid, reduction in production cost reduces environmental pollution.
Preparation pivalic acid's device, including the high pressure batch autoclave cauldron body, high pressure batch autoclave cauldron body top is provided with mixes feedstock line, CO air inlet line and carbonylation material discharging pipeline, mixes feedstock line, all stretches into the inside of the high pressure batch autoclave cauldron body with carbonylation material discharging pipeline, the external side cladding of high pressure batch autoclave cauldron has the cauldron jacket, the internal portion of high pressure batch autoclave cauldron is provided with agitator and cauldron inner coil pipe, agitator upper portion is provided with first stirring rake, the agitator bottom is provided with the second stirring rake, be provided with the solid acid coating on the internal wall of high pressure batch autoclave cauldron.
The mixing feed line in the high-pressure reaction kettle body is inclined downwards, and the pipe orifice of the mixing feed line faces to the first stirring paddle.
The downward inclination angle is 43-48 degrees.
The mixed feeding pipeline is respectively connected with an isobutene feeding pipeline and a water feeding pipeline.
The carbonylation material discharge pipeline extends into the bottom of the high-pressure reaction kettle body.
The first stirring paddle is provided with a solid acid coating.
The solid acid coating is arranged at the position 60-90% of the height of the inner wall of the high-pressure reaction kettle body.
The heat-conducting medium inlet pipeline is respectively connected with the kettle outer jacket and the kettle inner coil.
And the heat-conducting medium outlet pipeline is respectively connected with the kettle outer jacket and the kettle inner coil.
And a pressure gauge is arranged at the top of the high-pressure reaction kettle body.
And a thermometer is arranged at the top of the high-pressure reaction kettle body.
The high-pressure reaction kettle is flat.
The method for preparing the pivalic acid by adopting the device of the utility model is characterized in that CO is introduced into the high-pressure reaction kettle body to carry out air replacement and pressurization, the stirrer is arranged inside the high-pressure reaction kettle body, the first stirring paddle is arranged on the upper part of the stirrer, the second stirring paddle is arranged at the bottom of the stirrer, isobutene and water are mixed and then sprayed on the first stirring paddle in the high-pressure reaction kettle body, the heating stirring reaction is carried out, the carbonylation material is obtained, the standing layering is carried out, and the pivalic acid crude product at the upper layer is taken to be rectified to obtain the pivalic acid finished product; solid acid coatings are arranged on the inner wall of the high-pressure reaction kettle body and the first stirring paddle.
The fixingThe body acid coating is SO4 2-/ZrO2-V2O3Coating or SO4 2-/ZrO2-Co2O3And (4) coating.
The thickness of the solid acid coating is 5-10 mm.
The pressurizing pressure is 5.5-6.5 MPa.
The mass ratio of the isobutene to the water is 100: 25-40.
The reaction temperature is 140-150 ℃.
The stirring speed is 300-800 r/min; the stirring mode is that the stirring speed is controlled to be 300r/min in the feeding process, and is increased to 800r/min after the feeding is finished.
The rectification is vacuum rectification, the vacuum degree of the vacuum rectification is-0.095-0.099 Mpa, and the temperature of the vacuum rectification is 78-82 ℃.
The inner wall of the high-pressure reaction kettle and the first stirring paddle of the utility model are both loaded with the composite solid acid catalyst, which ensures that the reaction is mainly concentrated at the three-phase contact position, improves the conversion rate of isobutene and the selectivity of pivalic acid, and reduces the generation of isovaleric acid and isobutene polymer; the high-pressure reaction kettle is flat, the liquid level area in the kettle is increased by the flat shape, and the contact area of three phases of air, liquid and solid is indirectly increased; the isobutene feeding pipeline is directly sprayed on the first stirring paddle at a certain angle, so that the contact area of the gas, the liquid and the solid phases is increased; the temperature control system is jointly controlled by the coil pipe in the kettle and the jacket outside the kettle, so that the heating and cooling efficiency is improved; the positions of the inner wall of the kettle and the solid acid catalyst loaded on the stirring paddle are fixed, so that the conversion rate of isobutene and the selectivity of pivalic acid are enhanced, and the production of byproducts is reduced.
The temperature control of the high-pressure reaction kettle adopts the combined action of a coil pipe in the kettle and a jacket outside the kettle.
Isobutene and water are mixed in a mixing feed pipeline according to a certain proportion and then enter a high-pressure reaction kettle.
The mixing feed line sprays the material directly onto the first paddle at an angle of 43-48 °.
The first paddle is attached with a solid acid coating and the second paddle is not.
The liquid level is controlled at the position of about 80 percent of the height of the inner wall, the first stirring paddle is semi-immersed, and the liquid level is kept in a flying state in the reaction process.
The second stirring paddle adopts a propelling type, so that liquid is stirred and fully mixed conveniently, and the stability of materials on the upper layer and the lower layer is kept; the rotating speed of the stirring paddle is controlled to be 300r/min in the feeding process, and the rotating speed is increased to 800r/min after the feeding is finished. The reason that the liquid level in the initial kettle is low in the early-stage rotating speed is that the motor is damaged when the motor idles at a too high rotating speed, and the influence on the conversion rate and the selectivity is large when the later-stage rotating speed is increased to 800 r/min.
Adopt the method of device preparation pivalic acid specifically be at first utilize CO to carry out the cauldron air displacement and pressurize to certain pressure, later add mixed feed line with isobutene and water according to a certain proportion and mix, reentry high-pressure batch autoclave, the stirring in-process intensifies gradually, final liquid level is maintained about 80%, first stirring rake is half to soak below the liquid level, temperature control reacts about 145 ℃ in the cauldron, follow carbonylation material discharge pipeline sample detection behind the certain time, the isobutene conversion reaches the ejection of compact layering that stews more than 88%, take upper strata pivalic acid crude product to get into rectification system, make the pivalic acid finished product, it gets back to synthetic workshop section cyclic utilization to divide the aqueous phase.
The conversion rate of isobutene is about 90%, and the selectivity of pivalic acid is about 60%.
The operation steps of the device for preparing the pivalic acid of the utility model are that after the air tightness of the device is detected to be normal, CO is added into the high-pressure reaction kettle body through a CO air inlet pipeline to carry out air replacement and pressurization, after the pressure gauge displays that the set pressure is reached, a stirrer in the high-pressure reaction kettle body is set to a certain rotating speed to start stirring, meanwhile, steam enters the kettle outer jacket and the kettle inner coil pipe through a heat-conducting medium inlet pipeline to heat the high-pressure reaction kettle, and the steam is discharged from a heat-conducting medium outlet pipeline; isobutene enters a mixed feeding pipeline through an isobutene feeding pipeline, water enters the mixed feeding pipeline through a water feeding pipeline, isobutene and water are mixed in the mixed feeding pipeline and then enter a high-pressure reaction kettle body, a thermometer displays that the set temperature is reached, the rotating speed is increased to the set rotating speed to perform reaction to obtain a carbonylation material, the carbonylation material enters a separation tank through a carbonylation material discharging pipeline to perform standing and layering after being sampled and detected to be qualified, and an upper-layer organic-phase pivalic acid crude product is taken to perform reduced pressure rectification to obtain a pivalic acid finished product.
The utility model has the advantages as follows:
the utility model discloses can use solid acid catalysis to replace concentrated sulfuric acid catalysis preparation pivalic acid, reduce the corruption of reaction process to equipment, stop the production of a large amount of by-product concentrated sulfuric acid, reduction in production cost reduces environmental pollution.
Drawings
Fig. 1 is a schematic structural diagram of the present invention;
in the figure: 1. a high-pressure reaction kettle body; 2. a mixing feed line; 3. a CO inlet line; 4. a carbonylation feed discharge line; 5. a kettle outer jacket; 6. a stirrer; 7. a coil pipe in the kettle; 8. a first stirring paddle; 9. a second stirring paddle; 10. a solid acid coating; 11. an isobutylene feed line; 12. a water feed line; 13. a heat transfer medium inlet line; 14. a heat transfer medium outlet line; 15. a pressure gauge; 16. and (4) a thermometer.
Detailed Description
The present invention will be further described with reference to the following examples.
As shown in fig. 1, the utility model discloses a high pressure batch autoclave cauldron body 1, 1 top of the high pressure batch autoclave cauldron body is provided with mixes feedstock line 2, CO air inlet line 3 and carbonylation material discharging pipeline 4, mix feedstock line 2, all stretch into the inside of the high pressure batch autoclave cauldron body 1 with carbonylation material discharging pipeline 4, 1 outside cladding of the high pressure batch autoclave cauldron body has cauldron overcoat cover 5, 1 inside agitator 6 and the cauldron internal coil 7 of being provided with of the high pressure batch autoclave cauldron body, 6 upper portions of agitator are provided with first stirring rake 8, 6 bottoms of agitator are provided with second stirring rake 9, be provided with solid acid coating 10 on the 1 inner wall of the high pressure batch autoclave cauldron body.
The mixing feed line 2 inside the autoclave body 1 is inclined downward and the mouth of the mixing feed line 2 faces the first stirring paddle 8.
The downward inclination angle is 45 °.
The mixed feed line 2 is connected to an isobutylene feed line 11 and a water feed line 12, respectively.
The carbonylation material discharge pipeline 4 extends into the bottom of the high-pressure reaction kettle body 1.
The first stirring paddle 8 is provided with a solid acid coating.
The solid acid coating 10 is arranged at the position of 80% of the height of the inner wall of the high-pressure reaction kettle body 1.
The heat-conducting medium inlet pipeline 13 is respectively connected with the kettle outer jacket 5 and the kettle inner coil 7.
The heat-conducting medium outlet pipeline 14 is respectively connected with the kettle outer jacket 5 and the kettle inner coil 7.
The top of the high-pressure reaction kettle body 1 is provided with a pressure gauge 15.
A thermometer 16 is arranged on the top of the high-pressure reaction kettle body 1.
After the device is detected to be normal in air tightness, CO is added into the high-pressure reaction kettle body 1 through the CO air inlet pipeline 3 to carry out air replacement and pressurization, after the pressure gauge 15 shows that the set pressure is reached, the stirrer 6 in the high-pressure reaction kettle body 1 is set to be at a certain rotating speed to start stirring, meanwhile, steam enters the kettle outer jacket 5 and the kettle inner coil 7 through the heat-conducting medium inlet pipeline 13 to heat the high-pressure reaction kettle, and the steam is discharged from the heat-conducting medium outlet pipeline 14; isobutene enters the mixed feeding pipeline 2 through the isobutene feeding pipeline 11, water enters the mixed feeding pipeline 2 through the water feeding pipeline 12, isobutene and water are mixed in the mixed feeding pipeline 2 and then enter the high-pressure reaction kettle body 1, the temperature meter 16 shows that the set temperature is reached, the rotating speed is increased to the set rotating speed to react to obtain a carbonylation material, the carbonylation material enters the separation tank through the carbonylation material discharging pipeline 4 to be stood for layering after sampling and detection are qualified, and an upper-layer organic-phase crude pivalic acid product is taken to be subjected to reduced pressure rectification to obtain a finished pivalic acid product.
Claims (10)
1. The utility model provides a device of preparation pivalic acid, including the high pressure batch autoclave cauldron body (1), its characterized in that high pressure batch autoclave cauldron body (1) top is provided with mixes feedstock line (2), CO air inlet line (3) and carbonylation material discharging line (4), mix feedstock line (2), and carbonylation material discharging line (4) all stretch into the inside of the high pressure batch autoclave cauldron body (1), the outside cladding of the high pressure batch autoclave cauldron body (1) has cauldron overcoat cover (5), inside agitator (6) and the interior coil pipe of cauldron (7) of being provided with of the high pressure batch autoclave cauldron body (1), agitator (6) upper portion is provided with first stirring rake (8), agitator (6) bottom is provided with second stirring rake (9), be provided with solid acid coating (10) on the high pressure batch autoclave cauldron body (1) inner wall.
2. An apparatus for producing pivalic acid according to claim 1, wherein the mixing feed line (2) inside the autoclave body (1) is inclined downward and the orifice of the mixing feed line (2) is directed toward the first agitating blade (8).
3. An apparatus for preparing pivalic acid according to claim 2, wherein the downward inclination angle is 43 to 48 °.
4. An apparatus for producing pivalic acid according to claim 1, wherein the mixed feed line (2) is connected to the isobutylene feed line (11) and the water feed line (12), respectively.
5. The apparatus according to claim 1, wherein the carbonylate outlet line (4) extends to the bottom of the autoclave body (1).
6. An apparatus for producing pivalic acid according to claim 1, wherein the first stirring paddle (8) is provided with a solid acid coating.
7. An apparatus for producing pivalic acid according to claim 1, wherein the solid acid coating layer (10) is provided at a position 60 to 90% of the height of the inner wall of the autoclave body (1).
8. An apparatus for preparing pivalic acid according to claim 1, wherein the heat transfer medium inlet line (13) is connected to the tank outer jacket (5) and the tank inner coil (7), respectively.
9. An apparatus for producing pivalic acid according to claim 1, wherein the heat transfer medium outlet line (14) is connected to the tank outer jacket (5) and the tank inner coil (7), respectively.
10. The apparatus for preparing pivalic acid according to claim 1, wherein a pressure gauge (15) and a temperature gauge (16) are provided on the top of the autoclave body (1).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201922288490.0U CN211487670U (en) | 2019-12-17 | 2019-12-17 | Device for preparing pivalic acid |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201922288490.0U CN211487670U (en) | 2019-12-17 | 2019-12-17 | Device for preparing pivalic acid |
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| CN211487670U true CN211487670U (en) | 2020-09-15 |
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| CN201922288490.0U Active CN211487670U (en) | 2019-12-17 | 2019-12-17 | Device for preparing pivalic acid |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110787762A (en) * | 2019-12-17 | 2020-02-14 | 山东民基化工有限公司 | Method and device for preparing pivalic acid |
| WO2022099691A1 (en) * | 2020-11-16 | 2022-05-19 | 单县欣润化工有限公司 | Device and production method for continuously generating 2-chloro-5-trifluoromethylpyridine |
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2019
- 2019-12-17 CN CN201922288490.0U patent/CN211487670U/en active Active
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110787762A (en) * | 2019-12-17 | 2020-02-14 | 山东民基化工有限公司 | Method and device for preparing pivalic acid |
| CN110787762B (en) * | 2019-12-17 | 2024-01-12 | 山东民基新材料科技有限公司 | Method and device for preparing pivalic acid |
| WO2022099691A1 (en) * | 2020-11-16 | 2022-05-19 | 单县欣润化工有限公司 | Device and production method for continuously generating 2-chloro-5-trifluoromethylpyridine |
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