CN109336759A - Continuously prepare the method and device thereof of chloro-pivalyl chloride - Google Patents
Continuously prepare the method and device thereof of chloro-pivalyl chloride Download PDFInfo
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- CN109336759A CN109336759A CN201811465178.8A CN201811465178A CN109336759A CN 109336759 A CN109336759 A CN 109336759A CN 201811465178 A CN201811465178 A CN 201811465178A CN 109336759 A CN109336759 A CN 109336759A
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- optical chlorinating
- reaction
- chloro
- chlorine
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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
- C07C51/58—Preparation of carboxylic acid halides
- C07C51/62—Preparation of carboxylic acid halides by reactions not involving the carboxylic acid halide group
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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
- C07C51/58—Preparation of carboxylic acid halides
- C07C51/64—Separation; Purification; Stabilisation; Use of additives
Abstract
The invention belongs to chemical technology fields, and in particular to a method of chloro-pivalyl chloride continuously is prepared, pivaloyl chloride successively flows into concatenated optical chlorinating reaction device, and chlorine is passed through to each optical chlorinating reaction device, optical chlorinating reaction is carried out in the reactor, and reaction solution obtains chloro-pivalyl chloride through rectifying；The present invention also provides the devices for continuously preparing chloro-pivalyl chloride, including concatenated optical chlorinating reaction device and rectification zone, each optical chlorinating reaction device bottom to be connected with chlorine snorkel, and rectification zone includes light steaming tower and steams tower again；Preparation method pivaloyl chloride and chlorine of the invention feeds gas liquid reaction simultaneously, reduces reaction risk, improves reaction controllability, simultaneously by the way that concatenated optical chlorinating reaction continuously gets up with rectification section, reaction efficiency is improved, the reaction time is reduced, reduces the generation of by-product.
Description
Technical field
The invention belongs to chemical technology fields, and in particular to a kind of method and its dress for continuously preparing chloro-pivalyl chloride
It sets.
Background technique
The preparation process of chloro-pivalyl chloride has had many reports, mainly there is pivaloyl chloride, 3-hydroxypivalic acid, spy penta
Sour chloridising, China mostly uses pivaloyl chloride interval light chlorination process at present, the technique there are equipment capacities low, production week
Phase it is long (reaction time is longer, 30h or more), poor product quality (containing pivaloyl chloride, the pivalic acid acid anhydride for having more than 0.6% with
And more chloro-pivalyl chlorides etc.), production have gap (needing non-cutting time), reaction controlling difficulty it is big (reaction is mostly gas solid/liquid/gas reactions,
Reaction condition, which is difficult to control, causes stable product quality poor) the disadvantages of.
Chinese patent CN108341744A discloses a kind of method and device thereof for preparing chloro-pivalyl chloride, and this method is
Using pivaloyl chloride and chlorine as raw material, by the way that initiator, ultraviolet light are added in pivaloyl chloride and on chlorination inner wall of tower
Nano-titanium dioxide film is set, ultraviolet light and initiator, nano-titanium dioxide synergistic effect under, improve reaction efficiency,
The optical chlorinating reaction time is foreshortened into 8-12h.But the patent uses intermittent tank reactor, and production has gap, and reaction kettle holds
Product is limited to cause produce load low；And the patent needs to add initiator in the reaction system, requires reaction unit high, meeting
Lead to high production cost, cumbersome problem.
Summary of the invention
It is an object of the invention to overcome the prior art, there are disadvantages, provide a kind of side for continuously preparing chloro-pivalyl chloride
Method, pivaloyl chloride and chlorine feed gas liquid reaction simultaneously, while by the way that concatenated optical chlorinating reaction device and rectification section is continuous
Get up, improve reaction efficiency, reduce the reaction time, reduce the generation of by-product, improves product quality.
To achieve the above object, following technical scheme of the present invention:
A method of chloro-pivalyl chloride continuously being prepared, pivaloyl chloride successively flows into concatenated optical chlorinating reaction device, together
When to each optical chlorinating reaction device be passed through chlorine at different flow rates, carry out optical chlorinating reaction, reaction solution in the reactor under room temperature
Through rectifying, chloro-pivalyl chloride is obtained；Wherein, the number of optical chlorinating reaction device is no less than 3.
Further, the number of optical chlorinating reaction device is 5, and the ratio that each reactor is passed through amount of chlorine is 5:4.5:4:3.5:
3。
Further, reaction solution steams tower and again steaming tower completion rectifying twice through light.
Further, the mass ratio of pivaloyl chloride and chlorine is 8-15:1.
Further, the wavelength of optical chlorinating reaction is 320-370nm, and preferred optical chlorinating reaction wavelength is 345-365nm, light
The chlorination reaction time is 9-10h.
Further, gently steam tower rectifying condition be vacuum degree -0.095Mpa, 50-55 DEG C of tower top temperature；The rectifying of tower is steamed again
Condition be vacuum degree -0.095Mpa, 105-110 DEG C of tower top temperature.
It is a further object of the present invention to provide a kind of devices for continuously preparing chloro-pivalyl chloride.
A kind of device continuously preparing chloro-pivalyl chloride, including optical chlorinating reaction area and rectification zone, optical chlorinating reaction area
Including liquid feeding end and outlet end, the optical chlorinating reaction area is made of the concatenated optical chlorinating reaction device of at least three, and each Light chlorimation is anti-
Device bottom is answered to set chlorine inlet, chlorine inlet is connected with chlorine snorkel；Rectification zone includes light steaming tower and steams tower again, light to steam in tower
Portion's inlet is connected with optical chlorinating reaction area outlet end, top liquid outlet by pivaloyl chloride return pipe and optical chlorinating reaction area into
Liquid end is connected, and bottom liquid outlet is connected with steaming tower inlet again.
Further, optical chlorinating reaction area liquid feeding end is connected with pivaloyl chloride storage tank, steams tower top end liquid outlet again and chloro is special
The connection of valeric chloride high-boiling components storage tank is steamed tower bottom liquid outlet again and is connect with chloro-pivalyl chloride storage tank.
Further, optical chlorinating reaction device each reactor volume from liquid feeding end to outlet end successively successively decreases, specifically, each anti-
It answers device floor space identical, highly gradually decreases, by taking number of reactors is 5 as an example, the height ratio of each reactor is 5:4.5:4:
3.5:3.
Further, pivaloyl chloride storage tank is heat insulated tank, and the temperature of pivaloyl chloride is 50 DEG C in storage tank, pivaloyl chloride from
Storage tank enters in optical chlorinating reaction device, it is ensured that the initial reaction temperature of optical chlorinating reaction is 50 DEG C, so that it is anti-to improve Light chlorimation
The efficiency answered, since optical chlorinating reaction is exothermic reaction, subsequent optical chlorinating reaction can carry out at normal temperature, without another
External heat.
Further, optical chlorinating reaction device bottom end is equipped with multiband ultraviolet lamp, and optical chlorinating reaction device outside is ultraviolet equipped with blocking
The diaphragm of light.
When starting reaction, pivaloyl chloride flows into level-one optical chlorinating reaction device from pivaloyl chloride storage tank by pump, and chlorine is from light
Chlorination reactor bottom enters reactor, and each height for reactor successively successively decreases, and liquid is entered next anti-by overflow in reactor
It answers in device, therefore there are the residence time in each reactor, the reactant for facilitating optical chlorinating reaction connects liquid in reactor
Touching completely, to improve reaction efficiency, reduces the purpose of the generation of by-product impurity.
According to the above aspect of the present invention, the present invention has at least the following advantages:
1, preparation method pivaloyl chloride of the invention and chlorine feed gas liquid reaction simultaneously, and optical chlorinating reaction area is equipped with series connection
Multiple optical chlorinating reaction devices, compared with single reactor, chlorine is evenly distributed, raw material contact it is more complete, be beneficial to prevent office
Side reaction increases caused by portion's reaction excessively fierceness, to reduce the generation of by-product, improves product quality；Simultaneously pass through by
Concatenated optical chlorinating reaction device continuously gets up with rectification section, and optical chlorinating reaction liquid continuously enters rectifying section, with intermittent reaction
Kettle is compared, and gap is not reacted, to improve reaction efficiency, reduces total reaction time.The purity of product of the present invention is 99.5%
More than, total reaction time within 11h,.
2, preparation method pivaloyl chloride of the invention and chlorine feed gas liquid reaction simultaneously, and optical chlorinating reaction uses gas-liquid two
Phase reaction, reaction can carry out at normal temperature, so that pivaloyl chloride is gasified without heating, without adding catalyst, react more easily-controllable
System, low energy consumption.
3, each optical chlorinating reaction device of preparation method of the invention is passed through the amount difference of chlorine, to make the distributed effect of chlorine
Good, reaction efficiency is higher.
4, preparation method of the invention is by control pivaloyl chloride and chlorine feed ratio and concatenated number of reactors, when anti-
Answering device number is 5, and when pivaloyl chloride and chlorine feed mass ratio are 8-15:1, optical chlorinating reaction pivaloyl chloride conversion ratio is reachable
To 48% or more.
5, it is provided by the present invention continuously prepare the device of chloro-pivalyl chloride connected by concatenated optical chlorinating reaction device and
At, production capacity is strong, while continuous preparation solves the problems, such as reaction gap, when optical chlorinating reaction device number is 5, it can be achieved that
7000 tons of chloro-pivalyl chloride annual output.
Detailed description of the invention
Fig. 1 is the structural schematic diagram that 1-3 of the embodiment of the present invention prepares chloro-pivalyl chloride device:
Wherein: 1 pivaloyl chloride storage tank, 2 pivaloyl chloride return pipes, 3 optical chlorinating reaction device 1#, 4 optical chlorinating reaction device 2#, 5
Optical chlorinating reaction device 3#, 6 optical chlorinating reaction device 4#, 7 optical chlorinating reaction device 5#, 8 ultraviolet lamps, 9 shading diaphragms, 10 chlorine air inlets
Tower, 13 chloro-pivalyl chloride high-boiling components storage tanks, 14 chloro-pivalyl chloride product storage tanks are steamed in pipe, 11 light tower, 12 of steaming again
Fig. 2 is the structural schematic diagram that comparative example 2 of the present invention prepares chloro-pivalyl chloride device.
Specific embodiment
Below by embodiment, the invention will be described in further detail, but the invention is not limited to following embodiment party
Formula.
Raw material used in various embodiments of the present invention: pivaloyl chloride is that company has product by oneself；The technical indicator of pivaloyl chloride:
Colourless transparent liquid, content >=99.67%, impurity pivalic acid≤0.083%, pivalic acid acid anhydride≤0.13 are Grade A.
Reaction equation: (CH3) 3CCOCl+Cl2 → ClCH2C (CH3) 2COCl+HCl
Embodiment 1:
The present embodiment is calculated with producing 7000 tons per year according to 300 days production dates, and continuous preparation 24 hours one day produces 23 tons daily
For.
Pivaloyl chloride is successively flowed into optical chlorinating reaction device 1#, light chlorine by pivaloyl chloride storage tank 1 with 756.3kg/h flow velocity
Change reactor 2#, optical chlorinating reaction device 3#, optical chlorinating reaction device 4#, in optical chlorinating reaction device 5#, while controlling chlorine and being always passed through
Amount be 75.6kg/h, chlorine by the bottom optical chlorinating reaction device 1#, 2#, 3#, 4#, 5# respectively with 18.9kg/h, 17.1kg/h,
15.2kg/h, 13.2kg/h, 11.3kg/h are passed through, and are reacted at room temperature, sample tap are arranged in the reactor liquid outlet position 5#, wait have
Reaction solution is flowed out from 5# reactor liquid outlet, and the content that chloro-pivalyl chloride in reaction solution is measured by sampling is 55.0wt.%, is calculated
Obtaining pivaloyl chloride conversion ratio is 48.6%, and the optical chlorinating reaction time is 9.5h at this time；Optical chlorinating reaction liquid enters light steaming tower, vacuum
55 DEG C of recycling pivaloyl chlorides of tower top temperature are controlled under degree -0.095Mpa, are entered optical chlorinating reaction through pivaloyl chloride return pipe and are thought highly of
New reaction, tower bottom reaction solution is again introduced into steams tower again, and it is special that 105 DEG C of distillation chloros of tower top temperature are controlled under vacuum degree -0.095Mpa
Valeric chloride finished product enters chloro-pivalyl chloride product storage tank, and tower bottom high-boiling components enter the high boiling storage tank of chloro-pivalyl chloride.Product chlorine
It is 99.65% for pivaloyl chloride purity, impurity pivaloyl chloride, pivalic acid acid anhydride and more chloro-pivalyl chloride total amounts 0.32%.
Embodiment 2:
The present embodiment is calculated with producing 7000 tons per year according to 300 days production dates, and continuous preparation 24 hours one day produces 23 tons daily
For.
Pivaloyl chloride is successively flowed into optical chlorinating reaction device 1#, light chlorine by pivaloyl chloride storage tank with 756.3kg/h flow velocity
Change reactor 2#, optical chlorinating reaction device 3#, optical chlorinating reaction device 4#, in optical chlorinating reaction device 5#, while controlling chlorine and being always passed through
Amount be 94.5kg/h, chlorine by the bottom optical chlorinating reaction device 1#, 2#, 3#, 4#, 5# respectively with 23.6kg/h, 21.3kg/h,
18.9kg/h, 16.5kg/h, 14.2kg/h are passed through, and are reacted at room temperature, sample tap are arranged in the reactor liquid outlet position 5#, wait have
Reaction solution is flowed out from 5# reactor liquid outlet, and the content that chloro-pivalyl chloride in reaction solution is measured by sampling is 54.5wt.%, is calculated
Obtaining pivaloyl chloride conversion ratio is 48.1%, and the optical chlorinating reaction time is 10h at this time；Optical chlorinating reaction liquid enters light steaming tower, vacuum
Tower top temperature 50 C is controlled under degree -0.095Mpa and recycles pivaloyl chloride, is entered optical chlorinating reaction through pivaloyl chloride return pipe and is thought highly of
New reaction, tower bottom reaction solution is again introduced into steams tower again, and it is special that 108 DEG C of distillation chloros of tower top temperature are controlled under vacuum degree -0.095Mpa
Valeric chloride finished product enters chloro-pivalyl chloride product storage tank, and tower bottom high-boiling components enter the high boiling storage tank of chloro-pivalyl chloride.Product chlorine
It is 99.57% for pivaloyl chloride purity, impurity pivaloyl chloride, pivalic acid acid anhydride and more chloro-pivalyl chloride total amounts 0.30%.
Embodiment 3:
The present embodiment is calculated with producing 7000 tons per year according to 300 days production dates, and continuous preparation 24 hours one day produces 23 tons daily
For.
Pivaloyl chloride is successively flowed into optical chlorinating reaction device 1#, light chlorine by pivaloyl chloride storage tank with 756.3kg/h flow velocity
Change reactor 2#, optical chlorinating reaction device 3#, optical chlorinating reaction device 4#, in optical chlorinating reaction device 5#, while controlling chlorine and being always passed through
Amount be 50.4kg/h, chlorine by the bottom optical chlorinating reaction device 1#, 2#, 3#, 4#, 5# respectively with 12.6kg/h, 11.3kg/h,
10.1kg/h, 8.8kg/h, 7.6kg/h are passed through, and are reacted at room temperature, and sample tap is arranged in the reactor liquid outlet position 5#, anti-wait have
Liquid is answered to flow out from 5# reactor liquid outlet, the content that chloro-pivalyl chloride in reaction solution is measured by sampling is 55.1wt.%, is calculated
Pivaloyl chloride conversion ratio is 48.7%, and the optical chlorinating reaction time is 9.8h at this time；Optical chlorinating reaction liquid enters light steaming tower, vacuum
52 DEG C of recycling pivaloyl chlorides of tower top temperature are controlled under degree -0.095Mpa, are entered optical chlorinating reaction through pivaloyl chloride return pipe and are thought highly of
New reaction, tower bottom reaction solution is again introduced into steams tower again, and it is special that 110 DEG C of distillation chloros of tower top temperature are controlled under vacuum degree -0.095Mpa
Valeric chloride finished product enters chloro-pivalyl chloride product storage tank, and tower bottom high-boiling components enter the high boiling storage tank of chloro-pivalyl chloride.Product chlorine
It is 99.52% for pivaloyl chloride purity, impurity pivaloyl chloride, pivalic acid acid anhydride and more chloro-pivalyl chloride total amounts 0.43%.
Comparative example 1:
Using the device for preparing chloro-pivalyl chloride in embodiment 1, a 1# optical chlorinating reaction device is only set, remaining step
Suddenly with embodiment 1.The optical chlorinating reaction time is 3h, by measurement optical chlorinating reaction at the end of in reaction solution chloro-pivalyl chloride contain
Pivaloyl chloride conversion ratio 16.8% is calculated in amount, and obtaining its purity of chloro-pivalyl chloride finished product is 98.51%, impurity pivaloyl
Chlorine, pivalic acid acid anhydride and more chloro-pivalyl chloride total amounts 1.24%.
Comparative example 2:
Using the device for preparing chloro-pivalyl chloride in embodiment 1,3 optical chlorinating reaction devices are set, respectively 1#,
2# and 3#, remaining step is the same as embodiment 1.The optical chlorinating reaction time be 6h, by measurement optical chlorinating reaction at the end of 3# reaction solution
Pivaloyl chloride conversion ratio 43.7% is calculated in middle chloro-pivalyl chloride content, obtains chloro-pivalyl chloride finished product its purity and is
99.01%, impurity pivaloyl chloride, pivalic acid acid anhydride and more chloro-pivalyl chloride total amounts 0.85%.
Comparative example 3:
Using the device for preparing chloro-pivalyl chloride in embodiment 1, optical chlorinating reaction device number is 6, remaining step
With embodiment 1.The optical chlorinating reaction time is 11h, by measurement optical chlorinating reaction at the end of in the last one reactor reaction liquid
Pivaloyl chloride conversion ratio is calculated 49.0% in chloro-pivalyl chloride content, obtains chloro-pivalyl chloride finished product its purity and is
99.53%, impurity pivaloyl chloride, pivalic acid acid anhydride and more chloro-pivalyl chloride total amounts 0.34%.
From embodiment 1 and comparative example 1 as can be seen that optical chlorinating reaction area uses plural serial stage reactor, can be improved
The product purity of reaction efficiency and chloro-pivalyl chloride；As can be seen that optical chlorinating reaction device is 3 from embodiment 1 and comparative example 2
When a, the purity of product chloro-pivalyl chloride only reaches 99.01% since the number of reactor is 3, when reaction solution always stops
Between it is short, cause the reaction time short, reaction efficiency is low, product purity be lower than embodiment 1 product purity；From embodiment 1 and comparison
Example 3 is as can be seen that when number of reactors is 5 and 6, and the product purity that optical chlorinating reaction obtains is not much different, but comparative example 3
The optical chlorinating reaction time is longer than the reaction time of embodiment 1, this is because under optical chlorinating reaction area reaction solution is flowed by overflow
One reactor, reaction solution is there are the residence time in each reactor, and the time of optical chlorinating reaction is by number of reactors
It influences, number of reactors is more, and the reaction time is longer.As can be seen that working as concatenated smooth chlorine from embodiment 1 and comparative example 1-3
When change reactor is 5, the product purity of optical chlorinating reaction and reaction time reach optimal equalization point, this reaction time is
9-10h, product purity can be to 99.5% or more.
The device of chloro-pivalyl chloride is prepared used in embodiment 1-3, as shown in Figure 1, include optical chlorinating reaction area and
Rectification zone, the optical chlorinating reaction area are made of 5 concatenated optical chlorinating reaction device 3-7, and optical chlorinating reaction area includes liquid feeding end
And outlet end, liquid feeding end are set to 1# optical chlorinating reaction device 3, outlet end is set to 5# optical chlorinating reaction device 7, each optical chlorinating reaction
Device bottom opens up chlorine inlet, and chlorine inlet is connected with chlorine snorkel 10；Rectification zone includes light steaming tower 11 and steams tower 12 again, gently
It steams 11 middle part inlet of tower to be connected with optical chlorinating reaction area outlet end, top liquid outlet passes through pivaloyl chloride return pipe 2 and light chlorine
Change reaction zone liquid feeding end to be connected, bottom liquid outlet is connected with steaming tower inlet again；
Further, optical chlorinating reaction area liquid feeding end is connected with pivaloyl chloride storage tank 1, steams tower top end liquid outlet again and chloro is special
Valeric chloride high-boiling components storage tank 13 connects, and steams tower bottom liquid outlet again and connect with chloro-pivalyl chloride storage tank 14；
Further, optical chlorinating reaction device each reactor volume from liquid feeding end to outlet end successively successively decreases；
Further, optical chlorinating reaction device bottom end is equipped with multiband ultraviolet lamp 8, and optical chlorinating reaction device outside is ultraviolet equipped with blocking
The diaphragm 9 of light.
The implementation of the present invention is not limited to this, under the premise of above-mentioned basic fundamental thought of the invention, according to this field
Ordinary technical knowledge and customary means make the modification, replacement or change of other diversified forms to the content of present invention, all fall within
Within rights protection scope of the present invention.
Claims (10)
1. a kind of method for continuously preparing chloro-pivalyl chloride, which is characterized in that pivaloyl chloride successively flows into concatenated Light chlorimation
Reactor, and it is passed through chlorine to each optical chlorinating reaction device, optical chlorinating reaction is carried out in the reactor, and reaction solution is obtained through rectifying
Chloro-pivalyl chloride；The number of the optical chlorinating reaction device is no less than 3.
2. a kind of method for continuously preparing chloro-pivalyl chloride according to claim 1, which is characterized in that the pivaloyl
The mass ratio of chlorine and chlorine is 8-15:1.
3. a kind of method for continuously preparing chloro-pivalyl chloride according to claim 1, which is characterized in that the Light chlorimation
The number of reactor is 5, and the ratio that each reactor is passed through amount of chlorine is 5:4.5:4:3.5:3.
4. a kind of method for continuously preparing chloro-pivalyl chloride according to claim 1, which is characterized in that reaction solution is through light
It steams tower and steams tower again and complete rectifying twice.
5. a kind of method for continuously preparing chloro-pivalyl chloride according to claim 1, which is characterized in that the light chlorine
The wavelength for changing reaction is 345-365nm.
6. a kind of method for continuously preparing chloro-pivalyl chloride according to claim 4, which is characterized in that the light steaming tower
Rectifying condition be vacuum degree -0.095Mpa, 50-55 DEG C of tower top temperature；The heavy rectifying condition for steaming tower is vacuum degree-
0.095Mpa, 105-110 DEG C of tower top temperature.
7. a kind of device for continuously preparing chloro-pivalyl chloride, including optical chlorinating reaction area and rectification zone, which is characterized in that described
Optical chlorinating reaction area includes liquid feeding end and outlet end, and the optical chlorinating reaction area is by the concatenated optical chlorinating reaction device group of at least three
At each optical chlorinating reaction device bottom sets chlorine inlet, and chlorine inlet is connected with chlorine snorkel；Rectification zone is including light steaming tower and again
Tower is steamed, the light tower middle part inlet that steams is connected with optical chlorinating reaction area outlet end, and top liquid outlet passes through pivaloyl chloride return pipe (2)
It is connected with optical chlorinating reaction area liquid feeding end, bottom liquid outlet is connected with steaming tower inlet (12) again.
8. a kind of device for continuously preparing chloro-pivalyl chloride according to claim 7, which is characterized in that the Light chlorimation
Reaction zone liquid feeding end is connected with pivaloyl chloride storage tank (1), steams tower top end liquid outlet again and chloro-pivalyl chloride high-boiling components storage tank connects
It connects, steams tower bottom liquid outlet again and connect with chloro-pivalyl chloride storage tank.
9. a kind of device for continuously preparing chloro-pivalyl chloride according to claim 7, which is characterized in that the Light chlorimation
Reactor each reactor volume from liquid feeding end to outlet end successively successively decreases.
10. a kind of device for continuously preparing chloro-pivalyl chloride according to claim 8, which is characterized in that described special penta
Acyl chlorides storage tank (1) is heat insulated tank.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110818558A (en) * | 2019-12-17 | 2020-02-21 | 山东民基化工有限公司 | Method and device for continuously preparing chloro pivaloyl chloride by using micro-channel |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4770821A (en) * | 1985-06-05 | 1988-09-13 | Ihara Nikkei Chemical Industry Co., Ltd. | Method for preparing β-chloropivaloyl chloride |
| CN1491932A (en) * | 2002-10-24 | 2004-04-28 | 建湖建农农药化工有限公司 | Process for preparing chloro pivaloyl chloride |
| CN101311155A (en) * | 2007-05-25 | 2008-11-26 | 江苏建农农药化工有限公司 | Process for preparing chloro-pivalyl chloride |
| CN102107132A (en) * | 2009-12-28 | 2011-06-29 | 北京有色金属研究总院 | Rectifying photochlorination device |
| CN102701960A (en) * | 2012-05-22 | 2012-10-03 | 天津大学 | Method and device for refining crude products of m-phthaloyl chloride |
| CN103739473A (en) * | 2014-01-14 | 2014-04-23 | 江西科苑生物药业有限公司 | Continuous distillation process for aromatic acyl chloride |
| CN104225946A (en) * | 2014-09-30 | 2014-12-24 | 烟台裕祥精细化工有限公司 | Continuous rectifying device and rectifying method for acyl chloride |
| CN204093431U (en) * | 2014-09-30 | 2015-01-14 | 烟台裕祥精细化工有限公司 | A kind of tower continuous light chlorination reaction device |
| CN105348036A (en) * | 2015-12-14 | 2016-02-24 | 山东凯盛新材料有限公司 | Continuous production process of p-xylylene dichloride and device |
-
2018
- 2018-12-03 CN CN201811465178.8A patent/CN109336759A/en active Pending
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4770821A (en) * | 1985-06-05 | 1988-09-13 | Ihara Nikkei Chemical Industry Co., Ltd. | Method for preparing β-chloropivaloyl chloride |
| CN1491932A (en) * | 2002-10-24 | 2004-04-28 | 建湖建农农药化工有限公司 | Process for preparing chloro pivaloyl chloride |
| CN101311155A (en) * | 2007-05-25 | 2008-11-26 | 江苏建农农药化工有限公司 | Process for preparing chloro-pivalyl chloride |
| CN102107132A (en) * | 2009-12-28 | 2011-06-29 | 北京有色金属研究总院 | Rectifying photochlorination device |
| CN102701960A (en) * | 2012-05-22 | 2012-10-03 | 天津大学 | Method and device for refining crude products of m-phthaloyl chloride |
| CN103739473A (en) * | 2014-01-14 | 2014-04-23 | 江西科苑生物药业有限公司 | Continuous distillation process for aromatic acyl chloride |
| CN104225946A (en) * | 2014-09-30 | 2014-12-24 | 烟台裕祥精细化工有限公司 | Continuous rectifying device and rectifying method for acyl chloride |
| CN204093431U (en) * | 2014-09-30 | 2015-01-14 | 烟台裕祥精细化工有限公司 | A kind of tower continuous light chlorination reaction device |
| CN105348036A (en) * | 2015-12-14 | 2016-02-24 | 山东凯盛新材料有限公司 | Continuous production process of p-xylylene dichloride and device |
Non-Patent Citations (2)
| Title |
|---|
| 蒋卓良等: "气液反应精馏新工艺连续制备氯代特戊酰氯 ", 《化学与生物工程》 * |
| 蒋彪等: "连续液相氯化法合成β-氯代特戊酰氯 ", 《化工进展》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110818558A (en) * | 2019-12-17 | 2020-02-21 | 山东民基化工有限公司 | Method and device for continuously preparing chloro pivaloyl chloride by using micro-channel |
| CN110818558B (en) * | 2019-12-17 | 2023-09-08 | 山东民基新材料科技有限公司 | Method and device for continuously preparing chloro-pivaloyl chloride by utilizing micro-channel |
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