CN111675607A - Method for producing trimethyl orthoacetate through differential circulation and continuous production - Google Patents
Method for producing trimethyl orthoacetate through differential circulation and continuous production Download PDFInfo
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- CN111675607A CN111675607A CN202010519175.9A CN202010519175A CN111675607A CN 111675607 A CN111675607 A CN 111675607A CN 202010519175 A CN202010519175 A CN 202010519175A CN 111675607 A CN111675607 A CN 111675607A
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- HDPNBNXLBDFELL-UHFFFAOYSA-N 1,1,1-trimethoxyethane Chemical compound COC(C)(OC)OC HDPNBNXLBDFELL-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 20
- 238000010924 continuous production Methods 0.000 title claims abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 34
- 239000007788 liquid Substances 0.000 claims abstract description 33
- 239000002904 solvent Substances 0.000 claims abstract description 27
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000000926 separation method Methods 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 14
- 239000012528 membrane Substances 0.000 claims abstract description 12
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 72
- 238000010521 absorption reaction Methods 0.000 claims description 39
- 239000000243 solution Substances 0.000 claims description 34
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 27
- 238000006136 alcoholysis reaction Methods 0.000 claims description 22
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 16
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 16
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims description 15
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims description 15
- 238000006386 neutralization reaction Methods 0.000 claims description 10
- 235000019270 ammonium chloride Nutrition 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 8
- 239000011259 mixed solution Substances 0.000 claims description 7
- 239000006227 byproduct Substances 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 6
- 150000003839 salts Chemical class 0.000 claims description 6
- CYSGHNMQYZDMIA-UHFFFAOYSA-N 1,3-Dimethyl-2-imidazolidinon Chemical compound CN1CCN(C)C1=O CYSGHNMQYZDMIA-UHFFFAOYSA-N 0.000 claims description 3
- 239000002351 wastewater Substances 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 abstract description 3
- 230000036632 reaction speed Effects 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 24
- 238000002156 mixing Methods 0.000 description 15
- 239000000047 product Substances 0.000 description 10
- 230000001105 regulatory effect Effects 0.000 description 9
- 238000009835 boiling Methods 0.000 description 7
- 229910021529 ammonia Inorganic materials 0.000 description 6
- 238000003860 storage Methods 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- GWHJZXXIDMPWGX-UHFFFAOYSA-N 1,2,4-trimethylbenzene Chemical compound CC1=CC=C(C)C(C)=C1 GWHJZXXIDMPWGX-UHFFFAOYSA-N 0.000 description 2
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000003456 ion exchange resin Substances 0.000 description 2
- 229920003303 ion-exchange polymer Polymers 0.000 description 2
- 239000002608 ionic liquid Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 description 2
- NOWKCMXCCJGMRR-UHFFFAOYSA-N Aziridine Chemical compound C1CN1 NOWKCMXCCJGMRR-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- KXKVLQRXCPHEJC-UHFFFAOYSA-N acetic acid trimethyl ester Natural products COC(C)=O KXKVLQRXCPHEJC-UHFFFAOYSA-N 0.000 description 1
- NMVVJCLUYUWBSZ-UHFFFAOYSA-N aminomethylideneazanium;chloride Chemical compound Cl.NC=N NMVVJCLUYUWBSZ-UHFFFAOYSA-N 0.000 description 1
- CBHOOMGKXCMKIR-UHFFFAOYSA-N azane;methanol Chemical compound N.OC CBHOOMGKXCMKIR-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 239000012043 crude product Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 239000003350 kerosene Substances 0.000 description 1
- 125000000956 methoxy group Chemical group [H]C([H])([H])O* 0.000 description 1
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
- 239000001993 wax Substances 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/60—Preparation of compounds having groups or groups
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/009—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping in combination with chemical reactions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0093—Microreactors, e.g. miniaturised or microfabricated reactors
Abstract
The invention provides a method for producing trimethyl orthoacetate by differential circulation and continuity, which is characterized by comprising the following steps: the method comprises the following steps: the method adopts DMI as a solvent, improves the yield of hydrochloride, and has good salification quality; solid-liquid separation is realized by utilizing a membrane separation technology, and the product yield is improved; the differential circulation tube type reaction device is adopted, so that continuous production can be realized, the reaction speed is increased, and the production efficiency is improved; the trimethyl orthoacetate is separated by adopting a negative pressure rectification method, the product purity is high, the solvent in the tower kettle can be recycled, no waste water is generated, and the method is very environment-friendly.
Description
Technical Field
The invention relates to the field of fine chemical engineering, in particular to a method for producing trimethyl orthoacetate through differential circulation and continuity.
Background
Trimethyl orthoacetate is also known as 1,1, 1-trimethoxyethane. The liquid is colorless and transparent liquid with pleasant smell at normal pressure and temperature, is insoluble in water, and is soluble in organic solvents such as ethanol and diethyl ether. The molecular formula is C5H12O3, and the structural formula is CH3C (OCH3) 3. The main application is the organic intermediate for synthesizing medicines and pesticides.
At present, the commonly reported production process of trimethyl orthoacetate takes ethylene wax, absolute methanol and dry hydrogen chloride as raw materials, and performs salt forming reaction under the action of a solvent to generate ethylimine formamidine hydrochloride, and then methanol is added for alcoholysis reaction to prepare trimethyl orthoacetate. Wherein, the selection of the solvent has great influence on the reaction process, and the solvents with low boiling point, such as normal hexane, carbon tetrachloride and kerosene, which are commonly used in industry have large toxicity, easy volatilization and large dosage, are not beneficial to safe production and low-cost operation. Meanwhile, a centrifugal machine is adopted for filtering in the solid-liquid separation process of the byproduct ammonium chloride and trimethyl orthoacetate, the safety production is not facilitated, and the ammonium chloride carried in the filtered alcohol solution is washed by water due to low filtering precision, so that on one hand, waste water is generated, and on the other hand, the yield of methyl orthoacetate is reduced.
CN 102924244A (43), discloses a production process of high-quality trimethyl orthoacetate, which comprises the steps of preparing ethimine A hydrochloride by salifying ethyl wax, methanol and hydrogen chloride in the presence of pseudocumene as a solvent, then placing the ethimine A hydrochloride into a methanol solution, dropwise adding ammonia methanol solution to adjust the pH value, carrying out alcoholysis reaction to obtain a trimethyl orthoacetate crude product, filtering to remove solid ammonium chloride and recycling, adsorbing the filtrate by strong-basicity macroporous ion exchange resin to remove chloride ions, and finally obtaining the trimethyl orthoacetate product by continuous fine filling. The disadvantages of this method are: the strong-alkaline macroporous ion exchange resin generates an acid-base solution in the regeneration process, which causes the problem of wastewater treatment.
The invention has the following patent: a preparation method (CN201410047965.6) of a process for continuously preparing trimethyl orthoacetate by taking ionic liquid as a solvent comprises the steps of feeding anhydrous acetonitrile, anhydrous methanol and the solvent into a reaction kettle, cooling to-5 ℃ at a low temperature, introducing dry hydrogen chloride gas into the kettle, stirring for reaction for 6 hours, conveying the mixed solution into a second reaction kettle, adding precooled methanol at the temperature of 5 ℃, stirring for 0.5 hour, adjusting the pH of the reaction system to 5-6 by ammonia gas, and conducting alcoholysis on the mixed solution for 12 hours at the temperature of 40 ℃, wherein the solvent is hydrophobic ionic liquid; cooling the alcoholysis solution to 0 ℃, adjusting the pH value to 8.0 by using ammonia gas, then conveying the alcoholysis solution into a normal-pressure rectifying tower, and collecting fractions at 107-109 ℃ to obtain a trimethyl orthoacetate product; and (3) feeding the bottom kettle liquid of the rectifying tower into a washing kettle for washing, feeding the lower layer liquid into a drying kettle for drying, and recycling the dried solvent. The method has the disadvantages that the reaction process is a kettle type continuous reaction, the reaction time is long, the bottom liquid of the rectifying kettle is washed by adding water, the operation is complicated, and the problem of sewage treatment generated by washing water is solved.
The method for producing trimethyl orthoacetate by taking acetonitrile, methanol and hydrogen chloride as raw materials comprises the steps of intermittent production, continuous production and wastewater production, and causes pressure on the environment.
Disclosure of Invention
The invention aims to provide a method for producing trimethyl orthoacetate by differential circulation and continuous production, so as to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme:
a method for producing trimethyl orthoacetate by differential circulation continuity comprises the following steps:
(1) absorption and cooling: feeding anhydrous acetonitrile, anhydrous methanol and a solvent into a reaction absorption tower to be absorbed and mixed with introduced dry hydrogen chloride gas at low temperature;
(2) salt forming reaction: introducing the mixed solution into a differential circulation tube type reaction device for salt forming reaction;
(3) and (3) neutralization reaction: introducing ammonia gas into a differential circulation tube type reaction device for neutralization reaction;
(4) alcoholysis reaction: carrying out alcoholysis reaction in a differential circulating tube type reaction device;
(5) membrane separation: cooling the alcoholysis solution to 0 ℃, and separating a by-product ammonium chloride by a membrane separation method;
(6) and (3) rectification: and (3) feeding the separated alcoholysis solution into a normal pressure rectifying tower to recover excessive methanol solution, feeding the bottom liquid of the normal pressure rectifying tower into a negative pressure rectifying tower to obtain trimethyl orthoacetate, and returning the bottom liquid of the negative pressure rectifying tower to the step (1) to be used as a solvent.
Preferably, the solvent in the step 1 is dimethylethylene urea, abbreviated as DMI, the dosage of which is 1-2 times of the total mass of the anhydrous acetonitrile and the anhydrous methanol, the dosage of the anhydrous methanol is equal to the molar quantity of the anhydrous acetonitrile, and the cooling absorption temperature is-5 ℃.
Preferably, the reaction temperature in the step 2 is 10 ℃.
Preferably, the pH of the reaction system is adjusted to 5 to 7 in the step 3.
Preferably, the reaction temperature in the step 4 is 40 ℃.
Compared with the prior art, the invention has the following advantages: DMI is used as a solvent, so that the yield of hydrochloride is improved, and the salt formation quality is good; solid-liquid separation is realized by utilizing a membrane separation technology, and the product yield is improved; the differential circulation tube type reaction device is adopted, so that continuous production can be realized, the reaction speed is increased, and the production efficiency is improved; the trimethyl orthoacetate is separated by adopting a negative pressure rectification method, the product purity is high, the solvent in the tower kettle can be recycled, no waste water is generated, and the method is very environment-friendly.
Drawings
FIG. 1 is a schematic flow chart of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Accurately metering the methanol solution in the tank area by a pump through a flowmeter and then feeding the methanol solution into a bubble tower at the top of the absorption tower; the solvent DMI in the tank area is accurately metered by a pump through a flowmeter and then enters a bubble tower at the top of the absorption tower; the acetonitrile solution in the tank field enters a bubble tower at the top of the absorption tower after being accurately measured by a pump through a flowmeter; the flow of the dried hydrogen chloride from the previous procedure is regulated by a regulating valve, the dried hydrogen chloride enters the bottom of an absorption tower, the dried hydrogen chloride enters the absorption tower to be absorbed and mixed, the mixed liquid at the bottom of the absorption tower is pumped out by a circulating pump, the temperature of the mixed liquid at the bottom of the absorption tower is controlled to be minus 5 ℃, the mixed liquid enters the middle part of the absorption tower, and one part of the mixed liquid enters a mixing pump in front of a sali; the materials are fully mixed by a mixing pump and then enter a differential circulation tubular reactor, the differential circulation tubular reactor is a heat exchanger with heat exchange, the reaction temperature is controlled at 10 ℃, the materials of the differential circulation tubular reactor enter a buffer, one part of the materials enter the mixing pump, and the other part of the materials enter a neutralization device through a discharge pump.
The absorption mixed liquid from the discharge pump and the gas ammonia from the ammonia storage tank are subjected to neutralization reaction in the Venturi reactor through the regulating valve, and the PH value is controlled to be 5.
The mixed pump is used for pressurizing and half metering the solution in the methanol tank area by the pump and then feeding the solution and the neutralized solution into the alcoholysis differential circulating tubular reactor; the materials are fully mixed by a mixing pump and then enter a differential circulation tubular reactor, the differential circulation tubular reactor is a heat exchanger with heat exchange, the reaction temperature is controlled at 40 ℃, the materials of the differential circulation tubular reactor enter a buffer, one part of the materials enter the mixing pump, and the other part of the materials are cooled to 0 ℃ by a cooler through a discharge pump and then enter a membrane separation device.
And (3) carrying out solid-liquid separation on the cooled alcoholysis solution in a membrane separation device, wherein the separated ammonium chloride is a byproduct. The trimethyl orthoacetate containing the solvent enters a rectification device.
The mixed solution of trimethyl orthoacetate and solvent is pumped into the middle part of a low-boiling tower by a pump after passing through a storage tank, low-boiling substances at the top of the tower are condensed and then enter an alcoholysis reaction device, tower bottom liquid enters a vacuum rectifying tower, the product trimethyl orthoacetate at the top of the tower enters an absorption device, and the product trimethyl orthoacetate at the bottom of the tower enters an absorption device.
Example 2
Accurately metering the methanol solution in the tank area by a pump through a flowmeter and then feeding the methanol solution into a bubble tower at the top of the absorption tower; the solvent DMI in the tank area is accurately metered by a pump through a flowmeter and then enters a bubble tower at the top of the absorption tower; the acetonitrile solution in the tank field enters a bubble tower at the top of the absorption tower after being accurately measured by a pump through a flowmeter; the flow of the dried hydrogen chloride from the previous procedure is regulated by a regulating valve, the dried hydrogen chloride enters the bottom of an absorption tower, the dried hydrogen chloride enters the absorption tower to be absorbed and mixed, the mixed liquid at the bottom of the absorption tower is pumped out by a circulating pump, the temperature of the mixed liquid at the bottom of the absorption tower is controlled to be minus 0 ℃, the mixed liquid enters the middle part of the absorption tower, and one part of the mixed liquid enters a mixing pump in front of a sali; the materials are fully mixed by a mixing pump and then enter a tubular reactor, the tubular reactor is a heat exchanger with heat exchange, the reaction temperature is controlled at 18 ℃, the materials of the tubular reactor enter a buffer, one part of the materials enter the mixing pump, and the other part of the materials enter a neutralization device through a discharge pump.
The absorption mixed liquid from the discharge pump and the gas ammonia from the ammonia storage tank are subjected to neutralization reaction in the Venturi reactor through the regulating valve, and the PH value is controlled to be 6.
The mixed pump is used for pressurizing and half metering the solution in the methanol tank area by the pump and then feeding the solution and the neutralized solution into the alcoholysis differential circulating tubular reactor; the materials are fully mixed by a mixing pump and then enter a tubular reactor, the tubular reactor is a heat exchanger with heat exchange, the reaction temperature is controlled at 40 ℃, the materials of the tubular reactor enter a buffer, one part of the materials enter the mixing pump, and the other part of the materials enter a membrane separation device after being cooled to 0 ℃ by a cooler through a discharge pump.
And (3) carrying out solid-liquid separation on the cooled alcoholysis solution in a membrane separation device, wherein the separated ammonium chloride is a byproduct. The trimethyl orthoacetate containing the solvent enters a rectification device.
The mixed solution of trimethyl orthoacetate and solvent is pumped into the middle part of a low-boiling tower by a pump after passing through a storage tank, low-boiling substances at the top of the tower are condensed and then enter an alcoholysis reaction device, tower bottom liquid enters a vacuum rectifying tower, the product trimethyl orthoacetate at the top of the tower enters an absorption device, and the product trimethyl orthoacetate at the bottom of the tower enters an absorption device.
Example 3
Accurately metering the methanol solution in the tank area by a pump through a flowmeter and then feeding the methanol solution into a bubble tower at the top of the absorption tower; the solvent DMI in the tank area is accurately metered by a pump through a flowmeter and then enters a bubble tower at the top of the absorption tower; the acetonitrile solution in the tank field enters a bubble tower at the top of the absorption tower after being accurately measured by a pump through a flowmeter; the flow of the dried hydrogen chloride from the previous procedure is regulated by a regulating valve, the dried hydrogen chloride enters the bottom of an absorption tower, the dried hydrogen chloride enters the absorption tower to be absorbed and mixed, the mixed liquid at the bottom of the absorption tower is pumped out by a circulating pump, the temperature of the mixed liquid at the bottom of the absorption tower is controlled to be minus 10 ℃, the mixed liquid enters the middle part of the absorption tower, and one part of the mixed liquid enters a mixing pump in front of a sali; the materials are fully mixed by a mixing pump and then enter a tubular reactor, the tubular reactor is a heat exchanger with heat exchange, the reaction temperature is controlled at 16 ℃, the materials of the tubular reactor enter a buffer, one part of the materials enter the mixing pump, and the other part of the materials enter a neutralization device through a discharge pump.
The absorption mixed liquid from the discharge pump and the gas ammonia from the ammonia storage tank are subjected to neutralization reaction in the Venturi reactor through the regulating valve, and the PH value is controlled to be 7.
The mixed pump is used for pressurizing and half metering the solution in the methanol tank area by the pump and then feeding the solution and the neutralized solution into the alcoholysis differential circulating tubular reactor; the materials are fully mixed by a mixing pump and then enter a tubular reactor, the tubular reactor is a heat exchanger with heat exchange, the reaction temperature is controlled at 40 ℃, the materials of the tubular reactor enter a buffer, one part of the materials enter the mixing pump, and the other part of the materials enter a membrane separation device after being cooled to 0 ℃ by a cooler through a discharge pump.
And (3) carrying out solid-liquid separation on the cooled alcoholysis solution in a membrane separation device, wherein the separated ammonium chloride is a byproduct. The trimethyl orthoacetate containing the solvent enters a rectification device.
The mixed solution of trimethyl orthoacetate and solvent is pumped into the middle part of a low-boiling tower by a pump after passing through a storage tank, low-boiling substances at the top of the tower are condensed and then enter an alcoholysis reaction device, tower bottom liquid enters a vacuum rectifying tower, the product trimethyl orthoacetate at the top of the tower enters an absorption device, and the product trimethyl orthoacetate at the bottom of the tower enters an absorption device.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Claims (5)
1. A method for producing trimethyl orthoacetate by differential circulation continuity is characterized in that: the method comprises the following steps:
(1) absorption and cooling: feeding anhydrous acetonitrile, anhydrous methanol and a solvent into a reaction absorption tower to be absorbed and mixed with introduced dry hydrogen chloride gas at low temperature;
(2) salt forming reaction: introducing the mixed solution into a differential circulation tube type reaction device for salt forming reaction;
(3) and (3) neutralization reaction: introducing ammonia gas into a differential circulation tube type reaction device for neutralization reaction;
(4) alcoholysis reaction: carrying out alcoholysis reaction in a differential circulating tube type reaction device;
(5) membrane separation: cooling the alcoholysis solution to 0 ℃, and separating a by-product ammonium chloride by a membrane separation method;
(6) and (3) rectification: and (3) feeding the separated alcoholysis solution into a normal pressure rectifying tower to recover excessive methanol solution, feeding the bottom liquid of the normal pressure rectifying tower into a negative pressure rectifying tower to obtain trimethyl orthoacetate, and returning the bottom liquid of the negative pressure rectifying tower to the step (1) to be used as a solvent.
2. The method for producing trimethyl orthoacetate by differential loop continuous production according to claim 1, wherein: the solvent in the step 1 is dimethylethylene urea, DMI for short, the dosage of the dimethylethylene urea is 1-2 times of the total mass of the anhydrous acetonitrile and the anhydrous methanol, the dosage of the anhydrous methanol is equal to the molar quantity of the anhydrous acetonitrile, and the cooling absorption temperature is-5 ℃.
3. The method for producing trimethyl orthoacetate by differential loop continuous production according to claim 1, wherein: the reaction temperature in step 2 was 10 ℃.
4. The method for producing trimethyl orthoacetate by differential loop continuous production according to claim 1, wherein: and in the step 3, the pH value of the reaction system is adjusted to be 5-7.
5. The method for producing trimethyl orthoacetate by differential loop continuous production according to claim 1, wherein: the reaction temperature in step 4 was 40 ℃.
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| CN114605234A (en) * | 2020-12-09 | 2022-06-10 | 南通天泽化工有限公司 | Preparation method of trimethyl orthoacetate |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1583701A (en) * | 2003-08-18 | 2005-02-23 | 顾利华 | Environmental protection cleaning process for preparing high-purity ortho-acetate |
| CN101565360A (en) * | 2008-04-21 | 2009-10-28 | 南通天泽化工有限公司 | Trimethyl orthoacetate and synthetic method thereof |
| CN102060678A (en) * | 2010-12-27 | 2011-05-18 | 江苏优士化学有限公司 | Synthesis process of trimethyl orthoacetate |
| CN102924244A (en) * | 2012-11-02 | 2013-02-13 | 南通天泽化工有限公司 | Production technique of high-quality trimethyl orthoacetate |
| CN103787847A (en) * | 2014-02-12 | 2014-05-14 | 南京大学 | Technology for continuously preparing trimethyl orthoacetate by using ionic liquid as solvent |
| CN106699522A (en) * | 2015-11-16 | 2017-05-24 | 青岛森美克化工技术有限公司 | Production process of high-quality trimethyl orthoacetate |
| CN108203368A (en) * | 2016-12-20 | 2018-06-26 | 青岛祥智电子技术有限公司 | A kind of production technology of high-quality trimethyl orthoacetate |
| CN109134231A (en) * | 2018-10-30 | 2019-01-04 | 杭州众立化工科技有限公司 | A kind of chloroacetic device and process of differential circulation continuous production |
| CN109912395A (en) * | 2019-04-04 | 2019-06-21 | 杭州众立化工科技有限公司 | A kind of device and process of differential circulation continuous production dichloro pinacolone |
-
2020
- 2020-06-09 CN CN202010519175.9A patent/CN111675607A/en active Pending
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1583701A (en) * | 2003-08-18 | 2005-02-23 | 顾利华 | Environmental protection cleaning process for preparing high-purity ortho-acetate |
| CN101565360A (en) * | 2008-04-21 | 2009-10-28 | 南通天泽化工有限公司 | Trimethyl orthoacetate and synthetic method thereof |
| CN102060678A (en) * | 2010-12-27 | 2011-05-18 | 江苏优士化学有限公司 | Synthesis process of trimethyl orthoacetate |
| CN102924244A (en) * | 2012-11-02 | 2013-02-13 | 南通天泽化工有限公司 | Production technique of high-quality trimethyl orthoacetate |
| CN103787847A (en) * | 2014-02-12 | 2014-05-14 | 南京大学 | Technology for continuously preparing trimethyl orthoacetate by using ionic liquid as solvent |
| CN106699522A (en) * | 2015-11-16 | 2017-05-24 | 青岛森美克化工技术有限公司 | Production process of high-quality trimethyl orthoacetate |
| CN108203368A (en) * | 2016-12-20 | 2018-06-26 | 青岛祥智电子技术有限公司 | A kind of production technology of high-quality trimethyl orthoacetate |
| CN109134231A (en) * | 2018-10-30 | 2019-01-04 | 杭州众立化工科技有限公司 | A kind of chloroacetic device and process of differential circulation continuous production |
| CN109912395A (en) * | 2019-04-04 | 2019-06-21 | 杭州众立化工科技有限公司 | A kind of device and process of differential circulation continuous production dichloro pinacolone |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114605234A (en) * | 2020-12-09 | 2022-06-10 | 南通天泽化工有限公司 | Preparation method of trimethyl orthoacetate |
| CN114605234B (en) * | 2020-12-09 | 2023-12-26 | 南通天泽化工有限公司 | Preparation method of trimethyl orthoacetate |
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