阅读说明：本技术 一种3-甲氧基丙烯酸甲酯制备系统 (3-methoxy methyl acrylate preparation system ) 是由 不公告发明人 于 2020-06-22 设计创作，主要内容包括：本发明的一种3-甲氧基丙烯酸甲酯的制备系统,包括存储有乙酸甲酯和甲醇钠混合溶液的反应釜、蒸馏釜一、蒸馏釜二、滴液机构、输气机构、储气机构、测压机构,加热机构；反应釜内设有进气口,该进气口连通有输气机构,进气口内还设有测压机构,输气机构与储气机构连通；蒸馏釜一顶部设有滴液机构,该滴液机构用于滴加浓度10％的氯化氢甲醇溶液；蒸馏釜一与蒸馏釜二之间设有离心机构,蒸馏釜一反应后的料液通过离心机构离心后进入蒸馏釜二,蒸馏釜二顶部设有开口连通有抽气泵；反应釜底部、蒸馏釜一的底部和蒸馏釜二的底部均设有加热机构；乙酸甲酯和甲醇钠混合溶液中,乙酸甲酯与甲醇钠的摩尔比为1：1～20：1。(The invention relates to a preparation system of 3-methoxy methyl acrylate, which comprises a reaction kettle, a first distillation kettle, a second distillation kettle, a liquid dropping mechanism, a gas transmission mechanism, a gas storage mechanism, a pressure measuring mechanism and a heating mechanism, wherein the reaction kettle is used for storing a mixed solution of methyl acetate and sodium methoxide; an air inlet is arranged in the reaction kettle and is communicated with an air conveying mechanism, a pressure measuring mechanism is also arranged in the air inlet, and the air conveying mechanism is communicated with an air storage mechanism; a liquid dropping mechanism is arranged at the top of the distillation still and is used for dropping a hydrogen chloride methanol solution with the concentration of 10 percent; a centrifugal mechanism is arranged between the first distillation kettle and the second distillation kettle, the feed liquid after reaction in the first distillation kettle enters the second distillation kettle after being centrifuged by the centrifugal mechanism, and the top of the second distillation kettle is provided with an opening communicated with an air extracting pump; heating mechanisms are arranged at the bottom of the reaction kettle, the bottom of the first distillation kettle and the bottom of the second distillation kettle; in the mixed solution of methyl acetate and sodium methoxide, the molar ratio of methyl acetate to sodium methoxide is 1: 1-20: 1.)

1. A preparation system of methyl 3-methoxyacrylate is characterized in that: the device comprises a reaction kettle for storing a mixed solution of methyl acetate and sodium methoxide, a first distillation kettle, a second distillation kettle, a liquid dropping mechanism, a gas transmission mechanism, a gas storage mechanism, a pressure measuring mechanism and a heating mechanism;

an air inlet is arranged in the reaction kettle and is communicated with an air conveying mechanism, a pressure measuring mechanism is also arranged in the air inlet, and the air conveying mechanism is communicated with an air storage mechanism;

a discharge hole in the reaction kettle is communicated with a feed hole of the first distillation kettle, the feed liquid is conveyed to the first distillation kettle after the reaction of the raw materials in the reaction kettle is finished, and a liquid dropping mechanism is arranged at the top of the first distillation kettle and is used for dropping a hydrogen chloride methanol solution with the concentration of 10%;

a centrifugal mechanism is arranged between the first distillation kettle and the second distillation kettle, feed liquid after reaction in the first distillation kettle enters the second distillation kettle after being centrifuged by the centrifugal mechanism, and an opening communicated with an air pump is formed in the top of the second distillation kettle;

heating mechanisms are arranged at the bottom of the reaction kettle, the bottom of the first distillation kettle and the bottom of the second distillation kettle;

in the mixed solution of methyl acetate and sodium methoxide, the molar ratio of methyl acetate to sodium methoxide is 1: 1-20: 1.

2. the production system of methyl 3-methoxyacrylate according to claim 1, wherein: carbon monoxide is stored in the gas storage mechanism, and the air pressure of the carbon monoxide in the reaction kettle is 2-4 Mpa.

3. The production system of methyl 3-methoxyacrylate according to claim 1, wherein: the heating temperature of the heating mechanism at the bottom of the reaction kettle is 40-70 ℃, the heating temperature of the heating mechanism at the bottom of the first distillation kettle is 60-80 ℃, and the heating temperature of the heating mechanism at the bottom of the second distillation kettle is 120-150 ℃.

4. The production system of methyl 3-methoxyacrylate according to claim 1, wherein: and the first distillation kettle is used for distilling the feed liquid, evaporating and removing excessive methyl acetate in the feed liquid, and dropwise adding the methyl acetate through a dropping mechanism after the removal is finished.

5. The production system of methyl 3-methoxyacrylate according to claim 1, wherein: the molar ratio of hydrogen chloride in the hydrogen chloride methanol solution stored in the dropping mechanism to sodium methoxide stored in the reaction kettle is 1: 1-2: 1.

6. the production system of methyl 3-methoxyacrylate according to claim 1, wherein: be equipped with the velocity of flow governing valve in the dropping liquid mechanism, this velocity of flow governing valve is used for controlling the dropwise add speed of dropping liquid mechanism.

7. The production system of methyl 3-methoxyacrylate according to claim 1, wherein: the gas transmission mechanism is communicated with a gas inlet in the reaction kettle through a gas transmission pipe, and a one-way gas valve is arranged in the gas transmission pipe.

8. The production system of methyl 3-methoxyacrylate according to claim 1, wherein: and a movable storage bin is arranged in the second distillation kettle, and a catalyst is arranged in the storage bin and is p-toluenesulfonic acid, sodium bisulfate or potassium bisulfate.

9. The method for operating a system for producing methyl 3-methoxyacrylate according to any one of claims 1 to 8, wherein: introducing carbon monoxide into the reaction kettle through a gas conveying mechanism, controlling the pressure of the carbon monoxide in the reaction kettle to be 2-4 Mpa, opening a heating mechanism at the bottom of the reaction kettle to heat, controlling the heating temperature to be 40-70 ℃, conveying feed liquid in the reaction kettle into a first distillation kettle after the reaction is finished, opening a heating mechanism at the bottom of the first distillation kettle to heat, evaporating and removing methyl acetate in the first distillation kettle, dropwise adding 10% hydrogen chloride methanol solution through a dropping mechanism to react, adjusting the pH value after the reaction is finished, centrifuging through a centrifugal mechanism, conveying the centrifuged feed liquid into a second distillation kettle, opening a heating mechanism at the bottom of the second distillation kettle to heat and concentrate to obtain 3, 3-dimethoxy methyl propionate, moving a storage bin to enable a catalyst in the storage bin to be in contact with the 3, 3-dimethoxy methyl propionate, and controlling the heating mechanism at the bottom of the second distillation kettle to be heated to 120-150 ℃ to carry out cracking reaction, and opening an air pump to perform reduced pressure distillation after cracking is finished to obtain the 3-methoxy methyl acrylate.

10. The method according to claim 9, wherein the operation of the system for producing methyl 3-methoxyacrylate comprises: the distillation temperature of the reduced pressure distillation is 60-80 ℃, and the distillation time is 7-8 h.

Technical Field

The invention belongs to the technical field of chemical processes, and particularly relates to a preparation system of 3-methoxy methyl acrylate.

Background

The 3-methoxy Methyl Acrylate (MAME) is colorless transparent liquid, is a multifunctional compound, has good reaction activity, is an important C-3 building block in organic synthesis, is widely applied to the fields of pesticides, medicines, high polymer materials and the like, is used for synthesizing various organic compounds, has wide application and large demand, but has less domestic industrialization and depends on import.

The currently reported synthesis methods of MAME include the following: 1) wacker catalytic oxidation: the method is simple and efficient, but the catalyst is expensive and difficult to recycle, and chloride generates corrosive equipment; 2) methyl propiolate method: methyl propiolate and ethanol are catalyzed by sodium cyanide or potassium carbonate to synthesize 3, 3-diethoxypropionate, the catalytic yield of the sodium cyanide is 75 percent, the catalytic yield of the potassium carbonate is 70 percent, the process is mature, but the cost of the propiolic acid is high, the yield is not high, and the sodium cyanide is highly toxic; 3) trimethyl orthoformate and vinyl ketone process: ketene and trimethyl orthoformate are catalyzed by montmorillonite or boron trifluoride ether to prepare 3, 3-dimethoxy methyl propionate, and then are catalyzed by p-toluenesulfonic acid or similar substances to prepare 3-methoxy methyl acrylate by cracking, wherein the reaction yield is not high and is 52%, and the reaction process is violent in heat release; 4) carbon tetrachloride process: the method is characterized in that 1, 1, 1, 3-tetrachloro-3-ethoxypropane is synthesized by using carbon tetrachloride and vinyl ethyl ether as raw materials, a propane compound and methanol are refluxed and esterified to prepare 3, 3-dimethoxy methyl propionate, and then the 3-methoxy methyl acrylate is synthesized through cracking, and the yield of a target product is low.

Through search, the Chinese invention has the patent names: a preparation technology of 3-methoxy methyl acrylate (application No. CN201711263170.9, application No. 2018.04.06) comprises the steps of taking methyl acrylate and excessive methanol as initial raw materials, carrying out addition etherification reaction in an oxygen atmosphere under the action of a synthesis catalyst, filtering and extracting a product to obtain 3, 3-dimethoxy methyl propionate, carrying out catalytic cracking reaction on the 3, 3-dimethoxy methyl propionate to generate 3-methoxy methyl acrylate and methanol, rectifying to obtain a target product of 3-methoxy Methyl Acrylate (MAME), and recovering the methanol; the synthetic catalyst is cobalt oxide, indium oxide or a mixture of the cobalt oxide and the indium oxide in any proportion. The preparation process of the scheme is simple and efficient, but the scheme has the defect that excessive solvents are introduced, so that the separation and purification of the prepared methyl 3-methoxyacrylate are complex.

Disclosure of Invention

1. Technical problem to be solved by the invention

The invention aims to solve the problems of complex preparation process, high cost and low yield of the existing 3-methoxy methyl acrylate.

2. Technical scheme

In order to achieve the purpose, the technical scheme provided by the invention is as follows:

the invention relates to a preparation system of 3-methoxy methyl acrylate, which comprises a reaction kettle, a first distillation kettle, a second distillation kettle, a liquid dropping mechanism, a gas transmission mechanism, a gas storage mechanism, a pressure measuring mechanism and a heating mechanism, wherein the reaction kettle is used for storing a mixed solution of methyl acetate and sodium methoxide;

an air inlet is arranged in the reaction kettle and is communicated with an air conveying mechanism, a pressure measuring mechanism is also arranged in the air inlet, and the air conveying mechanism is communicated with an air storage mechanism;

a discharge hole in the reaction kettle is communicated with a feed hole of the first distillation kettle, the feed liquid is conveyed to the first distillation kettle after the reaction of the raw materials in the reaction kettle is finished, and a liquid dropping mechanism is arranged at the top of the first distillation kettle and is used for dropping a hydrogen chloride methanol solution with the concentration of 10%;

a centrifugal mechanism is arranged between the first distillation kettle and the second distillation kettle, feed liquid after reaction in the first distillation kettle enters the second distillation kettle after being centrifuged by the centrifugal mechanism, and an opening communicated with an air pump is formed in the top of the second distillation kettle;

heating mechanisms are arranged at the bottom of the reaction kettle, the bottom of the first distillation kettle and the bottom of the second distillation kettle;

in the mixed solution of methyl acetate and sodium methoxide, the molar ratio of methyl acetate to sodium methoxide is 1: 1-20: 1.

preferably, carbon monoxide is stored in the gas storage mechanism, and the pressure of the carbon monoxide in the reaction kettle is 2-4 Mpa.

Preferably, the heating temperature of the heating mechanism at the bottom of the reaction kettle is 40-70 ℃, the heating temperature of the heating mechanism at the bottom of the first distillation kettle is 60-80 ℃, and the heating temperature of the heating mechanism at the bottom of the second distillation kettle is 120-150 ℃.

Preferably, the first distillation kettle is used for distilling the feed liquid, evaporating and removing excessive methyl acetate in the feed liquid, and dropwise adding the methyl acetate through a dropping mechanism after the methyl acetate is removed.

Preferably, the molar ratio of hydrogen chloride in the hydrogen chloride methanol solution stored in the dropping mechanism to sodium methoxide stored in the reaction kettle is 1: 1-2: 1.

preferably, a flow rate regulating valve is arranged in the liquid dropping mechanism and used for controlling the dropping speed of the liquid dropping mechanism.

Preferably, the gas transmission mechanism is communicated with a gas inlet in the reaction kettle through a gas transmission pipe, and a one-way gas valve is arranged in the gas transmission pipe.

Preferably, a movable storage bin is arranged in the second distillation kettle, a catalyst is arranged in the storage bin, and the catalyst is p-toluenesulfonic acid, sodium bisulfate or potassium bisulfate.

An operation method of a preparation system of 3-methoxy methyl acrylate comprises the steps of introducing carbon monoxide into a reaction kettle through a gas conveying mechanism, controlling the pressure of the carbon monoxide in the reaction kettle to be 2-4 Mpa, opening a heating mechanism at the bottom of the reaction kettle to heat, controlling the heating temperature to be 40-70 ℃, conveying feed liquid in the reaction kettle into a first distillation kettle after reaction is finished, opening the heating mechanism at the bottom of the first distillation kettle to heat, evaporating and removing methyl acetate in the first distillation kettle, dropwise adding a hydrogen chloride methanol solution with the concentration of 10% through a liquid dropping mechanism to react, adjusting the pH value after reaction is finished, centrifuging through a centrifugal mechanism, conveying the centrifuged feed liquid into a second distillation kettle, opening a heating mechanism at the bottom of the second distillation kettle to heat and concentrate to obtain 3, 3-dimethoxy methyl propionate, moving a storage bin to enable a catalyst in the storage bin to be 3, and 3-dimethoxy methyl propionate is contacted with and controls a heating mechanism at the bottom of the second distillation kettle to be heated to 120-150 ℃ for cracking reaction, and after cracking is finished, an air pump is opened for reduced pressure distillation to obtain the 3-methoxy methyl acrylate.

Preferably, the distillation temperature of the reduced pressure distillation is 60-80 ℃, and the distillation time is 7-8 h.

3. Advantageous effects

Compared with the prior art, the technical scheme provided by the invention has the following beneficial effects:

the invention relates to a preparation system of 3-methoxy methyl acrylate, which comprises a reaction kettle, a first distillation kettle, a second distillation kettle, a liquid dropping mechanism, a gas transmission mechanism, a gas storage mechanism, a pressure measuring mechanism and a heating mechanism, wherein the reaction kettle is used for storing a mixed solution of methyl acetate and sodium methoxide; an air inlet is arranged in the reaction kettle and is communicated with an air conveying mechanism, a pressure measuring mechanism is also arranged in the air inlet, and the air conveying mechanism is communicated with an air storage mechanism; a discharge hole in the reaction kettle is communicated with a feed hole of the first distillation kettle, the feed liquid is conveyed to the first distillation kettle after the reaction of the raw materials in the reaction kettle is finished, and a liquid dropping mechanism is arranged at the top of the first distillation kettle and is used for dropping a hydrogen chloride methanol solution with the concentration of 10%; a centrifugal mechanism is arranged between the first distillation kettle and the second distillation kettle, feed liquid after reaction in the first distillation kettle enters the second distillation kettle after being centrifuged by the centrifugal mechanism, and an opening communicated with an air pump is formed in the top of the second distillation kettle; heating mechanisms are arranged at the bottom of the reaction kettle, the bottom of the first distillation kettle and the bottom of the second distillation kettle; in the mixed solution of methyl acetate and sodium methoxide, the molar ratio of methyl acetate to sodium methoxide is 1: 1-20: 1. under the action of strong base sodium alkoxide in the reaction kettle, alpha carbon on methyl acetate forms carbanion, then is combined with carbon monoxide, and forms enol sodium salt after rearrangement, the enol sodium salt and methanol respectively generate addition and substitution reaction in the presence of hydrogen chloride to generate 3, 3-dimethoxy methyl propionate, and then a catalyst is added for cracking reaction to obtain the 3-methoxy methyl acrylate.

Drawings

FIG. 1 is a flow chart showing the method of operating a system for producing methyl 3-methoxyacrylate according to the present invention.

Detailed Description

In order to facilitate an understanding of the invention, the invention will now be described more fully hereinafter with reference to the accompanying drawings, in which several embodiments of the invention are shown, but which may be embodied in many different forms and are not limited to the embodiments described herein, but rather are provided for the purpose of providing a more thorough disclosure of the invention.

It will be understood that when an element is referred to as being "secured to" another element, it can be directly on the other element or intervening elements may also be present; when an element is referred to as being "connected" to another element, it can be directly connected to the other element or intervening elements may also be present; the terms "vertical," "horizontal," "left," "right," and the like as used herein are for illustrative purposes only.

Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs; the terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention; as used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.

Example 1

Referring to the attached drawing 1, the system for preparing 3-methoxy methyl acrylate of the embodiment includes a reaction kettle storing a mixed solution of methyl acetate and sodium methoxide, a first distillation kettle, a second distillation kettle, a liquid dropping mechanism, a gas transmission mechanism, a gas storage mechanism, a pressure measuring mechanism and a heating mechanism;

an air inlet is arranged in the reaction kettle and is communicated with an air conveying mechanism, a pressure measuring mechanism is also arranged in the air inlet, and the air conveying mechanism is communicated with an air storage mechanism;

a discharge hole in the reaction kettle is communicated with a feed hole of the first distillation kettle, the feed liquid is conveyed to the first distillation kettle after the reaction of the raw materials in the reaction kettle is finished, and a liquid dropping mechanism is arranged at the top of the first distillation kettle and is used for dropping a hydrogen chloride methanol solution with the concentration of 10%;

a centrifugal mechanism is arranged between the first distillation kettle and the second distillation kettle, feed liquid after reaction in the first distillation kettle enters the second distillation kettle after being centrifuged by the centrifugal mechanism, and an opening communicated with an air pump is formed in the top of the second distillation kettle;

heating mechanisms are arranged at the bottom of the reaction kettle, the bottom of the first distillation kettle and the bottom of the second distillation kettle;

in the mixed solution of methyl acetate and sodium methoxide, the molar ratio of methyl acetate to sodium methoxide is 1: 1-20: 1.

under the action of strong base sodium alkoxide, alpha carbon on methyl acetate forms carbanion, then is combined with carbon monoxide, and forms enol sodium salt after rearrangement, the enol sodium salt and methanol respectively generate addition and substitution reaction in the presence of hydrogen chloride to generate 3, 3-dimethoxy methyl propionate, and then a catalyst is added for cracking reaction to obtain the 3-methoxy methyl acrylate.

Specifically, carbon monoxide is stored in the gas storage mechanism, and the air pressure of the carbon monoxide in the reaction kettle is 2-4 Mpa.

Specifically, the heating temperature of the heating mechanism at the bottom of the reaction kettle is 40-70 ℃, the heating temperature of the heating mechanism at the bottom of the first distillation kettle is 60-80 ℃, and the heating temperature of the heating mechanism at the bottom of the second distillation kettle is 120-150 ℃.

Specifically, the first distillation kettle is used for distilling the feed liquid, evaporating and removing excessive methyl acetate in the feed liquid, and then dropwise adding the methyl acetate through a dropping mechanism after the methyl acetate is removed.

Specifically, the molar ratio of hydrogen chloride in the hydrogen chloride methanol solution stored in the dropping mechanism to sodium methoxide stored in the reaction kettle is 1: 1-2: 1.

specifically, be equipped with the velocity of flow governing valve in the dropping liquid mechanism, this velocity of flow governing valve is used for controlling dropping liquid mechanism's dropwise add speed.

Specifically, the gas transmission mechanism is communicated with a gas inlet in the reaction kettle through a gas transmission pipe, and a one-way gas valve is arranged in the gas transmission pipe.

Specifically, a movable storage bin is arranged in the second distillation kettle, a catalyst is arranged in the storage bin, and the catalyst is p-toluenesulfonic acid, sodium bisulfate or potassium bisulfate.

An operation method of a preparation system of 3-methoxy methyl acrylate comprises the steps of introducing carbon monoxide into a reaction kettle through a gas conveying mechanism, controlling the pressure of the carbon monoxide in the reaction kettle to be 2-4 Mpa, opening a heating mechanism at the bottom of the reaction kettle to heat, controlling the heating temperature to be 40-70 ℃, conveying feed liquid in the reaction kettle into a first distillation kettle after reaction is finished, opening the heating mechanism at the bottom of the first distillation kettle to heat, evaporating and removing methyl acetate in the first distillation kettle, dropwise adding a hydrogen chloride methanol solution with the concentration of 10% through a liquid dropping mechanism to react, adjusting the pH value after reaction is finished, centrifuging through a centrifugal mechanism, conveying the centrifuged feed liquid into a second distillation kettle, opening a heating mechanism at the bottom of the second distillation kettle to heat and concentrate to obtain 3, 3-dimethoxy methyl propionate, moving a storage bin to enable a catalyst in the storage bin to be 3, and 3-dimethoxy methyl propionate is contacted with and controls a heating mechanism at the bottom of the second distillation kettle to be heated to 120-150 ℃ for cracking reaction, and after cracking is finished, an air pump is opened for reduced pressure distillation to obtain the 3-methoxy methyl acrylate. The distillation temperature of the reduced pressure distillation is 60-80 ℃, and the distillation time is 7-8 h.

The operation method is concretely

S100, mixing materials, namely adding a mixed solution of methyl acetate and sodium methoxide into a reaction kettle;

s200, carrying out primary reaction, namely introducing carbon monoxide into a reaction kettle and then heating to carry out reaction;

s300, primary distillation, namely transferring the feed liquid after the primary reaction to a first distillation kettle for distillation, and evaporating and removing excessive methyl acetate;

s400, performing secondary reaction, namely slowly submitting a hydrogen chloride methanol solution with the concentration of 10% to the feed liquid after primary distillation for secondary reaction;

s500, post-treatment, namely adding a pH value regulator into the feed liquid after the secondary reaction, and regulating the pH value of the feed liquid to 7-8;

s600, secondary distillation, namely heating, distilling and concentrating the feed liquid obtained by post-treatment to obtain 3, 3-dimethoxy methyl propionate;

s700, carrying out cracking reaction, namely adding a catalyst into 3, 3-dimethoxy methyl propionate, and carrying out cracking reaction at the temperature of 120-150 ℃ for 6-8 hours;

and S800, carrying out reduced pressure distillation, and carrying out reduced pressure distillation on the feed liquid obtained in the step S700 to obtain the 3-methoxy methyl acrylate.

The above-mentioned embodiments only express a certain implementation mode of the present invention, and the description thereof is specific and detailed, but not construed as limiting the scope of the present invention; it should be noted that, for those skilled in the art, without departing from the concept of the present invention, several variations and modifications can be made, which are within the protection scope of the present invention; therefore, the protection scope of the present patent shall be subject to the appended claims.