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Synthesis method of alkyl (meth) acrylate

A technique for the synthesis of alkyl acrylates, which is applied in the preparation of carboxylic acid esters, chemical instruments and methods, and the preparation of organic compounds, and can solve problems such as reducing the yield of target products and increasing the risk of polymerization tower blockage, and achieves maintenance Low cost, good catalytic effect, and reduced addition by-products

Pending Publication Date: 2021-12-03
ZHEJIANG HUANGMA TECH +3
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are following problems in this synthesis process: one, epoxide passes through in (meth)acrylic acid and reacts, and (meth)acrylic acid is in excessive state relative to epoxide in the early stage of reaction, easily forms two (meth)acrylic acid addition high Two, the homogeneous catalyst needs to be initially removed by vacuum distillation, and the distillation process will still cause the transformation of some by-products to reduce the yield of the target product; three, two high-boiling double (meth)acrylic acid addition Esters increase the risk of polymerization blockage in the subsequent rectification process

Method used

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  • Synthesis method of alkyl (meth) acrylate
  • Synthesis method of alkyl (meth) acrylate
  • Synthesis method of alkyl (meth) acrylate

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preparation example Construction

[0025] A kind of synthetic method of alkyl (meth)acrylate, it specifically comprises the following steps: specifically comprises the steps:

[0026] S1, put the heterogeneous solid acid catalyst, polymerization inhibitor and (meth)acrylic acid into the reactor;

[0027] S2. After raising the temperature to 50-90°C, feed epoxy into the reactor at a flow rate of 1200-1600kg / h for reaction, and the temperature during the reaction should not exceed 90°C;

[0028] S3. After the addition of epoxy oxide is completed, heat and mature at 50°C-90°C for 1-3h, filter the reaction solution to remove the non-homogeneous solid acid catalyst, keep the pressure below 50mTorr, and control the temperature at 70°C-90°C Rectification, that is, the target product.

[0029] Wherein, the heterogeneous solid acid catalyst is composed of a carrier and iron ions and chromium ions loaded on the carrier; the carrier is a layered silicate with a pillar structure, preferably, the layered silicate is select...

Embodiment 1

[0033] 1. Preparation of heterogeneous solid acid catalyst

[0034] Dissolve 4.5kg of chromium acetate and 1kg of ferric chloride in an appropriate amount of deionized water (the molar ratio of chromium ion to iron ion is 3:1), impregnate 16.6kg of montmorillonite and 13.4kg of saponite (average CEC is about 90mmol / 100g) in Sonicate the above solution for 4 hours at 80°C, filter and wash with water until there is no floating color, dry and grind it into powder; place the above powder in the air and calcinate at 550°C for 3 hours to prepare a heterogeneous solid acid catalyst for future use.

[0035] Two, the preparation of hydroxyethyl acrylate

[0036] Specifically include the following steps:

[0037] S1. Feeding and nitrogen placement: Vacuum pump 2500kg of acrylic acid into the reactor, put in 8.4kg of phenothiazine, and 21kg of the prepared heterogeneous solid acid catalyst, and replace the internal air with nitrogen, and the nitrogen pressure is ≥0.02 during replacement...

Embodiment 2

[0062] One, the preparation method of heterogeneous solid acid catalyst is identical with embodiment 1.

[0063] Two, the preparation of hydroxyethyl methacrylate

[0064] Specifically include the following steps:

[0065] S1. Feeding and nitrogen placement: Vacuum pump 3010kg of methacrylic acid into the reactor, put in 8.4kg of phenothiazine, 21kg of the above-mentioned heterogeneous solid acid catalyst, and replace the internal air with nitrogen, and the nitrogen pressure is ≥0.02MPa during replacement , the vacuum degree is pumped to -0.02MPa.

[0066] S2. Response: After the nitrogen setting is completed, close the vacuum valve. Raise the temperature to 50°C, feed 1700kg of ethylene oxide, and slowly raise the temperature to 65-70°C, control the pressure to ≤0.25MPa, and feed the ethylene oxide at a rate of 1200-1600kg / h (subject to the actual pressure).

[0067] S3. Ripening: After the feeding of ethylene oxide is completed, close the discharge valve of the ethylene o...

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Abstract

The invention discloses a synthesis method of alkyl (meth) acrylate, and belongs to the field of organic chemical synthesis. The synthesis method comprises the following steps: putting a heterogeneous solid acid catalyst, a polymerization inhibitor and (methyl) acrylic acid into a reaction kettle, heating to 50-90 DEG C, and introducing epoxide into the reaction kettle for reaction; and after the reaction is finished, preserving heat and curing, filtering reaction liquid to remove the heterogeneous solid acid catalyst, and rectifying to obtain a target product. The synthesis method provided by the invention not only can improve the selectivity of the target product alkyl (meth) acrylate, but also can effectively inhibit the generation of a by-product high-boiling-point diester generated by addition of bis (meth) acrylic acid, effectively ensures the product quality, reduces the material loss caused by polymerization in the subsequent purification process, and reduces the potential safety hazard.

Description

technical field [0001] The invention relates to the technical field of organic chemical synthesis, in particular to a method for synthesizing alkyl (meth)acrylate. Background technique [0002] Alkyl (meth)acrylate, as an organic polymer monomer, can be copolymerized with acrylic acid and esters, acrolein, acrylonitrile, acrylamide, vinyl chloride, styrene and other monomers, and is widely used in fiber processing , coatings, adhesives, rubber and paper and other fields. [0003] At present, the process of using (meth)acrylic acid and epoxides as raw materials to synthesize alkyl (meth)acrylates in a batch reaction system usually uses a homogeneous Lewis acid as a catalyst. The specific process is: first (meth)acrylic acid ) acrylic acid and catalyst are put into the reaction kettle together, and then the epoxide is put into reaction at a certain supply rate; . There are following problems in this synthesis process: one, epoxide passes through in (meth)acrylic acid and re...

Claims

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Application Information

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IPC IPC(8): C07C67/26C07C69/653B01J23/86
CPCC07C67/26B01J23/862C07C69/653Y02P20/584
Inventor 房凯王伟松万庆梅郑斌赵兴军
Owner ZHEJIANG HUANGMA TECH
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