Hydrolyzation separation apparatus for methyl acetate and technique

A methyl acetate and separation device technology, which is applied in the production of bulk chemicals, the preparation of organic compounds, and chemical recovery, can solve the problems of low hydrolysis rate of methyl acetate, high energy consumption and equipment investment, and low thermodynamic efficiency. Achieve the effect of saving separation equipment and cold exchange equipment, saving equipment investment and operating costs, and high thermodynamic efficiency

Inactive Publication Date: 2008-08-20
CHINA UNIV OF PETROLEUM (EAST CHINA)
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The shortcoming of fixed-bed cationic exchange resin catalytic hydrolysis process is: the hydrolysis rate of methyl acetate is low, when the molar ratio of water and methyl acetate is 1: 1, only reaches 23%~25%; Multiple azeotropic systems, the separation process is complicated; a large amount of unhydrolyzed methyl acetate needs to be recycled, coupled with the complicated separation process, resulting in large equipment investment and high energy consumption for separation
However, there are still some defects in this technology: as the above-mentioned patents generally operate with full reflux at the top of the tower, in order to achieve sufficient hydrolysis rate, it must be operated under the conditions of high water-ester ratio and high reflux flow, and the energy consumption is large; Both methanol and water are drawn from the bottom of the tower, and cannot be effectively separated. After the reactive distillation tower, a series of rectification towers must be used to further separate the reaction products, and intermediate components in the general rectification process will appear. The remixing phenomenon of methanol has a low thermodynamic efficiency; in addition, the acetic acid and methanol in the bottom of the reactive distillation tower and the extraction pump at the bottom of the tower and its pipeline are prone to reverse reactions to form methyl acetate, thereby reducing the hydrolysis rate
These factors all lead to the decrease of its hydrolysis rate, the consequences of high energy consumption and equipment investment, which are not conducive to improving economic benefits

Method used

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  • Hydrolyzation separation apparatus for methyl acetate and technique
  • Hydrolyzation separation apparatus for methyl acetate and technique
  • Hydrolyzation separation apparatus for methyl acetate and technique

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Embodiment 1: As shown in Figure 2, there is no tower top recycle stream flow. The feed flow rate and composition are shown in Table 1, and the molar ratio of water to ester is 3:1. The feeding position of methyl acetate (counting from top to bottom, the same below) is the 17th theoretical plate on the left, and the water feeding position is the 6th theoretical plate on the left. Both feeds are saturated liquid phase (the same below). The output at the top of the tower is 450kg / h, and its reflux ratio is 4.7. The output at the top of the methanol separation zone (4) is 310kg / h, and its reflux ratio is 1.1. 1. The temperature in the reaction zone (2) is about 60.4°C, and the temperature in the tower kettle is about 100.5°C. The one-way hydrolysis rate of the obtained methyl acetate was 50.8%. The number of theoretical plates in the common stripping area 5 includes the reboiler, the same below.

[0016] Table 1 The number of theoretical board...

Embodiment 2

[0018] Embodiment 2: As shown in Fig. 2, there is no tower top recycle stream flow. Feed, feed position and the number of theoretical plates in each area are the same as in Example 1, except that the water-ester mol ratio becomes 6: 1, the output at the top of the tower is 310kg / h, and its reflux ratio is 7.7. The methanol separation zone (4) The output at the top is 415kg / h, and its reflux ratio is 1.5. The flow rate and composition of each stream are shown in Table 2. The temperature of the reaction zone (2) is about 63° C., the temperature of the tower kettle is about 100.5° C., and the single-pass hydrolysis rate of the obtained methyl acetate is 74.9%.

[0019] Table 2 The mass fraction of each stream flow and each component of embodiment 2

[0020]

[0021] Lateral extraction

Embodiment 3

[0022] Embodiment 3: As shown in Figure 2, there is no tower top recycle stream flow. The feed is pure methyl acetate, its flow rate and composition are shown in Table 3, and the molar ratio of water to ester is 6:1. Feeding position and the number of theoretical plates in each area are the same as in Example 1. The output at the top of the tower is 230kg / h, and its reflux ratio is 8.0, and the output at the top of the methanol separation zone (4) is 225kg / h, and its reflux ratio is 1.4. The flow rate and composition of each stream are shown in Table 3. The temperature in the reaction zone (2) is about 62.8°C, and the temperature in the tower kettle is about 100.6°C. The one-way hydrolysis rate of the obtained methyl acetate was 74.9%.

[0023] Table 3 The mass fraction of each stream flow and each component of embodiment 3

[0024]

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Abstract

The invention provides a hydrolyzing and separation device of methyl acetate and a technique method thereof, which more particularly relates to a novel technique to catalyze and hydrolyze methyl acetate by a reaction bulkhead distillation tower, which can organically combine reaction process, product separation and recovery of no reactant into the tower. A separator extending from the upper part of the tower to the lower part of the tower is arranged on the vertical direction in the conventional distillation tower, the upper part of one side of which is covered and the other side of which is filled with a catalyst; therefore, the inner space of the reaction bulkhead distillation tower is divided into five regions with different functions. The hydrolyzing and separation device of methyl acetate can fully unleash the advantage of bulkhead tower and reaction distillation, and can cause hydrolysis reaction, product separation and recovery of non reactant to be realized in the same tower. The device provided by the invention and the technique process thereof can obtain the methyl acetate with 60 percent to 99.99 percent hydrolysis rate and products with high purity, restrain side effect effectively, reduce the volume of equipment markedly, simplify process, and reduce energy consumption and operation cost.

Description

technical field [0001] The invention relates to a chemical reaction separation device and process, in particular to an equipment and process for catalytic hydrolysis of methyl acetate by using a reactive distillation partition tower, which can combine the hydrolysis reaction of methyl acetate and the separation of its products in one tower completed. Background technique [0002] Methyl acetate is a by-product in the production process of polyvinyl alcohol. At present, all PVA manufacturers hydrolyze methyl acetate into acetic acid and methanol for recycling. The current methyl acetate hydrolysis process at home and abroad mainly adopts fixed bed cation exchange resin catalytic hydrolysis process and reactive distillation hydrolysis process. [0003] The shortcoming of fixed-bed cationic exchange resin catalytic hydrolysis process is: the hydrolysis rate of methyl acetate is low, when the molar ratio of water and methyl acetate is 1: 1, only reaches 23%~25%; With multiple ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C27/02C07C31/04C07C53/08
CPCY02P20/52Y02P20/584
Inventor 孙兰义李军杨德连刘立新
Owner CHINA UNIV OF PETROLEUM (EAST CHINA)
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