IP Library › Granted Patent US 7,342,130
Granted Patent B2
US 7,342,130 · App. 11/634,133 · Granted Mar 11, 2008

Method for producing acrylic acid

Assignee: Nippon Shokubai Co., Ltd.
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Quick Facts
Patent No.
US 7,342,130
App. No.
11/634,133
Granted
Mar 11, 2008
Kind
B2
Abstract

A method for producing acrylic acid, comprising (a) a absorption step of absorbing acrylic acid-containing gas obtained by oxidizing raw material gas in gas phase as crude acrylic acid-containing solution, (b 1 ) a step of separating high boiling point components that separates the crude high boiling point components at a distillation column as (b) a step of purifying the acrylic acid-containing solution, and further, (c) a decomposition step of decomposing Michael adducts contained in the high boiling point components to prepare acrylic acid and (d) a collection step of collecting acrylic acid generated in the decomposition step (c), whereby the proportion of the amount of maleic acid to a sum of the sum of the maleic acid and maleic anhydride in the high boiling point components that are fed from the high boiling point component separation step (b 1 ) to the decomposition step (c) satisfies a equation below: [ Equation ⁢ ⁢ 1 ] ⁢ ` [ Maleic ⁢ ⁢ acid ⁢ ⁢ ( mass ) ] [ Maleic ⁢ ⁢ acid ⁢ ⁢ ( mass ) ] + [ Maleic ⁢ ⁢ anhydride ⁡ ( mass ) ] × 100 ≦ 70 ⁢ ⁢ % ⁢ . ( 1 )

Claims (61)

1. A method for producing acrylic acid, comprising

(a) an absorption step of absorbing an acrylic acid-containing gas obtained by oxidizing a raw material gas in gas phase as a crude acrylic acid-containing solution;

(b 1 ) a high boiling point component separation step of separating high boiling point components at a distillation column as (b) a step of purifying the crude acrylic acid-containing solution;

(c) a decomposition step of decomposing Michael adducts contained in the high boiling point components to generate acrylic acid; and

(d) a collection step of collecting the acrylic acid generated in the decomposition step (c), wherein a column bottom of the distillation column at the high boiling point component separation step (b 1 ) has a temperature of 90 to 130° C., a residence time of a column bottom solution is 2 to 30 hours, and a ratio of a mass of solution fed to the distillation column to a mass of extraction solution from the column bottom of the distillation column is 5 to 20, and

a proportion of an amount of maleic acid to a sum of maleic acid and maleic anhydride in the high boiling point components fed from the high boiling point component separation step (b 1 ) to the decomposition step (c) satisfies equation (1) below:

[

Maleic

⁢

⁢

acid

⁢

⁢

(

mass

)

]

[

Maleic

⁢

⁢

acid

⁢

⁢

(

mass

)

]

+

[

Maleic

⁢

⁢

anhydride

⁢

⁢

(

mass

)

]

×

100

≦

70

⁢

%

.

(

1

)

2. A method for producing acrylic acid according to claim 1 , further comprising (b 2 ) a crystallization purification step of separating crystals obtained by crystallizing acrylic acid in the crude acrylic acid-containing solution from residual mother liquid as an additional step of purifying the acrylic acid-containing solution (b), wherein at least one portion of the residual mother liquid obtained in the crystallization purification step (b 2 ) is fed to the high boiling point component separation step (b 1 ).

3. A method for producing acrylic acid according to claim 2 , wherein a column bottom solution obtained in the high boiling point component separation step (b 1 ) is fed to the decomposition step (c), a portion of a distillate obtained in the decomposition step (c) is fed to the high boiling point component separation step (b 1 ), and a distillate obtained in the high boiling point component separation step (b 1 ) and/or the distillate obtained in the decomposition step (c) are fed to the absorption step (a).

4. A method for producing acrylic acid according to claim 1 , wherein a concentration of the Michael adducts in the high boiling point components fed to the decomposition step (c) is 20 to 60% by mass.

5. A method for producing acrylic acid according to claim 1 , wherein the decomposition step (c) is carried out by a reaction-distillation process.

6. A method for producing acrylic acid according to claim 5 , wherein the decomposition step (c) according to the reaction-distillation process is carried out at a reflux ratio of 0.5 to 6 using a shelf plate distillation column.

7. A method for producing acrylic acid according to claim 6 , wherein the shelf plate distillation column has 3 or more of theoretical stages, and the position of 70 to 100% of total theoretical stages setting a column top side of the shelf plate distillation column as a base point is heated at 125° C. or less.

8. A method for producing acrylic acid according to claim 6 , wherein the shelf plate distillation column is equipped with a tray having opening with a hole diameter of 10 to 50 mm.

9. A method for producing acrylic acid according to claim 1 , wherein the decomposition step (c) uses a forced circulation type heat exchanger, heats the high boiling point components fed to the decomposition step (c) to 155 to 220° C., and controls temperature difference between a heat source of the forced circulation type heat exchanger and the high boiling point components heated by the forced circulation type heat exchanger at 15 to 80° C.

10. A method for producing acrylic acid according to claim 1 , whereby the decomposition step (c) is carried out in a presence of an N-oxyl compound.

11. A method for producing acrylic acid according to claim 1 , wherein all of a distillate obtained in the decomposition step (c) is fed to the high boiling point component separation step (b 1 ) and fed to the absorption step (a) through the high boiling point component separation step (b 1 ).

12. A method for producing acrylic acid according to claim 11 , wherein a concentration of maleic acid in the distillate fed to the absorption step (a) is 2% by mass or less.

Assignments (1)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Dec 6, 2006
From: SHIBUSAWA, FUMIO; ISHIKAWA, MASARU
To: NIPPON SHOKUBAI CO., LTD.
Reel/Frame 018649/0645 →
Priority Claims (2)
JP 2005-352719 · Dec 6, 2005 · national
JP 2006-189542 · Jul 10, 2006 · national
Continuity (1)
Related Publication 20070129572A1 · Jun 7, 2007