Method for purifying methacrylic acid and method for producing methacrylic acid

Patent metadata

Field	Value
Publication number	US-10442747-B2
Application number	US-201816155027-A
Country	US
Kind code	B2
Filing date	Oct 9, 2018
Priority date	Apr 28, 2016
Publication date	Oct 15, 2019
Grant date	Oct 15, 2019

Abstract

A method for purifying methacrylic acid, including mixing raw material methacrylic acid and methanol; precipitating a crystal of methacrylic acid from the mixed solution; and separating the crystal and mother liquor, wherein the raw material methacrylic acid and methanol are mixed so that a concentration of methanol in the mixed liquid is 3.0 to 3.75% by mass, and the crystal of methacrylic acid is precipitated from the mixed solution in a cooling crystallization vessel.

First claim

The invention claimed is:

1. A method for purifying methacrylic acid, comprising:
mixing raw material methacrylic acid having a purity of 99.00% by mass or more and methanol;
precipitating a crystal of methacrylic acid from a mixed solution comprising the raw material methacrylic acid and methanol; and
separating the crystal and mother liquor,
wherein the raw material methacrylic acid and methanol are mixed so that a concentration of methanol in the mixed solution is 3.0 to 3.75% by mass, and
the crystal of methacrylic acid is precipitated from the mixed solution in a cooling crystallization vessel.

2. The method for purifying methacrylic acid according to claim 1 , wherein a temperature in the cooling crystallization vessel is controlled in the range of 4 to 8° C.

3. The method for purifying methacrylic acid according to claim 1 , wherein the raw material methacrylic acid and methanol are mixed so that the concentration of methanol in the mixed solution is 3.0 to 3.75% by mass, and then the mixed solution is supplied to the cooling crystallization vessel.

4. The method for purifying methacrylic acid according to claim 3 , wherein the mixed solution is continuously supplied to the cooling crystallization vessel.

5. The method for purifying methacrylic acid according to claim 3 , wherein the mixed solution having a temperature of 9 to 20° C. is supplied to the cooling crystallization vessel.

6. The method for purifying methacrylic acid according to claim 1 , wherein
the cooling crystallization vessel comprises a baffle-equipped cylindrical container equipped with a cooling jacket, and
the cooling crystallization vessel comprises, inside the cylindrical container:
a scraper unit for scraping a crystal precipitated on an inner surface of the cylindrical container;
a rotating shaft; and
an anchor-shaped scraper arm linking the rotating shaft and the scraper unit.

7. The method for purifying methacrylic acid according to claim 6 , wherein the scraper unit comprises:
a scraper blade for scraping a crystal precipitated on an inner surface of the cylindrical container;
a scraper blade holder comprising a blade supporting portion supporting the scraper blade, and an arm coupling portion fixed to the scraper arm; and
a spring type pressing apparatus for pressing the scraper blade against the inner surface of the cylindrical container via the blade supporting portion.

8. The method for purifying methacrylic acid according to claim 7 , wherein a lower portion of the scraper arm comprises a flat paddle blade portion, and
the lower portion of the scraper arm comprises a portion in which a length of the flat paddle blade portion in an axial direction of the cylindrical container shortens gradually from the rotating shaft toward a direction of a side surface of the cylindrical container.

9. A method for producing methacrylic acid, comprising:
forming raw material methacrylic acid; and
purifying the raw material methacrylic acid by the method according to claim 1 .

10. The method for producing methacrylic acid according to claim 9 , further comprising:
subjecting, to solid-liquid separation, a suspension slurry formed by the purifying of the raw material methacrylic acid; and
purifying a solid obtained by the solid-liquid separation, by a high purity operation.

11. The method for producing methacrylic acid according to claim 1 , wherein the purity of the raw material methacrylic acid is in a range of 99.00 to 99.99% by mass.

12. The method for producing methacrylic acid according to claim 1 , wherein the purity of the raw material methacrylic acid is in a range of 99.00 to 99.90% by mass.

13. The method for producing methacrylic acid according to claim 1 , wherein the raw material methacrylic acid and methanol are mixed so that a concentration of methanol in the mixed solution is 3.1 to 3.75% by mass.

14. The method for producing methacrylic acid according to claim 1 , further comprising conducting a high purity operation for removing the remaining mother liquor including methanol from the crystal.

Assignees

• Mitsubishi Chem Corp

Inventors

• Kanaya Koji
• Hino Tomomichi
• Kato Shinpei
• Toyoda Takafumi

Classifications

• B01D9/0077

  Screening for crystallisation conditions or for crystal forms · CPC title

• B01D9/0013

  by indirect heat exchange · CPC title

• C07C51/43 Primary

  by change of the physical state, e.g. crystallisation · CPC title

• B01D9/0009

  by direct heat exchange with added cooling fluid · CPC title

• B01D9/005

  Selection of auxiliary, e.g. for control of crystallisation nuclei, of crystal growth, of adherence to walls; Arrangements for introduction thereof · CPC title