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Process for manufacturing high purity methacrylic acid


Title: Process for manufacturing high purity methacrylic acid.
Abstract: A process is provided herein for the high yield production of high purity glacial methacrylic acid (“HPMAA”) that is substantially pure, specifically 99% pure or greater with a water content of 0.05% or less. This improved process comprises providing a crude MAA stream and purifying the crude methacrylic acid stream in a series of successive distillation steps ...




USPTO Applicaton #: #20090084667 - Class: 202158 (USPTO) - 04/02/09 - Class 202 
Inventors: Keith Frederick Briegel, James Clarence Day, Michael Stanley Decourcy, Donald Alan Ebert, Jamie Jerrick John Juliette

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The Patent Description & Claims data below is from USPTO Patent Application 20090084667, Process for manufacturing high purity methacrylic acid.

The present invention is related to a process for the production of substantially pure methacrylic acid that is at least 99% pure further having 0.05% or less water content.

Methacrylic acid (“MAA”) and methacrylate esters such as methyl methacrylate (“MMA”) are used in a wide variety of applications. Typical end-use applications include: acrylic plastic sheeting; molding resins; polyvinyl chloride modifiers; processing aids; acrylic lacquers; floor polishes; sealants; auto transmission fluids; crankcase oil modifiers; automotive coatings; ion exchange resins; cement modifiers; water treatment polymers; electronic adhesives; metal coatings; and acrylic fibers. MAA and methacrylate esters are especially prized in these applications and others because of the hardness they impart to the products in which they are used. They also enhance chemical stability and light stability, as well as ultraviolet radiation resistance, of the products in which they are used. Therefore, MAA and methacrylate esters are often used in applications requiring resins of excellent transparency, strength, and outdoor durability. The MAA market is extremely cost-sensitive; thus, any improvement in process yield, however slight, can result in significant market advantage.

MAA that has a very low percentage by weight of impurities is very desirable. MAA having an impurity level of less than 5% by weight is referred to herein as glacial methacrylic acid (“GMAA”). MAA having an impurity level of less than 1% by weight wherein no more than 0.05% by weight is water is referred to herein as high purity glacial methacrylic acid (“HPMAA”).

A conventional process for purifying MAA involves treating the stream with an excess of sulfuric acid to remove some of the water. While this process yields MAA of sufficient purity for use in batch production of direct-esterification esters, it also creates undesirable sulfur-bearing residue. Moreover, the MAA is not purified to 95%, and, therefore, does not meet the requirements of a GMAA or an HPMAA product. Further, such conventional processes for the removal of water from MAA have resulted in increased yield losses and additional waste. Thus, specifications for GMAA (i.e., MAA that is at least 95% pure) and HPMAA (i.e., MAA that is 99% pure further having less than 0.05% water content) have not been met with conventional purification processes.

Therefore, there is an unaddressed need for a method to produce HPMAA at a reduced cost for the manufacturer. Further, there is an unaddressed need to produce HPMAA that consistently meets the product specifications of at least 99% purity and less than 0.5% water.

The present invention solves the problems inherent in the prior art by providing an economical method for producing HPMAA. The present invention involves the purification of MAA to HPMAA via the use of distillation columns to remove various impurities (generally, light impurities, heavy impurities, and water) from an MAA stream such that the resultant product is at least 99% pure MAA with not more than 0.05% water.

Thus, provided herein is a process for the preparation of high purity glacial methacrylic acid, said process comprising: (i) providing a first distillation column, a second distillation column and a third distillation column; (ii) feeding a crude methacrylic acid to an upper section of said first distillation column, said crude methacrylic acid comprising methacrylic acid, light ends and heavy ends; (iii) distilling said crude methacrylic acid in said first distillation column to form a first overhead vapor stream comprising light ends and a first bottom liquid stream comprising methacrylic acid and heavy ends; (iv) feeding said first bottom liquid stream to a center section of said second distillation column; (v) distilling said first bottom liquid stream in said second distillation column to form a second overhead vapor stream comprising methacrylic acid and light ends and a second bottom liquid stream comprising heavy ends; (vi) feeding at least a portion of said second overhead vapor stream to an upper section of said third distillation column; (vii) distilling said at least a portion of said second overhead vapor stream in said third distillation column to form a third overhead vapor stream comprising light ends and a third bottom liquid stream comprising methacrylic acid wherein said methacrylic acid has an impurity level of not more than 1% by weight wherein no more than 0.05% by weight is water.

Additionally, provided herein is a further process for the preparation of high purity glacial methacrylic acid, said process comprising: (i) providing a first distillation column, a second distillation column and a third distillation column; (ii) feeding a crude methacrylic acid to an upper section of said first distillation column, said crude methacrylic acid comprising methacrylic acid, light ends and heavy ends; (iii) distilling said crude methacrylic acid in said first distillation column to form a first overhead vapor stream comprising light ends and a first bottom liquid stream comprising methacrylic acid and heavy ends; (iv) feeding said first bottom liquid stream to a center section of said second distillation column; (v) distilling said first bottom liquid stream in said second distillation column to form a second overhead vapor stream comprising methacrylic acid and light ends and a second bottom liquid stream comprising heavy ends; (vi) feeding at least a portion of said second overhead vapor stream to an upper section of said third distillation column; (vii) distilling said at least a portion of said second overhead vapor stream in said third distillation column to form a third overhead vapor stream comprising light ends and a third bottom liquid stream comprising heavy ends, while withdrawing a first liquid sidestream from a lower section of said third distillation column, said first liquid sidestream comprising methacrylic acid wherein said methacrylic acid has an impurity level of not more than 1% by weight wherein no more than 0.05% by weight is water; (viii) feeding said third bottom liquid stream to said center section of said second distillation column.

Additionally, provided herein is a still further process for the preparation of high purity glacial methacrylic acid, said process comprising: (i) providing a first distillation column, a second distillation column and a third distillation column; (ii) feeding a crude methacrylic acid to a center section of said first distillation column, said crude methacrylic acid comprising methacrylic acid, light ends and heavy ends; (iii) distilling said crude methacrylic acid in said first distillation column to form a first overhead vapor stream comprising methacrylic acid and light ends and a first bottom liquid stream comprising heavy ends; (iv) feeding at least a portion of said first overhead vapor stream to an upper section of said second distillation column; (v) distilling said at least a portion of said first overhead vapor stream in said second distillation column to form a second overhead vapor stream comprising light ends and a second bottom liquid stream comprising methacrylic acid and heavy ends; (vi) feeding said second bottom liquid stream to a center section of said third distillation column; (vii) distilling said second bottom liquid stream in said third distillation column to form a third overhead vapor stream comprising methacrylic acid wherein said methacrylic acid has an impurity level of not more than 1% by weight wherein no more than 0.05% by weight is water and a third bottom liquid stream comprising heavy ends; (viii) feeding at least a portion of said third overhead vapor stream to an upper section of said third distillation column; (ix) feeding said third bottom liquid stream to said center section of said first distillation column.

Moreover, the present invention also provides an apparatus for the preparation of high purity glacial methacrylic acid, said apparatus comprising: (i) a first distillation column, said first distillation column having a top, a bottom, an upper section adjacent said top, a lower section adjacent said bottom and a center section intermediate said upper section and said lower section; (ii) a second distillation column, said second distillation column having a top, a bottom, an upper section adjacent said top, a lower section adjacent said bottom and a center section intermediate said upper section and said lower section; (iii) a third distillation column, said third distillation column having a top, a bottom, an upper section adjacent said top, a lower section adjacent said bottom and a center section intermediate said upper section and said lower section; (iv) a first inlet line connected to said upper section of said first distillation column; (v) a first outlet line connected to said top of said first distillation column; (vi) a second outlet line connecting said bottom of said first distillation column and said center section of said second distillation column; (vii) a third outlet line connecting said top of said second distillation column with said upper section of said second distillation column and said upper section of said third distillation column; (viii) a fourth outlet line connected to said bottom of said second distillation column; (ix) a fifth outlet line connected to said top of said third distillation column; (x) a sixth outlet line connected to said bottom of said third distillation column.

Additionally, the present invention further provides an apparatus for the preparation of high purity glacial methacrylic acid, said apparatus comprising: (i) a first distillation column, said first distillation column having a top, a bottom, an upper section adjacent said top, a lower section adjacent said bottom and a center section intermediate said upper section and said lower section; (ii) a second distillation column, said second distillation column having a top, a bottom, an upper section adjacent said top, a lower section adjacent said bottom and a center section intermediate said upper section and said lower section; (iii) a third distillation column, said third distillation column having a top, a bottom, an upper section adjacent said top, a lower section adjacent said bottom and a center section intermediate said upper section and said lower section; (iv) a first inlet line connected to said upper section of said first distillation column; (v) a first outlet line connected to said top of said first distillation column; (vi) a second outlet line connecting said bottom of said first distillation column and said center section of said second distillation column; (vii) a third outlet line connecting said top of said second distillation column with said upper section of said second distillation column and said upper section of said third distillation column; (viii) a fourth outlet line connected to said bottom of said second distillation column; (ix) a fifth outlet line connected to said top of said third distillation column; (x) a sixth outlet line connected to said lower section of said third distillation column; (xi) a seventh outlet line connecting said bottom of said third distillation column to said center section of said second distillation column.

Additionally, the present invention still further provides an apparatus for the preparation of high purity glacial methacrylic acid, said apparatus comprising: (i) a first distillation column, said first distillation column having a top, a bottom, an upper section adjacent said top, a lower section adjacent said bottom and a center section intermediate said upper section and said lower section; (ii) a second distillation column, said second distillation column having a top, a bottom, an upper section adjacent said top, a lower section adjacent said bottom and a center section intermediate said upper section and said lower section; (iii) a third distillation column, said third distillation column having a top, a bottom, an upper section adjacent said top, a lower section adjacent said bottom and a center section intermediate said upper section and said lower section;


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stats Patent Info
Application #
US 20090084667 A1
Publish Date
04/02/2009
Document #
12069193
File Date
02/07/2008
USPTO Class
202158
Other USPTO Classes
International Class
01D3/16
Drawings
4


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