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Improved production method of N-phosphonomethyl glycine

A technology of phosphonomethylglycine and its production method, which is applied in the field of N-phosphonomethylglycine, can solve the problems of decreased reaction yield, difficult heat transfer in time, poor heat transfer effect of fixed bed, etc., so as to avoid excessive oxidation, Uniform residence time effect

Active Publication Date: 2010-11-10
ZHEJIANG XINAN CHEM INDAL GROUP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Diglyphosate oxidation is an exothermic reaction, and the heat transfer effect of the fixed bed used in this patent is poor, and the heat generated in the reaction process is difficult to transfer in time, so the temperature is too high and the by-product aminomethyl phosphoric acid is generated, which makes the reaction more efficient. rate drop

Method used

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  • Improved production method of N-phosphonomethyl glycine
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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Under the temperature of 100~110 ℃ and the pressure of 0.1~0.25MPa, put 98% PMIDA and deionized water into the dissolving kettle according to a certain ratio and be prepared with a solution of 2% diglyphosate by weight, and then use After the pump is metered, it is pumped into a total of three-stage fixed-bed reactors equipped with 4Kg of activated carbon catalyst at each stage. Pure oxygen gas is metered into the fixed bed reactor at a rate of 3.9Kg / h. The reactor pressure was maintained at about 0.7 MPa, and the reactor temperature at each stage was maintained at 120°C. Experiments were carried out at various liquid feed rates. The reaction results are shown in Table 1.

[0037] Table 1

[0038]

[0039]

Embodiment 2

[0041] Under the temperature of 100~110 ℃ and the pressure of 0.1~0.25MPa, put 98% PMIDA and deionized water into the dissolving kettle according to a certain ratio and be prepared with a solution of 2% diglyphosate by weight, and then use After the pump is metered, it is pumped into a total of three-stage fixed-bed reactors equipped with 4Kg of activated carbon catalyst at each stage. Pure oxygen gas is metered into the fixed bed reactor at a rate of 3.4Kg / h. The reactor pressure was maintained at about 0.55MPa, the primary reactor temperature was maintained at 115°C, the secondary reactor temperature was maintained at 110°C, and the tertiary reactor temperature was maintained at 90°C. Experiments were performed at various liquid feed rates conduct. The reaction results are shown in Table 2.

[0042] Table 2

[0043]

Embodiment 3

[0045] Under the temperature of 120~140 ℃ and the pressure of 0.2~0.4MPa, put 98% PMIDA and deionized water into the feed mixer according to a certain proportion and be mixed with the aqueous solution of 6% diglyphosate in weight percent concentration, Squeeze into the total two-stage fixed-bed reactor that every stage is equipped with 9Kg active carbon catalyst after metering with pump then. Pure oxygen gas is metered into the fixed bed reactor at a rate of 14.0Kg / h. The reactor pressure was maintained at about 0.55 MPa, the primary reactor temperature was maintained at 120°C, and the secondary reactor temperature was maintained at 90°C. Experiments were carried out at various liquid feed rates. The reaction results are shown in Table 3.

[0046] table 3

[0047]

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Abstract

The invention relates to an improved production method of N-phosphonomethyl glycine, in which a carbon catalyst is filled in a multi-stage fixed bed reactor; phosphonomethyl iminodiacetic acid slurry with the concentration in percentage by weight of 2-10% is used as a feed liquid to be mixed and heated firstly, then is sent into the fixed bed reactor after being pumped and metered, and is fully contacted with oxygen-containing gas which is supplied into the fixed bed reactor via a gas distributor so as to carry out catalytic oxidation reaction to continuously oxidize the phosphonomethy liminodiacetic acid into glyphosate; and the multi-stage fixed bed reactor is an isothermal reaction system formed by a plurality of stages of reactors connected in series, the top of each stage of reactor is provided with the feed liquid and the gas distributor, and the temperature of each stage of reactor is provided by heating or cooling media. A reaction pressure of 0-1.5 MPa and a reaction temperature of 30-180 DEG C are maintained in each stage of fixed bed reactor, and gas, liquid and solid in the reactor are fully contacted to carry out oxidizing reaction to obtain glyphosate feed liquid. The invention has the advantages of finding a multi-stage series isothermal reactor mode which has more uniform retention time than the existing fixed bed reactor and avoids excessive oxidation, and provides an application process which can keep ideal yield of glyphosate after being amplified.

Description

technical field [0001] The present invention relates to an improved method for preparing glyphosate by catalytic oxidation continuous reaction of N-phosphonomethyliminodiacetic acid, i.e., bisglyphosate (PMIDA), which belongs to N-phosphonomethylglycine, i.e. glyphosate Field of preparation of phosphine (PMG). Background technique [0002] Glyphosate is a systemic conductive broad-spectrum herbicide with the advantages of high efficiency, broad-spectrum, low toxicity and no residue. In recent years, due to the expansion of global planting of genetically modified crops, the recovery and modernization of global agriculture, especially in developing countries, and the production of renewable energy, the market demand for glyphosate has grown rapidly, and the sales volume has increased by nearly 15% per year. , has occupied the first place in the world's pesticide sales for many years, and has become the fastest growing pesticide variety. [0003] There are currently two produ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/38B01J8/04A01N57/20A01P13/00
Inventor 王伟周曙光陈静杨旭张海良任不凡佘慧玲
Owner ZHEJIANG XINAN CHEM INDAL GROUP
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