Novel technique for coproduction of 2-phosphonobutane-1,2,4-tricabroxylic acid and methyl chloride

A technology of phosphonobutane and methyl chloride, which is applied in the chemical industry, can solve problems such as non-existence, and achieve the effects of reducing costs, protecting the environment, and absorbing high costs

Active Publication Date: 2011-06-15
CHANGZHOU JIAYOU CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there is no industrial process for the production of PBTCA water treatment agent with good performance and the co-production of important organic synthesis intermediate methyl chloride.

Method used

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  • Novel technique for coproduction of 2-phosphonobutane-1,2,4-tricabroxylic acid and methyl chloride
  • Novel technique for coproduction of 2-phosphonobutane-1,2,4-tricabroxylic acid and methyl chloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) Put 700 kg of dimethyl maleate and 540 kg of dimethyl phosphite into the reaction kettle, open the main kettle to freeze brine, add 30 kg of sodium methoxide dropwise, control the dropping temperature at 30°C, and pass the test after dropping Semi-finished tetramethyl phosphonosuccinate;

[0025] (2) Add 560 kg of methyl acrylate to the above-mentioned qualified semi-finished tetramethyl phosphonosuccinate, add dropwise 40 kg of sodium methoxide after cooling, control the dropping temperature at 25°C, and detect the qualified intermediate 2-phosphonic acid after dropping Pentamethyl butane-1,2,4-tricarboxylate;

[0026] (3) Pass 1780 kilograms of hydrogen chloride gas into the intermediate 2-phosphonobutane-1,2,4-tricarboxylate pentamethyl ester that is qualified as above-mentioned detection, control ventilation temperature 50 ℃, reflux 8 hours, detect and obtain Product 2-phosphonobutane-1,2,4-tricarboxylic acid, open the methyl chloride recovery device at the sam...

Embodiment 2

[0032] (1) Put 700 kg of dimethyl maleate and 540 kg of dimethyl phosphite into the reaction kettle, open the main kettle to freeze brine, add 25 kg of sodium methoxide dropwise, control the dropping temperature at 50°C, and pass the test after dropping Semi-finished tetramethyl phosphonosuccinate;

[0033] (2) Add 550 kg of methyl acrylate to the above-mentioned qualified semi-finished tetramethyl phosphonosuccinate, add 35 kg of sodium methoxide dropwise after cooling, control the dropping temperature at 50°C, and obtain the qualified intermediate 2-phosphonic acid after dropping Pentamethyl butane-1,2,4-tricarboxylate;

[0034] (3) Pass into 2150 kilograms of hydrogen chloride gas in the intermediate 2-phosphonobutane-1,2,4-tricarboxylate pentamethyl ester that is qualified as above-mentioned detection, control aeration temperature 70 ℃, reflux 9 hours, detect and obtain Product 2-phosphonobutane-1,2,4-tricarboxylic acid, open the methyl chloride recovery device at the sam...

Embodiment 3

[0040] (1) Put 700 kg of dimethyl maleate and 540 kg of dimethyl phosphite into the reaction kettle, open the main kettle to freeze the brine, add 37 kg of sodium methoxide dropwise, control the dropwise addition temperature at 70°C, and pass the test after dropping Semi-finished tetramethyl phosphonosuccinate;

[0041] (2) Add 630 kg of methyl acrylate to the above-mentioned qualified semi-finished tetramethyl phosphonosuccinate, add 56 kg of sodium methoxide dropwise after cooling, control the dropping temperature at 80°C, and obtain the qualified intermediate 2-phosphonic acid after dropping Pentamethyl butane-1,2,4-tricarboxylate;

[0042] (3) Pass 2150 kilograms of hydrogen chloride gas into the intermediate 2-phosphonobutane-1,2,4-tricarboxylate pentamethyl ester that is qualified as above-mentioned detection, control ventilation temperature 80 ℃, reflux 10 hours, detect and obtain Product 2-phosphonobutane-1,2,4-tricarboxylic acid, open the methyl chloride recovery dev...

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Abstract

The invention relates to a novel process for producing 2-phosphonobutane-1,2,4-tricarboxylic acid co-production methyl chloride. The process comprises the following steps: firstly, putting dimethyl maleate and dimethyl phosphite in a reaction kettle, and dripping sodium methoxide to prepare a semi-finished phosphono succinic acid tetramethylester; then adding methyl acrylate in the semi-finished phosphono succinic acid tetramethylester; cooling and dripping sodium methoxide to obtain a midbody 2-phosphonobutane-1,2,4-tricarboxylic acid pentamethyl ester; leading chlorine hydride gas into the midbody; carrying out circumfluence for hours to obtain a finished product 2-phosphonobutane-1,2,4-tricarboxylic acid; opening a methyl chloride recovering device to recover methyl chloride; discharging methyl chloride gas into a gas cabinet through a vacuum pump, and then discharging the methyl chloride gas after being dried to a condenser through a methyl chloride compressor; and finally, collecting liquid methyl chloride in a methyl chloride storage tank for standby selling. The process conforms to the environment protection requirement, can maximize the benefit of hydrochloric acid with low added value, obtains the methylated chemical product, i.e. the methyl chloride, and can reduce the cost and save energy.

Description

technical field [0001] The invention relates to the technical field of chemical industry, in particular to a process for producing 2-phosphonobutane-1,2,4-tricarboxylic acid (PBTCA) and co-producing methyl chloride. Background technique [0002] Scaling of the circulating cooling water system is a common problem in industrial production. Scale will significantly reduce the efficiency of the heat exchange system. At present, the method of adding phosphorus-containing scale inhibitors to the cooling water system is generally used in the industry to prevent water pipes from Wall corrosion and scaling. [0003] Organic phosphonic acid is the most widely used water treatment agent at present. It has excellent chelating ability for many metal ions, such as calcium, magnesium, iron and zinc, and it has excellent chelating ability for inorganic salt scale of these metals, especially carbonic acid. The scale inhibition ability of salt is also very strong. Because of the unique corro...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/38C07C19/03C07C17/00C02F5/14
Inventor 吴林华陈志龙赵荣明
Owner CHANGZHOU JIAYOU CHEM CO LTD
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