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Preparation method and device of acetyl chloride and hydroxy ethylene diphosphonic acid coproduction

A technology for the co-production of acetyl chloride to hydroxyethylene diphosphonic acid and a preparation device, which is applied in the chemical industry and can solve the problems of long overall process time, non-recyclable residual liquid, and prone to accidents, so as to ensure continuous stability and standardization , Realize the effect of standardization and controllability, production safety guarantee

Inactive Publication Date: 2008-12-17
常州晓舟科贸有限公司
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AI Technical Summary

Problems solved by technology

[0012] 1. Due to the excessive phosphorus trichloride input in the production process, and the complex reaction of the process itself, there are more impurities in the finished acetyl chloride
[0013] 2. The finished acetyl chloride contains a small amount of phosphorus impurities, which will become turbid after long-term storage
[0014] 3. The by-product phosphorous acid contains a certain amount of hydroxyethylidene diphosphonic acid acetate, and the appearance is not good, which affects the application of the by-product phosphorous acid, and the economic benefit is poor
[0015] 4. In the process of purifying 98% acetyl chloride to 99%, the residual liquid in the kettle will be produced, which cannot be recycled, and three wastes will be produced
[0028] 1. A large amount of by-product hydrochloric acid is produced. In the case of poor sales of hydrochloric acid in the market, it will have an impact on expanding the production of hydroxyethylene diphosphonic acid, thereby affecting economic benefits
[0029] 2. During the dropping process, phosphorus trichloride reacts violently with water. If the operation is improper, a large amount of hydrogen chloride gas will be generated in the kettle, which will increase the pressure in the system and cause accidents easily.
[0030] 3. Under the condition of negative pressure, the material in the kettle is easy to escape, and the unit consumption of raw materials is 170.5kg of theoretical ton of 58% hydroxyethylidene diphosphonic acid and 785kg of 98.5% phosphorus trichloride.
The market price of acetyl chloride is about twice that of glacial acetic acid, and only 765 kg of glacial acetic acid can be obtained by consuming 1000 kg of acetyl chloride. It can be seen that this process wastes a part of the possible economic benefits
[0032] 5. The overall process time is too long and the energy consumption is too large
[0033] 6. In the production steps of dropping and heating up, due to the complicated operation, the superior product of hydroxyethylene diphosphonic acid cannot be produced stably

Method used

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  • Preparation method and device of acetyl chloride and hydroxy ethylene diphosphonic acid coproduction

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preparation example Construction

[0051] A kind of preparation method of acetyl chloride coproduction hydroxyethylene diphosphonic acid, it is characterized in that adopting following steps:

[0052] a) After adding glacial acetic acid into the reactor, start stirring, and complete the dropwise addition of phosphorus trichloride to the reactor under normal pressure for 1 to 2 hours, so that the molar number of acetic acid in the reactor is 3.0 to 3.0 to the molar number of phosphorus trichloride. 3.2 times.

[0053] b) Turn on the jacket steam of the reaction kettle, and control the jacket steam flow rate to 30-200kg / h. , so that the reactor can continue to heat up, and through the following three steps:

[0054] Step 1. Directly receive liquid acetyl chloride, and at the same time control the amount of hydrogen chloride gas generated by the reaction in the kettle to be stable at 30-60kg / h, operate for 8-12 hours, and raise the temperature in the kettle to 40-55°C;

[0055] Step 2. Control the reflux rate of...

Embodiment 1

[0065]Add 2190kg of glacial acetic acid into a 3000-liter reactor; start stirring, and dropwise add 1664kg of 98.5% phosphorus trichloride under normal pressure within 1 hour. Kmol. Directly receive the condensed acetyl chloride, the hydrogen chloride gas production is stable at 35-50kg / h, it takes 8 hours, and the temperature in the kettle slowly rises to 46°C; 2.5h, the temperature in the kettle is 54℃, and the temperature at the top of the rectification tower can be stabilized for 0.5h; The temperature began to drop, the reflux of acetyl chloride was stopped, and 1632 kg of 99.21% finished product acetyl chloride was finally received; the temperature in the kettle was 120±2°C, and it took 1.5 hours to keep the hydroxyethylidene diphosphonic acid acetate; the tail gas was used by the absorption tower After absorbing 400kg of glacial acetic acid at 20-30℃, it will be absorbed into 1500kg of 31% hydrochloric acid in the falling film absorber, and finally the weight of the abs...

Embodiment 2

[0067] Add 3360kg of glacial acetic acid into a 5000-liter reactor; start stirring, and dropwise add 2550kg of 98.5% phosphorus trichloride under normal pressure within 1.5 hours. It is 18.29Kmol. Directly receive the condensed acetyl chloride, the hydrogen chloride gas production is stable at 40-55kg / h, it takes 11 hours, and the temperature in the kettle slowly rises to 53°C; 3.5 hours, the temperature in the kettle is 63°C, and the temperature at the top of the rectification tower can be stabilized for 0.5h; The temperature begins to drop, stop the reflux of acetyl chloride, and finally receive 2500 kg of 99.16% finished product acetyl chloride; the temperature in the kettle is 120 ± 2 ° C, and it takes 2 hours to carry out the insulation of hydroxyethylene diphosphonic acid acetate; After absorbing 800kg of glacial acetic acid at ~30°C, it will be absorbed into 2300kg of 31% hydrochloric acid in the falling film absorber, and finally the weight of the absorbed liquid will...

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Abstract

The present invention belongs to the field of chemical technology, in the concrete, it relates to a preparation method for simultaneously producing acetyl chloride and hydroxyethylidene diphosphonate and its equipment. Said method includes the following steps: adding glacial acetic acid and phosphorus trichloride according to the mole ratio of 3.0-3.2:1 in a reaction still, adopting continuous three-stage heating mode: 40-55 deg.C, 48-65 deg.C and 55-100 deg.C to make them produce reaction in the still so as to form hydroxyethylidene diphosphonate acetate and produce acetyl chloride vapor, making said acetyl chloride vapor be passed through rectification device and condensation device so as to obtain the liquid acetyl chloride whose content is greater than 99%.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to a preparation method and device for co-producing hydroxyethylene diphosphonic acid with acetyl chloride. Background technique [0002] Acetyl chloride is an important organic synthesis intermediate and acetylation reagent. Its acylation ability is stronger than that of acetic anhydride. It is widely used in organic synthesis and can be used in the production of pesticides, medicines, new electroplating complexing agents, and other fine organic synthesis Intermediate, it can be used in medicine to make 2,4-dichloro-5-fluoroacetophenone (intermediate of ciprofloxacin), ibuprofen, etc. Acetyl chloride is also a catalyst for the chlorination of carboxylic acids. [0003] The main industrial method of acetyl chloride is the glacial acetic acid-phosphorus trichloride method. Under normal pressure, add excess phosphorus trichloride slowly to glacial acetic acid, ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C53/40C07C51/60C07F9/38
Inventor 周烜
Owner 常州晓舟科贸有限公司
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