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Preparation method of cyclic carbonate with joint product of ammonium hydrogen phosphate

A technology of cyclic carbonate and ammonium hydrogen phosphate, which is applied in the direction of phosphate, phosphorus oxyacids, chemical instruments and methods, etc., can solve the problems of non-environmental friendliness, poor safety, high production cost, etc., so as to reduce production cost and produce The effect of high strength and high equipment utilization

Inactive Publication Date: 2012-05-23
淮安市淮安区综合检验检测中心
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to overcome the problems of poor safety, high production cost and non-environmental friendliness in the background technology, the present invention provides a new process for synthesizing cyclic carbonates that can simultaneously co-produce diammonium hydrogen phosphate or ammonium dihydrogen phosphate products, with Features of high safety, low production cost and environmental friendliness

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  • Preparation method of cyclic carbonate with joint product of ammonium hydrogen phosphate
  • Preparation method of cyclic carbonate with joint product of ammonium hydrogen phosphate

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preparation example Construction

[0018] The preparation method of the cyclic carbonate co-producing ammonium hydrogen phosphate at the same time of the present invention includes the following steps:

[0019] A certain proportion of urea, adjacent diol and catalyst are added to the reactor 1, and then a certain amount of phosphoric acid or polyphosphoric acid aqueous solution is added to the ammonia absorption device 3. The reactor is sealed, condensed water is passed into the condensing reflux device 2, the vacuum pump is turned on to vacuum the reaction system, and the reaction solution is heated to reach the desired reaction temperature. After the reaction is over, the vacuum pump is turned off and the heating is stopped. After the reactor drops to room temperature, the reaction solution is weighed and sampled for analysis. The samples were analyzed by Fuli 9790II gas chromatograph, FID detector, and KB-5 column. Set the vaporization chamber temperature to 260°C, the column temperature to 170°C, and the dete...

Embodiment 1

[0022] 50 g of 85% phosphoric acid was added to the ammonia absorption device 3. 15.00g of urea, 23.3g of ethylene glycol, and 0.75g of basic lead carbonate were added to the reactor 1, the reaction temperature was 126°C, the reaction pressure was 9KPa, and the reaction time was 3h. The product obtained in reactor 1 is ethylene carbonate. The yield was 60.2%. The ammonium dihydrogen phosphate crystal can be directly obtained in the ammonia absorption device 3, and its mass is 30g.

Embodiment 2

[0024] Add 40 g of polyphosphoric acid and 20 ml of water (60 g of polyphosphoric acid with a concentration of 66%) into the ammonia absorption device, and mix them evenly. 15.00 g of urea, 28 g of 1,2-propanediol, and 1.20 g of basic zinc carbonate were added to the reactor at a reaction temperature of 150° C., a reaction pressure of 21 KPa, and a reaction time of 4 h. The yield of the product propylene carbonate obtained in reactor 1 was 71%. The ammonium dihydrogen phosphate crystal can be directly obtained in the ammonia absorption device, and its mass is 40g.

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Abstract

The invention discloses a preparation method of cyclic carbonate with a joint product of ammonium hydrogen phosphate. The method comprises the following steps: adding urea, vicinal diol and a subcarbonate catalyst with a weight ratio of 1: (1.5-2.0) : (0.05-0.1) to a reactor, wherein the reactor is provided with a condensing reflux device communicated with an ammonia absorption device connected with a vacuum pump; adding an aqueous solution of phosphoric acid or polyphosphoric acid, which is 1.3-4.2 times the weight of the urea; leading condensed water into the condensing reflux device; and opening the vacuum pump to vacuumize a reaction system so that pressure in the reaction is 5-50 kPa, reaction temperature is controlled at 120-190 DEG C, and reaction time is 2-10 hours. A reaction product of ethylene carbonate or propylene carbonate is obtained in the reactor after the reaction is finished, and the joint reaction product of monoammonium phosphate or diammonium phosphate is also obtained in the ammonia absorption device.

Description

Technical field [0001] The invention relates to a preparation method of cyclic carbonate, in particular to the synthesis of ethylene carbonate or propylene carbonate from urea and ethylene glycol or 1,2-propylene glycol as raw materials, and the simultaneous co-production of diammonium hydrogen phosphate or dihydrogen phosphate Preparation method of ammonium. Background technique [0002] Ethylene carbonate and propylene carbonate have a wide range of uses. They can be used as electrolyte solutions for lithium batteries, plasticizers for solid polymer electrolytes, spinning liquids on textiles, and for removing acid gases (such as carbon dioxide, sulfur dioxide, etc.) Solvents, concrete additives, plastic foaming agents and synthetic lubricant stabilizers, etc. As intermediates in organic synthesis, they undergo transesterification with methanol and ethanol to produce dimethyl carbonate and diethyl carbonate, respectively. In addition, they can also be used to synthesize polyca...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D317/38C07D317/36C01B25/28B01J27/236
Inventor 杨伯伦邱鹏
Owner 淮安市淮安区综合检验检测中心