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vb 13 production method

A production method and product technology, applied in the production field of VB13, can solve the problem of high cost, achieve the effects of low production cost, improved color and appearance, and cost saving

Active Publication Date: 2017-09-26
PENGLAI MARINE SHANDONG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The orotic acid that above-mentioned method makes is VB 13 The color is pink, its yield is 86%, and its cost is also relatively high, basically at 200 yuan per kilogram

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] Embodiment 1 is the embodiment of laboratory test:

[0062] condensation reaction

[0063] (1) Put 85g of urea into the flask, 112g of maleic anhydride into the flask, add 55g of acetic acid, start stirring, heat up the hot water circulation, keep warm at 65°C for 10 hours, turn on the cooling water to cool down, add an appropriate amount of production water, dilute the material, and generate flow Sex, out of material.

[0064] (2) Suction filtration. After the completion, send a sample to test the water content, weigh it and dry it, and prepare for the acidification reaction.

[0065] Bromination reaction:

[0066] (1) Feeding: Add 1000ml of water into the flask, cool down to about 0°C, add 275g of bromine, add the condensation material from batch 1), and react for 20 hours.

[0067] (2) Suction filtration: release appropriate amount of material for suction filtration, after draining, rinse with about 50g of water, drain and prepare for acidification reaction.

[0...

Embodiment 2

[0079] Embodiment 2 is the embodiment of pilot production:

[0080] VB 13 A production method comprising the steps of:

[0081] (1) condensation

[0082] Put 86 kg of urea into a 500-liter condensation reactor (dry the condensation reactor at 100°C for 2-3 hours to ensure anhydrous), add 122 kg of maleic anhydride, add 80 kg of acetic acid under vacuum, and stir , heat the material in the condensation reaction kettle (heating can be heated by hot water circulation at 70-80°C), heat the material to 65°C, keep it warm for 12 hours, cool down to about 45°C, and then add 60 kg to the condensation reaction kettle The left and right water dilutes the material to make the material fluid, and then the material is released and centrifuged to obtain the condensed material;

[0083] When centrifuging, start the centrifuge to discharge the material. After the material is discharged, adjust the speed and wash it with water for 15-20 minutes. As long as there is no acetic acid smell at t...

Embodiment 3

[0095] VB 13 A production method comprising the steps of:

[0096] (1) condensation

[0097] Put urea into the condensation reaction kettle, add maleic anhydride, add acetic acid in a vacuum state, stir, heat the material in the condensation reaction kettle, heat it to 60°C, keep it warm for 8 hours, cool down to 40°C, and then add water to the condensation reaction kettle , release the material, and centrifuge to obtain the condensation material; the urea:maleic anhydride:acetic acid=7:11:7, the ratio is the weight ratio;

[0098] (2) Bromination

[0099] Put the condensation material obtained in step (1) into the bromination reaction kettle, add water and bromine, react for 20 hours, and centrifuge to obtain the bromination material; the addition of the water is 2.5 times the weight of the obtained condensation material, and the The weight ratio of the condensed material to bromine = 1:0.9; the weight of the condensed material is based on the dry product after removing mo...

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PUM

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Abstract

The invention belongs to the technical field of trace element production and particularly relates to a VB13 production method. The VB13 production method comprises the following steps that 1, urea, maleic anhydride and acetic acid are condensed; 2, the condensed material and bromine perform bromination reaction; 3, the brominated material performs acidification reaction with caustic soda liquid and hydrochloric acid; 4, the acidified material is crystallized; 5, the crystallized material is dried. The purity of VB13 produced by adopting the VB13 production method is above 98.5%, and the VB13 produced by means of the VB13 production method is a white crystal, the VB13 produced by adopting a traditional method is pink or light yellow, namely the color and luster appearance of the product is greatly improved. The VB13 production method is low in production cost. Compared with the prior art, the process cost of the VB13 production method is saved by 40%-45%.

Description

technical field [0001] The invention belongs to the technical field of trace element production, in particular to VB 13 production method. Background technique [0002] "Liaoning Chemical Industry" 2000 NO.2, Vol29 disclosed "Synthesis and Refining of Orotic Acid", the VB disclosed in this article 13 The operational route is as follows: get 2 kilograms of acetic acid, 10 kilograms of water, and 1.92 kilograms of maleic anhydride generate maleic acid monoureide in the presence of urea, then put it into a 15 kilogram pressure autoclave, and add 1.93 kilograms of bromine , Keep the reaction temperature at -5°C, keep it for 1.5 hours, filter, add 20 kg of 12% NaOH, heat it to 60-80°C, keep it for 4 hours, add 3.7 kg of acetic acid to adjust pH = 5, filter, wash, dry, Add 4.5 kg of 12% hydrochloric acid, stir for 3 hours, cool, wash, and dry at 130°C to obtain the finished product with a yield of about 56%. [0003] The orotic acid that above-mentioned method makes is VB 13 T...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D239/557
CPCC07D239/557
Inventor 隋晓明石丕强聂洪夫
Owner PENGLAI MARINE SHANDONG
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