Preparation method of adiponitrile and product thereof

A technology of adiponitrile and adipic acid, which is applied in the field of preparation of adiponitrile, can solve problems such as poor mixing effect, influence on operation cycle, and generation of coke, so as to avoid by-products and coke, and reduce production costs , the effect of improving the catalytic performance

Active Publication Date: 2018-11-16
重庆华峰聚酰胺有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Adipic acid will generate by-products such as decarboxylation, decomposition, and coking at high temperatures, which not only affect the unit consumption; adipic acid will also generate coke at high temperatures and affect the operating cycle.
[0005] Patent CN201510185122.7 discloses the method for producing adiponitrile by adipic acid liquid phase method. Its main innovation point is the use of solid phosphoric acid catalyst. Although it can be stirred, the mixing effect is not very good, and its catalytic performance will also be affected.
[0006] Patent CN201

Method used

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  • Preparation method of adiponitrile and product thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] The molten adipic acid with a flow rate of 2400kg / h is sent from the adipic acid buffer tank 1, and the liquid phosphoric acid catalyst of 4.8kg / h is uniformly mixed through the mixer 3 at the outlet of the adipic acid feed pump, and then sent to the ammoniation reaction device 4. The reactor is fed with ammonia gas of 2236kg / h through the ammonia gas inlet 43 (the molar ratio of adipic acid is 8:1, that is, the excess of ammonia gas is 3 times), and the reaction is carried out under the conditions of 160°C and 90KPa, and the adipic acid The acid ammoniation rate is 95%. The ammoniated material enters the nitrilation reactor 5, and is heated to 260°C by steam heating of VP-1 heat transfer oil with good thermal stability and low liquid phase viscosity to generate adiponitrile for dehydration. The reaction will generate by-products such as cyclopentanone and ICCP and intermediate products such as cyanovaleric acid and cyanovaleramide simultaneously. The adiponitrile con...

Embodiment 2

[0033] After flow is the molten adipic acid of 2400kg / h and the liquid phosphoric acid catalyst of 7.2kg / h by the circulation line of mixer and feed pump after uniform mixing, feed the ammonia gas of 2794kg / h (with the mol ratio of adipic acid 10:1, that is, the excess of ammonia is 4 times), wherein the fresh ammonia is about 485kg / h, and the circulating ammonia is about 2309kg / h. Under the condition of 170 DEG C and 90KPa, in the ammoniation reactor 4, the ammoniation rate of adipic acid is 96.5%. The ammoniated material enters the nitrilation reactor, and is dehydrated at 270°C by using VP-1 heat transfer oil steam to generate adiponitrile; the reaction will also generate cyclopentanone, ICCP and other by-products, cyanovaleric acid, cyano Intermediate products such as pentamide. The adiponitrile comprising intermediate product can also continue to enter the lower part of the separation tower for separation, while a part of the circulating liquid is sent back to the bottom...

Embodiment 3

[0035] After flow is the molten adipic acid of 2400kg / h and the liquid ammonium phosphate catalyst of 16.2kg / h by the circulation line of mixer and feed pump after evenly mixing, pass into the ammonia gas of 4471kg / h (with the mole of adipic acid The ratio is 16:1, that is, the excess of ammonia is 7 times) to react, wherein the fresh ammonia is about 776kg / h, and the circulating ammonia is about 3695kg / h. Under the condition of 180 DEG C and 90KPa, in the ammoniation reactor 4, the ammoniation rate of adipic acid is 98.5%. The ammoniated material enters the nitrilation reactor, and is dehydrated at 290°C by using VP-1 heat transfer oil steam to generate adiponitrile; the reaction will also generate cyclopentanone, ICCP and other by-products, cyanovaleric acid, cyano Intermediate products such as pentamide. The adiponitrile containing the intermediate product can also continue to enter the lower part of the separation tower for separation, and the pipeline at the bottom of th...

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Abstract

The invention relates to a preparation method of adiponitrile. The preparation method comprises the following steps: firstly performing a reaction on adipic acid and ammonia at 155-200 DEG C to produce diammonium adipate, and then dehydrating under a catalytic reaction of phosphoric acid or ammonium phosphate to produce adiponitrile; a product can be further separated in a separation tower. The reaction is performed on the adipic acid and the ammonia gas at the low temperature of 155-200 DEG C to produce H4NOOC(CH2)4COONH4 first, and then high-temperature cyanation is performed, so that the opportunity of producing a by-product and a coke from the adipic acid at high temperature is effectively avoided, not only the yield is increased by 3-5%, but also the operation cycle of a production device is prolonged by 30-60 days, and the production per unit time is increased. Liquid phosphoric acid is used as a catalyst, firstly ammonium salt of the phosphoric acid is produced, and the ammoniumphosphate can be mixed with ammonium salt of the adipic acid very well, so that the catalytic performance is improved better and the selectivity of the adiponitrile is increased by more than 2%.

Description

technical field [0001] The invention belongs to the field of chemical industry, and relates to a preparation method of adiponitrile and a product thereof. Background technique [0002] Adiponitrile (ADN), also known as 1,4‐dicyanobutane, has a molecular formula of NC(CH3)4CN. Addition of adiponitrile and hydrogen can generate hexamethylenediamine, and hexamethylenediamine and adipic acid can be produced under strict material distribution. The lower reaction produces nylon 66 salt. As an important intermediate for the synthesis of nylon 66, adiponitrile is the most important and most valuable industrial application developed by adiponitrile. Research has found that hexamethylenediamine can be used to synthesize 1,6‐hexamethylene diisocyanate (HDI), which is another important use for the development of the downstream product chain of adiponitrile; with the rapid development of science and technology, adiponitrile is used in light industry, electronics and other organic Appli...

Claims

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Application Information

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IPC IPC(8): C07C255/04C07C253/22
CPCC07C51/412C07C253/22C07C53/126C07C255/04
Inventor 陈恩之赵风轩姜曦徐淑媛王焕哲张楠李全周晓燕孟启贵刘新安陈发挥
Owner 重庆华峰聚酰胺有限公司
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